# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

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

data_compound2a
_database_code_depnum_ccdc_archive 'CCDC 1055961'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_audit_creation_date             2015-05-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H60 Ce2 O21'
_chemical_formula_sum            'C54 H60 Ce2 O21'
_chemical_formula_weight         1325.26
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.2020(11)
_cell_length_b                   15.9564(14)
_cell_length_c                   16.1020(11)
_cell_angle_alpha                116.872(5)
_cell_angle_beta                 93.433(5)
_cell_angle_gamma                92.854(5)
_cell_volume                     3236.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    29992
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.268
_cell_measurement_theta_min      1.424
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.760
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   0.9643
_exptl_transmission_factor_min   0.7581
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.1299
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20909
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.424
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7369
_reflns_number_total             11352
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         11352
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0676
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1891
_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.

 After refinement of the primary molecule including part of lattice solvent
 molecule, attempts to model the residual electron density in the lattice 
 voids as disordered solvents gave unsatisfactory refinements. Subsequently,
 the electron density in voids was accounted for using PLATON/SQUEEZE (see below). 
;
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 -0.003 0.000 655 474
_platon_squeeze_details          
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
2. Shared sites
{C29, C229}
3. Restrained distances
 C4-C5 = C5-C6 = C6-C7 = C7-C8 = C8-C9 = C9-C4
 1.4 with sigma of 0.02
 C104-C105 = C105-C106 = C106-C107 = C107-C108 = C108-C109 = C109-C104
 1.4 with sigma of 0.02
 C231-C36 = C231-C232 = C232-C233 = C233-C34
 1.4 with sigma of 0.02
 C4-C6 = C5-C7 = C6-C8 = C7-C9 = C8-C4 = C9-C5
 2.38 with sigma of 0.02
 C231-C233 = C231-C35 = C232-C36 = C232-C34
 2.38 with sigma of 0.02
 C230-C36 = C230-C232
 2.55 with sigma of 0.02
 C231-C36 \\sim C231-C232
 with sigma of 0.02
 C230-C36 \\sim C230-C232
 with sigma of 0.02
4. Restrained planarity
 C34, C35, C36, C231, C232, C233, C230, O12
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uiso(C232) = Uiso(C233)
Uiso(C231) = Uiso(C233)
6. Others
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) C103(0.5) H10A(0.5) H10B(0.5) C4(0.5)
 C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9A(0.5)
 C33(0.7) H33(0.7) C32(0.7) H32(0.7) C104(0.5) C109(0.5) H109(0.5) C102(0.5)
 H10C(0.5) H10D(0.5) C3(0.5) H3A(0.5) H3B(0.5) C105(0.5) H105(0.5) C106(0.5)
 H106(0.5) C107(0.5) C108(0.5) H108(0.5) C31(0.7) C30(0.7) H30A(0.7) H30B(0.7)
 C29(0.7) H29A(0.7) H29B(0.7) C233(0.3) H233(0.3) C230(0.3) H23A(0.3) H23B(0.3)
 C232(0.3) H232(0.3) C231(0.3) C229(0.3) H22A(0.3) H22B(0.3)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C103(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B), C38(H38A,H38B), C39(H39A,H39B), C47(H47A,H47B), C48(H48A,H48B),
  C102(H10C,H10D), C3(H3A,H3B), C30(H30A,H30B), C29(H29A,H29B), C230(H23A,H23B),
  C229(H22A,H22B)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9A), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27), C33(H33), C32(H32), C41(H41), C42(H42),
  C44(H44), C45(H45), C50(H50), C51(H51), C53(H53), C54(H54), C109(H109),
 C105(H105), C106(H106), C108(H108), C35(H35), C233(H233), C232(H232)
7.c X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2), O3Z(H3Z1,H3Z2)
7.d Idealised tetrahedral OH refined as rotating group:
 O6(H6H), O9(H9), O12(H12), O15(H15H), O18(H18H)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.44605(3) 0.08646(4) 0.44046(3) 0.01419(16) Uani 1 1 d . . . . .
O1 O 0.3084(5) -0.0182(5) 0.3143(4) 0.0256(17) Uani 1 1 d . . . . .
C1 C 0.2672(7) -0.0422(8) 0.3699(7) 0.027(3) Uani 1 1 d . . . . .
Ce2 Ce 0.45595(4) 0.35111(4) 0.44948(3) 0.01592(17) Uani 1 1 d . . . . .
O2 O 0.3019(4) -0.0089(5) 0.4544(4) 0.0223(16) Uani 1 1 d . . . . .
C2 C 0.1677(19) -0.088(2) 0.3374(18) 0.040(7) Uiso 0.5 1 d . . P A 1
H2A H 0.1664 -0.1412 0.2737 0.048 Uiso 0.5 1 calc R U P A 1
H2B H 0.1255 -0.0418 0.3344 0.048 Uiso 0.5 1 calc R U P A 1
O3 O -0.2483(4) -0.2741(5) 0.3481(5) 0.0270(17) Uani 1 1 d . . . . .
H3 H -0.2854 -0.2313 0.3688 0.032 Uiso 1 1 calc R U . B 1
C103 C 0.0974(14) -0.0714(16) 0.3532(14) 0.028(5) Uiso 0.5 1 d . . P A 2
H10A H 0.1059 -0.0162 0.4159 0.034 Uiso 0.5 1 calc R U P A 2
H10B H 0.0880 -0.0469 0.3070 0.034 Uiso 0.5 1 calc R U P A 2
O4 O 0.3947(4) 0.1669(5) 0.6101(4) 0.0214(16) Uani 1 1 d . . . . .
C4 C 0.0223(11) -0.1671(13) 0.3768(16) 0.041(6) Uiso 0.5 1 d D . P A 1
O5 O 0.5105(4) 0.0749(4) 0.5925(4) 0.0164(14) Uani 1 1 d . . . . .
C5 C -0.0481(12) -0.1053(12) 0.3958(15) 0.033(6) Uiso 0.5 1 d D . P A 1
H5 H -0.0324 -0.0395 0.4192 0.039 Uiso 0.5 1 calc R U P A 1
O6 O 0.3305(8) 0.2773(7) 1.1659(5) 0.060(3) Uani 1 1 d . . . . .
H6H H 0.3083 0.2284 1.1677 0.072 Uiso 1 1 calc R U . . .
C6 C -0.1421(12) -0.1420(13) 0.380(2) 0.021(7) Uiso 0.5 1 d D . P A 1
H6 H -0.1918 -0.1027 0.3850 0.025 Uiso 0.5 1 calc R U P A 1
O7 O 0.4906(5) 0.0715(5) 0.2929(5) 0.0251(16) Uani 1 1 d . . . . .
C7 C -0.1626(12) -0.2365(13) 0.3558(17) 0.012(7) Uiso 0.5 1 d D . P A 1
O8 O 0.4889(6) 0.2170(6) 0.3124(5) 0.0373(19) Uani 1 1 d . . . . .
C8 C -0.0917(13) -0.2972(12) 0.3373(17) 0.041(6) Uiso 0.5 1 d D . P A 1
H8 H -0.1069 -0.3629 0.3152 0.050 Uiso 0.5 1 calc R U P A 1
O9 O 0.7897(5) 0.0324(7) -0.1622(5) 0.042(2) Uani 1 1 d . . . . .
H9 H 0.7590 0.0298 -0.2097 0.051 Uiso 1 1 calc R U . . .
C9 C 0.0009(12) -0.2611(13) 0.3514(16) 0.047(6) Uiso 0.5 1 d D . P A 1
H9A H 0.0505 -0.3012 0.3435 0.057 Uiso 0.5 1 calc R U P A 1
O10 O 0.3413(4) 0.1979(5) 0.4309(4) 0.0217(15) Uani 1 1 d . . . . .
C10 C 0.4512(6) 0.1274(7) 0.6430(6) 0.018(2) Uani 1 1 d . . . . .
O11 O 0.2963(5) 0.2849(5) 0.3642(5) 0.0334(19) Uani 1 1 d . . . . .
C11 C 0.4504(7) 0.1456(8) 0.7435(7) 0.028(3) Uani 1 1 d . . . . .
H11A H 0.5144 0.1719 0.7760 0.034 Uiso 1 1 calc R U . . .
H11B H 0.4364 0.0849 0.7448 0.034 Uiso 1 1 calc R U . . .
O12 O -0.2834(5) 0.1853(5) 0.3728(6) 0.0346(19) Uani 1 1 d . . . . .
H12 H -0.3082 0.2363 0.3880 0.041 Uiso 1 1 calc R U . . .
C12 C 0.3782(9) 0.2136(10) 0.7969(8) 0.047(3) Uani 1 1 d . . . . .
H12A H 0.3943 0.2752 0.7980 0.056 Uiso 1 1 calc R U . . .
H12B H 0.3149 0.1888 0.7623 0.056 Uiso 1 1 calc R U . . .
O13 O 0.5242(4) 0.2515(5) 0.5227(4) 0.0217(16) Uani 1 1 d . . . . .
C13 C 0.3727(8) 0.2292(11) 0.8962(8) 0.043(3) Uani 1 1 d . . . . .
O14 O 0.5491(4) 0.4037(5) 0.6122(4) 0.0229(16) Uani 1 1 d . . . . .
C14 C 0.3924(9) 0.3168(12) 0.9703(9) 0.054(4) Uani 1 1 d . . . . .
H14 H 0.4161 0.3682 0.9608 0.065 Uiso 1 1 calc R U . . .
O15 O 0.8835(6) 0.3144(7) 1.0105(6) 0.051(2) Uani 1 1 d . . . . .
H15H H 0.9375 0.3069 0.9911 0.061 Uiso 1 1 calc R U . . .
C15 C 0.3777(10) 0.3296(11) 1.0587(9) 0.056(4) Uani 1 1 d . . . . .
H15 H 0.3892 0.3912 1.1094 0.068 Uiso 1 1 calc R U . . .
O16 O 0.6401(5) 0.3464(5) 0.4332(5) 0.0304(18) Uani 1 1 d . . . . .
C16 C 0.3468(8) 0.2564(10) 1.0768(7) 0.043(3) Uani 1 1 d . . . . .
O17 O 0.5927(4) 0.4873(5) 0.4855(5) 0.0221(16) Uani 1 1 d . . . . .
C17 C 0.3288(9) 0.1648(10) 1.0012(8) 0.047(3) Uani 1 1 d . . . . .
H17 H 0.3090 0.1121 1.0105 0.057 Uiso 1 1 calc R U . . .
O18 O 1.1404(6) 0.6072(8) 0.8047(6) 0.066(3) Uani 1 1 d . . . . .
H18H H 1.1339 0.6333 0.8623 0.079 Uiso 1 1 calc R U . . .
C18 C 0.3417(9) 0.1553(10) 0.9106(7) 0.049(4) Uani 1 1 d . . . . .
H18 H 0.3282 0.0951 0.8581 0.058 Uiso 1 1 calc R U . . .
C19 C 0.5065(6) 0.1333(7) 0.2667(6) 0.018(2) Uani 1 1 d . . . . .
C20 C 0.5526(8) 0.1054(8) 0.1770(7) 0.030(3) Uani 1 1 d . . . . .
H20A H 0.5060 0.0648 0.1237 0.036 Uiso 1 1 calc R U . . .
H20B H 0.6060 0.0677 0.1766 0.036 Uiso 1 1 calc R U . . .
C21 C 0.5892(8) 0.1890(8) 0.1631(7) 0.031(3) Uani 1 1 d . . . . .
H21A H 0.5354 0.2233 0.1563 0.037 Uiso 1 1 calc R U . . .
H21B H 0.6318 0.2330 0.2184 0.037 Uiso 1 1 calc R U . . .
C22 C 0.6419(7) 0.1548(8) 0.0770(7) 0.028(3) Uani 1 1 d . . . . .
C23 C 0.5961(7) 0.1275(8) -0.0116(7) 0.028(3) Uani 1 1 d . . . . .
H23 H 0.5310 0.1369 -0.0177 0.034 Uiso 1 1 calc R U . . .
C24 C 0.6453(7) 0.0863(8) -0.0922(7) 0.026(2) Uani 1 1 d . . . . .
H24 H 0.6127 0.0674 -0.1520 0.031 Uiso 1 1 calc R U . . .
C25 C 0.7374(8) 0.0733(9) -0.0856(7) 0.031(3) Uani 1 1 d . . . . .
C26 C 0.7891(8) 0.1024(10) 0.0022(8) 0.043(3) Uani 1 1 d . . . . .
H26 H 0.8549 0.0951 0.0068 0.052 Uiso 1 1 calc R U . . .
C27 C 0.7404(8) 0.1417(10) 0.0806(8) 0.044(3) Uani 1 1 d . . . . .
H27 H 0.7742 0.1612 0.1400 0.053 Uiso 1 1 calc R U . . .
C28 C 0.2780(7) 0.2249(8) 0.3915(7) 0.028(3) Uani 1 1 d . . . . .
C33 C -0.1309(10) 0.1671(11) 0.4323(12) 0.030(4) Uani 0.7 1 d . U P C 1
H33 H -0.1609 0.1344 0.4616 0.036 Uiso 0.7 1 calc R U P C 1
C32 C -0.0318(13) 0.1858(14) 0.4427(14) 0.050(5) Uani 0.7 1 d . U P C 1
H32 H 0.0072 0.1617 0.4755 0.060 Uiso 0.7 1 calc R U P C 1
C37 C 0.5610(7) 0.3222(8) 0.5986(7) 0.025(2) Uani 1 1 d . . . . .
C38 C 0.6234(7) 0.3049(8) 0.6668(6) 0.024(2) Uani 1 1 d . . . . .
H38A H 0.6868 0.2925 0.6438 0.028 Uiso 1 1 calc R U . . .
H38B H 0.5968 0.2476 0.6693 0.028 Uiso 1 1 calc R U . . .
C39 C 0.6342(8) 0.3866(8) 0.7654(7) 0.034(3) Uani 1 1 d . . . . .
H39A H 0.6589 0.4445 0.7631 0.041 Uiso 1 1 calc R U . . .
H39B H 0.5713 0.3974 0.7899 0.041 Uiso 1 1 calc R U . . .
C40 C 0.6998(7) 0.3680(8) 0.8304(6) 0.027(2) Uani 1 1 d . . . . .
C41 C 0.6682(8) 0.3411(9) 0.8939(7) 0.038(3) Uani 1 1 d . . . . .
H41 H 0.6019 0.3343 0.8971 0.045 Uiso 1 1 calc R U . . .
C42 C 0.7282(8) 0.3232(9) 0.9541(8) 0.041(3) Uani 1 1 d . . . . .
H42 H 0.7029 0.3058 0.9980 0.049 Uiso 1 1 calc R U . . .
C43 C 0.8230(8) 0.3307(9) 0.9500(7) 0.035(3) Uani 1 1 d . . . . .
C44 C 0.8597(8) 0.3581(9) 0.8863(7) 0.040(3) Uani 1 1 d . . . . .
H44 H 0.9261 0.3631 0.8824 0.048 Uiso 1 1 calc R U . . .
C45 C 0.7965(7) 0.3780(9) 0.8283(8) 0.035(3) Uani 1 1 d . . . . .
H45 H 0.8210 0.3989 0.7866 0.042 Uiso 1 1 calc R U . . .
C46 C 0.6588(7) 0.4334(8) 0.4758(7) 0.024(2) Uani 1 1 d . . . . .
C47 C 0.7572(7) 0.4758(8) 0.5177(8) 0.028(2) Uani 1 1 d . . . . .
H47A H 0.7590 0.5454 0.5453 0.033 Uiso 1 1 calc R U . . .
H47B H 0.8014 0.4539 0.4683 0.033 Uiso 1 1 calc R U . . .
C48 C 0.7879(8) 0.4476(9) 0.5927(8) 0.040(3) Uani 1 1 d . . . . .
H48A H 0.7382 0.4621 0.6366 0.048 Uiso 1 1 calc R U . . .
H48B H 0.7914 0.3785 0.5626 0.048 Uiso 1 1 calc R U . . .
C49 C 0.8795(8) 0.4930(8) 0.6476(7) 0.034(3) Uani 1 1 d . . . . .
C50 C 0.9645(8) 0.4652(8) 0.6106(8) 0.039(3) Uani 1 1 d . . . . .
H50 H 0.9640 0.4175 0.5479 0.046 Uiso 1 1 calc R U . . .
C51 C 1.0507(9) 0.5055(10) 0.6633(9) 0.051(4) Uani 1 1 d . . . . .
H51 H 1.1084 0.4875 0.6357 0.061 Uiso 1 1 calc R U . . .
C52 C 1.0520(9) 0.5708(10) 0.7545(8) 0.046(3) Uani 1 1 d . . . . .
C53 C 0.9702(8) 0.6021(9) 0.7940(8) 0.043(3) Uani 1 1 d . . . . .
H53 H 0.9713 0.6497 0.8568 0.052 Uiso 1 1 calc R U . . .
C54 C 0.8857(8) 0.5625(9) 0.7396(8) 0.041(3) Uani 1 1 d . . . . .
H54 H 0.8285 0.5842 0.7667 0.049 Uiso 1 1 calc R U . . .
O1Z O 0.6219(4) 0.0757(5) 0.4346(5) 0.0265(17) Uani 1 1 d . . . . .
H1Z1 H 0.6507 0.0695 0.3805 0.032 Uiso 1 1 calc R U . . .
H1Z2 H 0.6596 0.0778 0.4864 0.032 Uiso 1 1 calc R U . . .
O2Z O 0.3360(5) 0.3838(5) 0.5741(4) 0.0264(17) Uani 1 1 d . . . . .
H2Z1 H 0.2923 0.3343 0.5690 0.032 Uiso 1 1 calc R U . . .
H2Z2 H 0.3358 0.4452 0.6247 0.032 Uiso 1 1 calc R U . . .
O3Z O 0.4432(7) 0.4008(6) 0.3210(5) 0.053(3) Uani 1 1 d . . . . .
H3Z1 H 0.4538 0.3575 0.2589 0.063 Uiso 1 1 calc R U . . .
H3Z2 H 0.4279 0.4627 0.3347 0.063 Uiso 1 1 calc R U . . .
C104 C 0.0090(10) -0.1274(10) 0.3481(10) 0.007(3) Uiso 0.5 1 d D . P A 2
C109 C 0.0012(12) -0.2264(12) 0.3142(12) 0.022(4) Uiso 0.5 1 d D . P A 2
H109 H 0.0544 -0.2609 0.2913 0.026 Uiso 0.5 1 calc R U P A 2
C102 C 0.1903(14) -0.1192(16) 0.3366(14) 0.017(5) Uiso 0.5 1 d . . P A 2
H10C H 0.1962 -0.1561 0.3720 0.021 Uiso 0.5 1 calc R U P A 2
H10D H 0.1926 -0.1622 0.2694 0.021 Uiso 0.5 1 calc R U P A 2
C3 C 0.1308(18) -0.125(2) 0.4038(18) 0.051(7) Uiso 0.5 1 d . . P A 1
H3A H 0.1377 -0.0731 0.4684 0.061 Uiso 0.5 1 calc R U P A 1
H3B H 0.1703 -0.1750 0.4027 0.061 Uiso 0.5 1 calc R U P A 1
C105 C -0.0715(12) -0.0786(16) 0.3816(14) 0.029(5) Uiso 0.5 1 d D . P A 2
H105 H -0.0684 -0.0129 0.4003 0.035 Uiso 0.5 1 calc R U P A 2
C106 C -0.1562(18) -0.1240(19) 0.388(2) 0.039(9) Uiso 0.5 1 d D . P A 2
H106 H -0.2063 -0.0885 0.4193 0.047 Uiso 0.5 1 calc R U P A 2
C107 C -0.1647(16) -0.2239(17) 0.348(2) 0.027(9) Uiso 0.5 1 d D . P A 2
C108 C -0.0851(11) -0.2741(14) 0.3140(12) 0.017(4) Uiso 0.5 1 d D . P A 2
H108 H -0.0896 -0.3406 0.2910 0.020 Uiso 0.5 1 calc R U P A 2
C31 C 0.0086(10) 0.2410(10) 0.4037(11) 0.027(4) Uani 0.7 1 d . U P C 1
C30 C 0.1133(10) 0.2703(12) 0.4281(14) 0.040(4) Uani 0.7 1 d . U P C 1
H30A H 0.1267 0.3012 0.4970 0.048 Uiso 0.7 1 calc R U P C 1
H30B H 0.1306 0.3174 0.4062 0.048 Uiso 0.7 1 calc R U P C 1
C36 C -0.0506(8) 0.2762(8) 0.3508(8) 0.049(3) Uani 1 1 d D . . . .
H36 H -0.0239 0.3075 0.3185 0.058 Uiso 1 1 calc R U . C 1
C35 C -0.1462(7) 0.2618(7) 0.3504(7) 0.030(3) Uani 1 1 d D . . . .
H35 H -0.1857 0.2982 0.3323 0.037 Uiso 1 1 calc R U . . .
C34 C -0.1871(7) 0.2004(8) 0.3735(8) 0.033(3) Uani 1 1 d D U . . .
C29 C 0.1752(8) 0.1889(10) 0.3858(11) 0.065(13) Uani 0.7 1 d . . P C 1
H29A H 0.1517 0.1481 0.3196 0.078 Uiso 0.7 1 calc R U P C 1
H29B H 0.1713 0.1504 0.4196 0.078 Uiso 0.7 1 calc R U P C 1
C233 C -0.1291(15) 0.1344(19) 0.374(3) 0.050(7) Uiso 0.3 1 d D . P C 2
H233 H -0.1564 0.0751 0.3650 0.060 Uiso 0.3 1 calc R U P C 2
C230 C 0.1183(13) 0.245(2) 0.380(3) 0.039(11) Uiso 0.3 1 d D . P C 2
H23A H 0.1378 0.2601 0.3297 0.047 Uiso 0.3 1 calc R U P C 2
H23B H 0.1281 0.3039 0.4390 0.047 Uiso 0.3 1 calc R U P C 2
C232 C -0.0309(13) 0.152(2) 0.386(3) 0.050(7) Uiso 0.3 1 d D . P C 2
H232 H 0.0072 0.1216 0.4130 0.060 Uiso 0.3 1 calc R U P C 2
C231 C 0.0099(13) 0.216(2) 0.360(3) 0.050(7) Uiso 0.3 1 d D . P C 2
C229 C 0.1752(8) 0.1889(10) 0.3858(11) 0.038(18) Uiso 0.3 1 d . . P C 2
H22A H 0.1621 0.1264 0.3306 0.046 Uiso 0.3 1 calc R U P C 2
H22B H 0.1650 0.1810 0.4422 0.046 Uiso 0.3 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O1 2.621(6) . ?
Ce1 O2 2.572(6) . ?
Ce1 O4 2.609(6) . ?
Ce1 O5 2.501(6) 2_656 ?
Ce1 O5 2.650(6) . ?
Ce1 O7 2.405(6) . ?
Ce1 O10 2.425(6) . ?
Ce1 O13 2.510(6) . ?
Ce1 O1Z 2.517(7) . ?
O1 C1 1.281(12) . ?
C1 O2 1.273(11) . ?
C1 C2 1.51(3) . ?
C1 C102 1.48(2) . ?
Ce2 O8 2.371(8) . ?
Ce2 O10 2.757(7) . ?
Ce2 O11 2.494(7) . ?
Ce2 O13 2.563(6) . ?
Ce2 O14 2.610(5) . ?
Ce2 O16 2.646(7) . ?
Ce2 O17 2.671(6) . ?
Ce2 O17 2.459(7) 2_666 ?
Ce2 O2Z 2.598(7) . ?
Ce2 O3Z 2.529(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.54(4) . ?
O3 H3 0.8400 . ?
O3 C7 1.303(17) . ?
O3 C107 1.40(3) . ?
C103 H10A 0.9900 . ?
C103 H10B 0.9900 . ?
C103 C104 1.48(3) . ?
C103 C102 1.53(3) . ?
O4 C10 1.273(11) . ?
C4 C5 1.389(16) . ?
C4 C9 1.377(16) . ?
C4 C3 1.60(3) . ?
O5 Ce1 2.501(6) 2_656 ?
O5 C10 1.269(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(15) . ?
O6 H6H 0.8400 . ?
O6 C16 1.355(13) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(16) . ?
O7 C19 1.253(12) . ?
C7 C8 1.383(15) . ?
O8 C19 1.247(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.373(15) . ?
O9 H9 0.8400 . ?
O9 C25 1.389(13) . ?
C9 H9A 0.9500 . ?
O10 C28 1.271(11) . ?
C10 C11 1.511(13) . ?
O11 C28 1.243(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.530(15) . ?
O12 H12 0.8400 . ?
O12 C34 1.375(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.511(15) . ?
O13 C37 1.288(12) . ?
C13 C14 1.366(19) . ?
C13 C18 1.359(19) . ?
O14 C37 1.239(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.375(17) . ?
O15 H15H 0.8400 . ?
O15 C43 1.382(12) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(19) . ?
O16 C46 1.243(13) . ?
C16 C17 1.414(17) . ?
O17 Ce2 2.459(7) 2_666 ?
O17 C46 1.273(12) . ?
C17 H17 0.9500 . ?
C17 C18 1.421(16) . ?
O18 H18H 0.8400 . ?
O18 C52 1.395(14) . ?
C18 H18 0.9500 . ?
C19 C20 1.507(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.521(14) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.504(15) . ?
C22 C23 1.397(13) . ?
C22 C27 1.426(15) . ?
C23 H23 0.9500 . ?
C23 C24 1.409(14) . ?
C24 H24 0.9500 . ?
C24 C25 1.340(15) . ?
C25 C26 1.414(14) . ?
C26 H26 0.9500 . ?
C26 C27 1.378(16) . ?
C27 H27 0.9500 . ?
C28 C29 1.524(16) . ?
C28 C229 1.524(16) . ?
C33 H33 0.9500 . ?
C33 C32 1.41(2) . ?
C33 C34 1.490(18) . ?
C32 H32 0.9500 . ?
C32 C31 1.41(2) . ?
C37 C38 1.500(12) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.524(14) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.498(13) . ?
C40 C41 1.365(14) . ?
C40 C45 1.379(14) . ?
C41 H41 0.9500 . ?
C41 C42 1.386(14) . ?
C42 H42 0.9500 . ?
C42 C43 1.354(16) . ?
C43 C44 1.400(16) . ?
C44 H44 0.9500 . ?
C44 C45 1.405(14) . ?
C45 H45 0.9500 . ?
C46 C47 1.499(13) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.516(14) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.479(14) . ?
C49 C50 1.382(17) . ?
C49 C54 1.386(16) . ?
C50 H50 0.9500 . ?
C50 C51 1.391(16) . ?
C51 H51 0.9500 . ?
C51 C52 1.363(17) . ?
C52 C53 1.365(17) . ?
C53 H53 0.9500 . ?
C53 C54 1.380(15) . ?
C54 H54 0.9500 . ?
O1Z H1Z1 0.9500 . ?
O1Z H1Z2 0.9500 . ?
O2Z H2Z1 0.9500 . ?
O2Z H2Z2 0.9500 . ?
O3Z H3Z1 0.9500 . ?
O3Z H3Z2 0.9500 . ?
C104 C109 1.415(16) . ?
C104 C105 1.408(17) . ?
C109 H109 0.9500 . ?
C109 C108 1.409(16) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C105 H105 0.9500 . ?
C105 C106 1.408(18) . ?
C106 H106 0.9500 . ?
C106 C107 1.419(18) . ?
C107 C108 1.410(17) . ?
C108 H108 0.9500 . ?
C31 C30 1.51(2) . ?
C31 C36 1.464(19) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C29 1.52(2) . ?
C36 H36 0.9500 . ?
C36 C35 1.365(14) . ?
C36 C231 1.371(13) . ?
C35 H35 0.9500 . ?
C35 C34 1.317(15) . ?
C34 C233 1.371(18) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C233 H233 0.9500 . ?
C233 C232 1.393(17) . ?
C230 H23A 0.9900 . ?
C230 H23B 0.9900 . ?
C230 C231 1.56(2) . ?
C230 C229 1.26(3) . ?
C232 H232 0.9500 . ?
C232 C231 1.384(13) . ?
C229 H22A 0.9900 . ?
C229 H22B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ce1 O5 128.4(2) . . ?
O2 Ce1 O1 50.1(2) . . ?
O2 Ce1 O4 69.7(2) . . ?
O2 Ce1 O5 81.58(18) . . ?
O4 Ce1 O1 113.5(2) . . ?
O4 Ce1 O5 49.58(19) . . ?
O5 Ce1 O1 79.2(2) 2_656 . ?
O5 Ce1 O2 70.5(2) 2_656 . ?
O5 Ce1 O4 107.6(2) 2_656 . ?
O5 Ce1 O5 66.8(2) 2_656 . ?
O5 Ce1 O13 136.82(19) 2_656 . ?
O5 Ce1 O1Z 68.7(2) 2_656 . ?
O7 Ce1 O1 73.4(2) . . ?
O7 Ce1 O2 122.8(2) . . ?
O7 Ce1 O4 158.6(2) . . ?
O7 Ce1 O5 93.4(2) . 2_656 ?
O7 Ce1 O5 142.8(2) . . ?
O7 Ce1 O10 84.0(2) . . ?
O7 Ce1 O13 90.6(2) . . ?
O7 Ce1 O1Z 70.3(2) . . ?
O10 Ce1 O1 75.3(2) . . ?
O10 Ce1 O2 89.2(2) . . ?
O10 Ce1 O4 78.7(2) . . ?
O10 Ce1 O5 127.5(2) . . ?
O10 Ce1 O5 154.1(2) . 2_656 ?
O10 Ce1 O13 69.1(2) . . ?
O10 Ce1 O1Z 133.0(2) . . ?
O13 Ce1 O1 142.3(2) . . ?
O13 Ce1 O2 138.5(2) . . ?
O13 Ce1 O4 71.6(2) . . ?
O13 Ce1 O5 84.60(19) . . ?
O13 Ce1 O1Z 72.5(2) . . ?
O1Z Ce1 O1 129.0(2) . . ?
O1Z Ce1 O2 137.8(2) . . ?
O1Z Ce1 O4 113.44(19) . . ?
O1Z Ce1 O5 73.1(2) . . ?
C1 O1 Ce1 94.1(5) . . ?
O1 C1 C2 116.3(12) . . ?
O1 C1 C102 122.5(11) . . ?
O2 C1 O1 119.1(8) . . ?
O2 C1 C2 122.7(13) . . ?
O2 C1 C102 117.5(12) . . ?
O8 Ce2 O10 71.5(2) . . ?
O8 Ce2 O11 76.6(3) . . ?
O8 Ce2 O13 80.1(2) . . ?
O8 Ce2 O14 122.9(2) . . ?
O8 Ce2 O16 68.8(2) . . ?
O8 Ce2 O17 145.8(2) . 2_666 ?
O8 Ce2 O17 107.4(2) . . ?
O8 Ce2 O2Z 135.0(2) . . ?
O8 Ce2 O3Z 74.8(3) . . ?
O11 Ce2 O10 49.2(2) . . ?
O11 Ce2 O13 112.5(2) . . ?
O11 Ce2 O14 141.4(2) . . ?
O11 Ce2 O16 144.2(2) . . ?
O11 Ce2 O17 142.5(2) . . ?
O11 Ce2 O2Z 72.6(2) . . ?
O11 Ce2 O3Z 74.3(3) . . ?
O13 Ce2 O10 63.38(18) . . ?
O13 Ce2 O14 50.1(2) . . ?
O13 Ce2 O16 70.7(2) . . ?
O13 Ce2 O17 104.82(19) . . ?
O13 Ce2 O2Z 82.3(2) . . ?
O14 Ce2 O10 101.80(19) . . ?
O14 Ce2 O16 69.6(2) . . ?
O14 Ce2 O17 68.6(2) . . ?
O16 Ce2 O10 122.9(2) . . ?
O16 Ce2 O17 48.2(2) . . ?
O17 Ce2 O10 123.8(2) 2_666 . ?
O17 Ce2 O10 168.19(18) . . ?
O17 Ce2 O11 91.5(2) 2_666 . ?
O17 Ce2 O13 133.6(2) 2_666 . ?
O17 Ce2 O14 86.2(2) 2_666 . ?
O17 Ce2 O16 112.1(2) 2_666 . ?
O17 Ce2 O17 63.9(2) 2_666 . ?
O17 Ce2 O2Z 67.3(2) 2_666 . ?
O17 Ce2 O3Z 71.1(3) 2_666 . ?
O2Z Ce2 O10 63.6(2) . . ?
O2Z Ce2 O14 71.0(2) . . ?
O2Z Ce2 O16 140.5(2) . . ?
O2Z Ce2 O17 117.1(2) . . ?
O3Z Ce2 O10 118.9(2) . . ?
O3Z Ce2 O13 151.7(3) . . ?
O3Z Ce2 O14 139.3(2) . . ?
O3Z Ce2 O16 87.8(3) . . ?
O3Z Ce2 O17 71.1(2) . . ?
O3Z Ce2 O2Z 125.1(3) . . ?
C1 O2 Ce1 96.6(6) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C1 C2 C3 111.2(19) . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C7 O3 H3 109.5 . . ?
H10A C103 H10B 107.1 . . ?
C104 C103 H10A 107.6 . . ?
C104 C103 H10B 107.6 . . ?
C104 C103 C102 118.8(18) . . ?
C102 C103 H10A 107.6 . . ?
C102 C103 H10B 107.6 . . ?
C10 O4 Ce1 95.9(6) . . ?
C5 C4 C3 119.0(17) . . ?
C9 C4 C5 121.2(13) . . ?
C9 C4 C3 118.7(17) . . ?
Ce1 O5 Ce1 113.2(2) 2_656 . ?
C10 O5 Ce1 94.0(5) . . ?
C10 O5 Ce1 132.7(6) . 2_656 ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.4(13) . . ?
C6 C5 H5 120.8 . . ?
C16 O6 H6H 109.5 . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.5(13) . . ?
C7 C6 H6 120.3 . . ?
C19 O7 Ce1 130.2(7) . . ?
O3 C7 C6 123.1(15) . . ?
O3 C7 C8 115.8(15) . . ?
C8 C7 C6 121.1(13) . . ?
C19 O8 Ce2 154.5(7) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.0(13) . . ?
C9 C8 H8 120.5 . . ?
C25 O9 H9 109.5 . . ?
C4 C9 H9A 119.9 . . ?
C8 C9 C4 120.3(13) . . ?
C8 C9 H9A 119.8 . . ?
Ce1 O10 Ce2 106.4(2) . . ?
C28 O10 Ce1 154.8(7) . . ?
C28 O10 Ce2 86.8(6) . . ?
O4 C10 C11 120.2(9) . . ?
O5 C10 O4 120.4(8) . . ?
O5 C10 C11 119.4(8) . . ?
C28 O11 Ce2 99.9(6) . . ?
C10 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
C10 C11 C12 113.6(9) . . ?
H11A C11 H11B 107.7 . . ?
C12 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
C34 O12 H12 109.5 . . ?
C11 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 C11 114.6(9) . . ?
C13 C12 H12A 108.6 . . ?
C13 C12 H12B 108.6 . . ?
Ce1 O13 Ce2 109.9(2) . . ?
C37 O13 Ce1 149.6(6) . . ?
C37 O13 Ce2 95.4(5) . . ?
C14 C13 C12 121.2(13) . . ?
C18 C13 C12 118.5(12) . . ?
C18 C13 C14 120.1(12) . . ?
C37 O14 Ce2 94.4(6) . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.3(15) . . ?
C15 C14 H14 120.4 . . ?
C43 O15 H15H 109.5 . . ?
C14 C15 H15 118.7 . . ?
C14 C15 C16 122.7(14) . . ?
C16 C15 H15 118.7 . . ?
C46 O16 Ce2 95.5(6) . . ?
O6 C16 C15 117.9(11) . . ?
O6 C16 C17 123.3(13) . . ?
C15 C16 C17 118.7(11) . . ?
Ce2 O17 Ce2 116.1(2) 2_666 . ?
C46 O17 Ce2 93.5(6) . . ?
C46 O17 Ce2 148.0(6) . 2_666 ?
C16 C17 H17 121.6 . . ?
C16 C17 C18 116.8(13) . . ?
C18 C17 H17 121.6 . . ?
C52 O18 H18H 109.5 . . ?
C13 C18 C17 122.4(12) . . ?
C13 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
O7 C19 C20 118.0(9) . . ?
O8 C19 O7 123.3(9) . . ?
O8 C19 C20 118.7(9) . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C19 C20 C21 113.6(9) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 109.7 . . ?
C20 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C22 C21 C20 109.6(9) . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
C23 C22 C21 121.9(9) . . ?
C23 C22 C27 116.2(10) . . ?
C27 C22 C21 121.7(9) . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.7(10) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.9(9) . . ?
C25 C24 H24 119.6 . . ?
O9 C25 C26 114.9(9) . . ?
C24 C25 O9 123.7(9) . . ?
C24 C25 C26 121.4(10) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 C25 117.4(10) . . ?
C27 C26 H26 121.3 . . ?
C22 C27 H27 118.4 . . ?
C26 C27 C22 123.3(10) . . ?
C26 C27 H27 118.4 . . ?
O10 C28 C29 118.4(10) . . ?
O10 C28 C229 118.4(10) . . ?
O11 C28 O10 122.2(10) . . ?
O11 C28 C29 119.2(10) . . ?
O11 C28 C229 119.2(10) . . ?
C32 C33 H33 121.2 . . ?
C32 C33 C34 117.7(15) . . ?
C34 C33 H33 121.2 . . ?
C33 C32 H32 120.6 . . ?
C33 C32 C31 118.8(17) . . ?
C31 C32 H32 120.6 . . ?
O13 C37 C38 119.3(9) . . ?
O14 C37 O13 120.0(8) . . ?
O14 C37 C38 120.6(9) . . ?
C37 C38 H38A 108.8 . . ?
C37 C38 H38B 108.8 . . ?
C37 C38 C39 113.8(9) . . ?
H38A C38 H38B 107.7 . . ?
C39 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C38 C39 H39A 109.2 . . ?
C38 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 C38 112.1(9) . . ?
C40 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C41 C40 C39 122.7(10) . . ?
C41 C40 C45 116.9(9) . . ?
C45 C40 C39 120.4(10) . . ?
C40 C41 H41 118.4 . . ?
C40 C41 C42 123.3(10) . . ?
C42 C41 H41 118.4 . . ?
C41 C42 H42 120.2 . . ?
C43 C42 C41 119.5(10) . . ?
C43 C42 H42 120.2 . . ?
O15 C43 C44 120.0(10) . . ?
C42 C43 O15 120.0(10) . . ?
C42 C43 C44 119.9(10) . . ?
C43 C44 H44 120.7 . . ?
C43 C44 C45 118.6(10) . . ?
C45 C44 H44 120.7 . . ?
C40 C45 C44 121.7(11) . . ?
C40 C45 H45 119.1 . . ?
C44 C45 H45 119.1 . . ?
O16 C46 O17 119.4(9) . . ?
O16 C46 C47 121.2(10) . . ?
O17 C46 C47 119.4(10) . . ?
C46 C47 H47A 109.6 . . ?
C46 C47 H47B 109.6 . . ?
C46 C47 C48 110.3(9) . . ?
H47A C47 H47B 108.1 . . ?
C48 C47 H47A 109.6 . . ?
C48 C47 H47B 109.6 . . ?
C47 C48 H48A 108.2 . . ?
C47 C48 H48B 108.2 . . ?
H48A C48 H48B 107.4 . . ?
C49 C48 C47 116.2(9) . . ?
C49 C48 H48A 108.2 . . ?
C49 C48 H48B 108.2 . . ?
C50 C49 C48 121.3(11) . . ?
C50 C49 C54 116.1(10) . . ?
C54 C49 C48 122.6(12) . . ?
C49 C50 H50 119.3 . . ?
C49 C50 C51 121.4(11) . . ?
C51 C50 H50 119.3 . . ?
C50 C51 H51 120.1 . . ?
C52 C51 C50 119.8(13) . . ?
C52 C51 H51 120.1 . . ?
C51 C52 O18 117.4(12) . . ?
C51 C52 C53 121.1(11) . . ?
C53 C52 O18 121.5(11) . . ?
C52 C53 H53 121.1 . . ?
C52 C53 C54 117.9(11) . . ?
C54 C53 H53 121.1 . . ?
C49 C54 H54 118.2 . . ?
C53 C54 C49 123.7(12) . . ?
C53 C54 H54 118.2 . . ?
Ce1 O1Z H1Z1 120.0 . . ?
Ce1 O1Z H1Z2 120.0 . . ?
H1Z1 O1Z H1Z2 120.0 . . ?
Ce2 O2Z H2Z1 120.0 . . ?
Ce2 O2Z H2Z2 120.0 . . ?
H2Z1 O2Z H2Z2 120.0 . . ?
Ce2 O3Z H3Z1 120.0 . . ?
Ce2 O3Z H3Z2 120.0 . . ?
H3Z1 O3Z H3Z2 120.0 . . ?
C109 C104 C103 123.9(15) . . ?
C105 C104 C103 117.9(16) . . ?
C105 C104 C109 118.1(16) . . ?
C104 C109 H109 119.8 . . ?
C108 C109 C104 120.4(17) . . ?
C108 C109 H109 119.8 . . ?
C1 C102 C103 106.1(17) . . ?
C1 C102 H10C 110.5 . . ?
C1 C102 H10D 110.5 . . ?
C103 C102 H10C 110.5 . . ?
C103 C102 H10D 110.5 . . ?
H10C C102 H10D 108.7 . . ?
C2 C3 C4 113(2) . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C104 C105 H105 118.8 . . ?
C104 C105 C106 122(2) . . ?
C106 C105 H105 118.8 . . ?
C105 C106 H106 120.9 . . ?
C105 C106 C107 118(3) . . ?
C107 C106 H106 120.9 . . ?
O3 C107 C106 121.6(18) . . ?
O3 C107 C108 118.5(19) . . ?
C108 C107 C106 120(2) . . ?
C109 C108 C107 121(2) . . ?
C109 C108 H108 119.7 . . ?
C107 C108 H108 119.7 . . ?
C32 C31 C30 116.8(16) . . ?
C32 C31 C36 121.1(13) . . ?
C36 C31 C30 121.9(15) . . ?
C31 C30 H30A 108.8 . . ?
C31 C30 H30B 108.8 . . ?
C31 C30 C29 113.7(13) . . ?
H30A C30 H30B 107.7 . . ?
C29 C30 H30A 108.8 . . ?
C29 C30 H30B 108.8 . . ?
C31 C36 H36 121.8 . . ?
C35 C36 C31 116.4(11) . . ?
C35 C36 H36 121.8 . . ?
C35 C36 C231 121.5(12) . . ?
C36 C35 H35 118.0 . . ?
C34 C35 C36 123.9(10) . . ?
C34 C35 H35 118.0 . . ?
O12 C34 C33 113.6(10) . . ?
C35 C34 O12 124.2(10) . . ?
C35 C34 C33 119.2(10) . . ?
C35 C34 C233 113.7(13) . . ?
C233 C34 O12 119.9(13) . . ?
C28 C29 H29A 109.4 . . ?
C28 C29 H29B 109.4 . . ?
C30 C29 C28 111.0(11) . . ?
C30 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C34 C233 H233 119.3 . . ?
C34 C233 C232 121.5(18) . . ?
C232 C233 H233 119.3 . . ?
H23A C230 H23B 106.8 . . ?
C231 C230 H23A 107.2 . . ?
C231 C230 H23B 107.2 . . ?
C229 C230 H23A 107.2 . . ?
C229 C230 H23B 107.2 . . ?
C229 C230 C231 120(2) . . ?
C233 C232 H232 120.7 . . ?
C231 C232 C233 118.5(15) . . ?
C231 C232 H232 120.7 . . ?
C36 C231 C230 119.7(14) . . ?
C36 C231 C232 114.7(14) . . ?
C232 C231 C230 120.7(14) . . ?
C28 C229 H22A 109.3 . . ?
C28 C229 H22B 109.3 . . ?
C230 C229 C28 111.8(15) . . ?
C230 C229 H22A 109.3 . . ?
C230 C229 H22B 109.3 . . ?
H22A C229 H22B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce1 O1 C1 O2 1.8(11) . . . . ?
Ce1 O1 C1 C2 166.6(16) . . . . ?
Ce1 O1 C1 C102 -167.6(14) . . . . ?
Ce1 O4 C10 O5 4.6(9) . . . . ?
Ce1 O4 C10 C11 -177.6(8) . . . . ?
Ce1 O5 C10 O4 -131.5(7) 2_656 . . . ?
Ce1 O5 C10 O4 -4.5(8) . . . . ?
Ce1 O5 C10 C11 50.7(11) 2_656 . . . ?
Ce1 O5 C10 C11 177.7(8) . . . . ?
Ce1 O7 C19 O8 -10.2(13) . . . . ?
Ce1 O7 C19 C20 167.6(6) . . . . ?
Ce1 O10 C28 O11 -109.4(16) . . . . ?
Ce1 O10 C28 C29 76.4(19) . . . . ?
Ce1 O10 C28 C229 76.4(19) . . . . ?
Ce1 O13 C37 O14 -143.4(9) . . . . ?
Ce1 O13 C37 C38 40.6(17) . . . . ?
O1 C1 O2 Ce1 -1.8(11) . . . . ?
O1 C1 C2 C3 172.6(19) . . . . ?
O1 C1 C102 C103 -98.8(16) . . . . ?
C1 C2 C3 C4 175.3(19) . . . . ?
Ce2 O8 C19 O7 19(2) . . . . ?
Ce2 O8 C19 C20 -159.2(12) . . . . ?
Ce2 O10 C28 O11 13.6(10) . . . . ?
Ce2 O10 C28 C29 -160.6(10) . . . . ?
Ce2 O10 C28 C229 -160.6(10) . . . . ?
Ce2 O11 C28 O10 -15.3(11) . . . . ?
Ce2 O11 C28 C29 158.9(10) . . . . ?
Ce2 O11 C28 C229 158.9(10) . . . . ?
Ce2 O13 C37 O14 3.4(10) . . . . ?
Ce2 O13 C37 C38 -172.6(8) . . . . ?
Ce2 O14 C37 O13 -3.4(10) . . . . ?
Ce2 O14 C37 C38 172.6(8) . . . . ?
Ce2 O16 C46 O17 -18.8(10) . . . . ?
Ce2 O16 C46 C47 159.7(8) . . . . ?
Ce2 O17 C46 O16 177.4(7) 2_666 . . . ?
Ce2 O17 C46 O16 18.6(10) . . . . ?
Ce2 O17 C46 C47 -1.2(18) 2_666 . . . ?
Ce2 O17 C46 C47 -160.0(8) . . . . ?
O2 C1 C2 C3 -23(3) . . . . ?
O2 C1 C102 C103 91.7(17) . . . . ?
C2 C1 O2 Ce1 -165.7(17) . . . . ?
O3 C7 C8 C9 -175(2) . . . . ?
O3 C107 C108 C109 -178.7(18) . . . . ?
C103 C104 C109 C108 178.2(16) . . . . ?
C103 C104 C105 C106 -174(2) . . . . ?
O4 C10 C11 C12 -0.3(14) . . . . ?
C4 C5 C6 C7 7(4) . . . . ?
O5 C10 C11 C12 177.5(9) . . . . ?
C5 C4 C9 C8 5(4) . . . . ?
C5 C4 C3 C2 -74(3) . . . . ?
C5 C6 C7 O3 173(2) . . . . ?
C5 C6 C7 C8 -7(4) . . . . ?
O6 C16 C17 C18 174.7(12) . . . . ?
C6 C7 C8 C9 6(4) . . . . ?
O7 C19 C20 C21 -166.7(9) . . . . ?
C7 C8 C9 C4 -5(4) . . . . ?
O8 C19 C20 C21 11.2(13) . . . . ?
O9 C25 C26 C27 -178.7(11) . . . . ?
C9 C4 C5 C6 -6(4) . . . . ?
C9 C4 C3 C2 117(3) . . . . ?
O10 C28 C29 C30 124.9(14) . . . . ?
O10 C28 C229 C230 155(2) . . . . ?
C10 C11 C12 C13 177.2(11) . . . . ?
O11 C28 C29 C30 -49.5(18) . . . . ?
O11 C28 C229 C230 -20(3) . . . . ?
C11 C12 C13 C14 119.0(14) . . . . ?
C11 C12 C13 C18 -65.2(16) . . . . ?
O12 C34 C233 C232 -172(3) . . . . ?
C12 C13 C14 C15 173.7(12) . . . . ?
C12 C13 C18 C17 -176.1(11) . . . . ?
O13 C37 C38 C39 -159.8(9) . . . . ?
C13 C14 C15 C16 2(2) . . . . ?
O14 C37 C38 C39 24.2(14) . . . . ?
C14 C13 C18 C17 -0.2(19) . . . . ?
C14 C15 C16 O6 -177.1(13) . . . . ?
C14 C15 C16 C17 -1(2) . . . . ?
O15 C43 C44 C45 -177.4(11) . . . . ?
C15 C16 C17 C18 -1.6(18) . . . . ?
O16 C46 C47 C48 -62.5(14) . . . . ?
C16 C17 C18 C13 2.1(18) . . . . ?
O17 C46 C47 C48 116.0(11) . . . . ?
O18 C52 C53 C54 -180.0(12) . . . . ?
C18 C13 C14 C15 -2.0(19) . . . . ?
C19 C20 C21 C22 174.5(8) . . . . ?
C20 C21 C22 C23 87.6(13) . . . . ?
C20 C21 C22 C27 -87.7(13) . . . . ?
C21 C22 C23 C24 -173.2(10) . . . . ?
C21 C22 C27 C26 173.8(12) . . . . ?
C22 C23 C24 C25 -0.8(17) . . . . ?
C23 C22 C27 C26 -1.7(19) . . . . ?
C23 C24 C25 O9 179.4(10) . . . . ?
C23 C24 C25 C26 -1.5(18) . . . . ?
C24 C25 C26 C27 2.2(19) . . . . ?
C25 C26 C27 C22 0(2) . . . . ?
C27 C22 C23 C24 2.3(16) . . . . ?
C33 C32 C31 C30 171.8(16) . . . . ?
C33 C32 C31 C36 -2(3) . . . . ?
C32 C33 C34 O12 -175.4(14) . . . . ?
C32 C33 C34 C35 -14(2) . . . . ?
C32 C31 C30 C29 69(2) . . . . ?
C32 C31 C36 C35 7(2) . . . . ?
C37 C38 C39 C40 -177.9(9) . . . . ?
C38 C39 C40 C41 -102.2(13) . . . . ?
C38 C39 C40 C45 78.0(13) . . . . ?
C39 C40 C41 C42 179.6(12) . . . . ?
C39 C40 C45 C44 -177.9(11) . . . . ?
C40 C41 C42 C43 -1(2) . . . . ?
C41 C40 C45 C44 2.3(18) . . . . ?
C41 C42 C43 O15 179.1(12) . . . . ?
C41 C42 C43 C44 1(2) . . . . ?
C42 C43 C44 C45 0.5(19) . . . . ?
C43 C44 C45 C40 -2.3(19) . . . . ?
C45 C40 C41 C42 -0.6(19) . . . . ?
C46 C47 C48 C49 -173.4(11) . . . . ?
C47 C48 C49 C50 -76.0(15) . . . . ?
C47 C48 C49 C54 106.7(13) . . . . ?
C48 C49 C50 C51 -177.7(11) . . . . ?
C48 C49 C54 C53 176.2(12) . . . . ?
C49 C50 C51 C52 3(2) . . . . ?
C50 C49 C54 C53 -1.3(17) . . . . ?
C50 C51 C52 O18 178.4(12) . . . . ?
C50 C51 C52 C53 -4(2) . . . . ?
C51 C52 C53 C54 3(2) . . . . ?
C52 C53 C54 C49 0(2) . . . . ?
C54 C49 C50 C51 -0.2(17) . . . . ?
C104 C103 C102 C1 -165.7(15) . . . . ?
C104 C109 C108 C107 0(3) . . . . ?
C104 C105 C106 C107 -9(4) . . . . ?
C109 C104 C105 C106 5(3) . . . . ?
C102 C1 O2 Ce1 168.1(12) . . . . ?
C102 C103 C104 C109 -11(3) . . . . ?
C102 C103 C104 C105 167.5(17) . . . . ?
C3 C4 C5 C6 -174(2) . . . . ?
C3 C4 C9 C8 173(2) . . . . ?
C105 C104 C109 C108 0(2) . . . . ?
C105 C106 C107 O3 -177(2) . . . . ?
C105 C106 C107 C108 9(4) . . . . ?
C106 C107 C108 C109 -5(4) . . . . ?
C31 C30 C29 C28 165.5(14) . . . . ?
C31 C36 C35 C34 -17.3(14) . . . . ?
C30 C31 C36 C35 -166.2(13) . . . . ?
C36 C31 C30 C29 -118.0(17) . . . . ?
C36 C35 C34 O12 -179.7(10) . . . . ?
C36 C35 C34 C33 21.1(14) . . . . ?
C36 C35 C34 C233 -16.8(19) . . . . ?
C35 C36 C231 C230 -168(2) . . . . ?
C35 C36 C231 C232 -12(4) . . . . ?
C35 C34 C233 C232 25(4) . . . . ?
C34 C33 C32 C31 5(2) . . . . ?
C34 C233 C232 C231 -27(5) . . . . ?
C233 C232 C231 C36 20(5) . . . . ?
C233 C232 C231 C230 175(3) . . . . ?
C231 C36 C35 C34 12(2) . . . . ?
C231 C230 C229 C28 172(3) . . . . ?
C229 C230 C231 C36 -178(3) . . . . ?
C229 C230 C231 C232 28(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
#=======================================================
#ALERT LEVEL B
_vrf_PLAT220                     
;
PROBLEM:Large Non-Solvent C Ueq(max)/Ueq(min) Range 9.6 Ratio
RESPONSE: Disordered fragments from 4-hydroxycinnamate ligands 
unstabilise the refinement.
;
_vrf_PLAT420                     
;
PROBLEMS: D-H Without Acceptor O2Z - H2Z2 .. Please Check;
D-H Without Acceptor O6 - H6H .. Please Check;
D-H Without Acceptor O15 - H15H .. Please Check
RESPONSE: The listed hydrogen bonds have been checked, but not found
;
#=======================================================
####################################################################### 
# 
# 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_compound6
_database_code_depnum_ccdc_archive 'CCDC 1055962'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_audit_creation_date             2015-05-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H31 Er O11'
_chemical_formula_sum            'C27 H31 Er O11'
_chemical_formula_weight         698.78
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   24.425(5)
_cell_length_b                   5.3513(11)
_cell_length_c                   22.945(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2999.0(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    30827
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.504
_cell_measurement_theta_min      1.775
_shelx_estimated_absorpt_T_max   0.932
_shelx_estimated_absorpt_T_min   0.330
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.9320
_exptl_absorpt_correction_T_min  0.3290
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_process_details   SORTAV
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.1229
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26496
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.775
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4452
_reflns_number_total             6590
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         1.774
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.97(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0627
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1337
_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.
 
 After refinement of the primary molecule including part of lattice solvent
 molecule, attempts to model the residual electron density in the lattice 
 voids as disordered solvents gave unsatisfactory refinements. Subsequently,
 the electron density in voids was accounted for using PLATON/SQUEEZE (see below). 
;
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 0.025 0.025 0.147 103 75
2 0.525 0.023 0.147 103 75
3 0.975 -0.067 0.647 103 75
4 0.475 -0.174 0.647 103 75
_platon_squeeze_details          
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.02838 0.97162
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C13-C18
 1.4 with sigma of 0.01
 C5-C6 = C7-C8 = C8-C9
 1.39 with sigma of 0.02
 C5-C6 \\sim C17-C18
 with sigma of 0.02
 C7-C8 \\sim C16-C17
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C3) = Uanis(C2)
Uanis(C21) = Uanis(C20)
Uanis(C23) = Uanis(C27)
Uanis(C17) = Uanis(C15)
Uanis(C19) = Uanis(C1)
Uanis(O8) = Uanis(O7)
Uanis(O1Z) = Uanis(O2Z)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27)
5.c X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6A), O9(H9A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.88118(2) 0.57259(10) 1.00108(5) 0.01798(17) Uani 1 1 d . . . . .
O1 O 0.9230(4) 0.5863(19) 0.9050(4) 0.026(3) Uani 1 1 d . . . . .
O1Z O 0.9044(4) 0.8129(19) 1.0837(4) 0.0222(17) Uani 1 1 d . . . . .
H1Z1 H 0.8911 0.9788 1.0875 0.027 Uiso 1 1 calc R . . . .
H1Z2 H 0.9272 0.7437 1.1132 0.027 Uiso 1 1 calc R . . . .
O2Z O 0.9595(3) 0.3250(16) 1.0112(4) 0.0222(17) Uani 1 1 d . . . . .
H2Z1 H 0.9929 0.3753 0.9935 0.027 Uiso 1 1 calc R . . . .
H2Z2 H 0.9579 0.1741 1.0329 0.027 Uiso 1 1 calc R . . . .
O3 O 1.2116(4) 0.6383(19) 1.0363(5) 0.030(3) Uani 1 1 d . . . . .
H3 H 1.2128 0.4816 1.0343 0.036 Uiso 1 1 calc GR . . . .
O4 O 0.7977(4) 0.5559(19) 1.0563(5) 0.026(2) Uani 1 1 d . . . . .
O5 O 0.8606(4) 0.2850(19) 1.0798(4) 0.021(2) Uani 1 1 d . . . . .
O6 O 0.5838(5) -0.122(2) 1.3000(5) 0.034(3) Uani 1 1 d . . . . .
H6A H 0.5852 -0.0517 1.3327 0.041 Uiso 1 1 calc GR . . . .
O7 O 0.8327(4) 0.302(2) 0.9474(5) 0.0275(18) Uani 1 1 d . . . . .
O8 O 0.8345(4) -0.1068(17) 0.9707(4) 0.0275(18) Uani 1 1 d . . . . .
C1 C 0.9561(5) 0.757(3) 0.9186(6) 0.019(2) Uani 1 1 d . . . . .
C2 C 0.9970(6) 0.845(3) 0.8737(6) 0.025(3) Uani 1 1 d . . . . .
H2A H 0.9764 0.9287 0.8420 0.030 Uiso 1 1 calc R . . . .
H2B H 1.0147 0.6959 0.8567 0.030 Uiso 1 1 calc R . . . .
C3 C 1.0431(6) 1.027(3) 0.8941(6) 0.025(3) Uani 1 1 d . U . . .
H3A H 1.0602 1.1029 0.8592 0.030 Uiso 1 1 calc R . . . .
H3B H 1.0263 1.1631 0.9171 0.030 Uiso 1 1 calc R . . . .
C4 C 1.0870(6) 0.907(3) 0.9300(7) 0.030(4) Uani 1 1 d . . . . .
C5 C 1.1357(6) 1.030(3) 0.9355(7) 0.028(4) Uani 1 1 d D . . . .
H5 H 1.1402 1.1839 0.9154 0.033 Uiso 1 1 calc R . . . .
C6 C 1.1776(6) 0.943(3) 0.9679(7) 0.032(4) Uani 1 1 d D . . . .
H6 H 1.2112 1.0329 0.9688 0.038 Uiso 1 1 calc R . . . .
C8 C 1.1242(5) 0.600(2) 0.9961(15) 0.032(5) Uani 1 1 d D . . . .
H8 H 1.1198 0.4485 1.0171 0.038 Uiso 1 1 calc R . . . .
C9 C 1.0824(6) 0.688(3) 0.9628(7) 0.034(4) Uani 1 1 d D . . . .
H9 H 1.0489 0.5979 0.9618 0.041 Uiso 1 1 calc R . . . .
C10 C 0.8135(6) 0.375(3) 1.0875(6) 0.021(4) Uani 1 1 d . . . . .
C11 C 0.7753(6) 0.263(3) 1.1319(7) 0.026(4) Uani 1 1 d . U . . .
H11A H 0.7919 0.2854 1.1709 0.031 Uiso 1 1 calc R . . . .
H11B H 0.7728 0.0814 1.1245 0.031 Uiso 1 1 calc R . . . .
C12 C 0.7180(6) 0.368(3) 1.1335(7) 0.029(4) Uani 1 1 d . U . . .
H12A H 0.7011 0.3496 1.0946 0.035 Uiso 1 1 calc R . . . .
H12B H 0.7198 0.5492 1.1425 0.035 Uiso 1 1 calc R . . . .
C13 C 0.6814(6) 0.238(3) 1.1793(6) 0.028(4) Uani 1 1 d D . . . .
C14 C 0.6541(8) 0.025(3) 1.1650(7) 0.036(5) Uani 1 1 d . U . . .
H14 H 0.6570 -0.0426 1.1268 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6219(8) -0.093(4) 1.2068(9) 0.027(3) Uani 1 1 d . . . . .
H15 H 0.6029 -0.2419 1.1966 0.032 Uiso 1 1 calc R . . . .
C16 C 0.6169(7) -0.001(4) 1.2623(9) 0.025(4) Uani 1 1 d D U . . .
C17 C 0.6448(7) 0.213(3) 1.2763(7) 0.027(3) Uani 1 1 d D U . . .
H17 H 0.6423 0.2799 1.3146 0.032 Uiso 1 1 calc R . . . .
C18 C 0.6759(7) 0.330(3) 1.2357(7) 0.032(5) Uani 1 1 d D . . . .
H18 H 0.6945 0.4789 1.2460 0.038 Uiso 1 1 calc R . . . .
C19 C 0.8177(5) 0.080(3) 0.9426(6) 0.019(2) Uani 1 1 d . . . . .
C20 C 0.7696(6) 0.028(3) 0.9015(6) 0.018(3) Uani 1 1 d . . . . .
H20A H 0.7354 0.0182 0.9247 0.021 Uiso 1 1 calc R . . . .
H20B H 0.7751 -0.1371 0.8827 0.021 Uiso 1 1 calc R . . . .
C21 C 0.7625(6) 0.229(3) 0.8533(7) 0.018(3) Uani 1 1 d . U . . .
H21A H 0.7572 0.3936 0.8723 0.021 Uiso 1 1 calc R . . . .
H21B H 0.7967 0.2381 0.8303 0.021 Uiso 1 1 calc R . . . .
C22 C 0.7151(7) 0.183(3) 0.8121(6) 0.021(3) Uani 1 1 d . . . . .
C23 C 0.7043(7) 0.341(3) 0.7669(7) 0.028(3) Uani 1 1 d . . . . .
H23 H 0.7279 0.4806 0.7619 0.033 Uiso 1 1 calc R . . . .
C24 C 0.6616(7) 0.314(3) 0.7277(7) 0.031(4) Uani 1 1 d . U . . .
H24 H 0.6562 0.4311 0.6971 0.037 Uiso 1 1 calc R . . . .
C25 C 0.6266(6) 0.109(3) 0.7349(8) 0.018(4) Uani 1 1 d . U . . .
C26 C 0.6340(8) -0.043(4) 0.7810(9) 0.036(6) Uani 1 1 d . . . . .
H26 H 0.6086 -0.1752 0.7873 0.043 Uiso 1 1 calc R . . . .
C27 C 0.6771(7) -0.015(3) 0.8194(8) 0.028(3) Uani 1 1 d . . . . .
H27 H 0.6812 -0.1280 0.8509 0.033 Uiso 1 1 calc R . . . .
O9 O 0.5839(4) 0.098(3) 0.6961(5) 0.044(4) Uani 1 1 d . . . . .
H9A H 0.5565 0.1706 0.7104 0.053 Uiso 1 1 calc GR . . . .
C7 C 1.1721(4) 0.726(2) 0.9997(10) 0.020(3) Uani 1 1 d D U . . .
O2 O 0.9543(4) 0.8561(16) 0.9689(4) 0.022(2) Uani 1 1 d . U . . .


_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
Er1 O1 2.430(10) . ?
Er1 O1Z 2.360(9) . ?
Er1 O2Z 2.338(8) . ?
Er1 O4 2.403(10) . ?
Er1 O5 2.426(9) . ?
Er1 O7 2.241(11) . ?
Er1 O8 2.174(10) 1_565 ?
Er1 O2 2.456(9) . ?
O1 C1 1.259(17) . ?
O1Z H1Z1 0.9500 . ?
O1Z H1Z2 0.9500 . ?
O2Z H2Z1 0.9500 . ?
O2Z H2Z2 0.9500 . ?
O3 H3 0.8400 . ?
O3 C7 1.362(18) . ?
O4 C10 1.267(17) . ?
O5 C10 1.259(17) . ?
O6 H6A 0.8400 . ?
O6 C16 1.35(2) . ?
O7 C19 1.247(17) . ?
O8 Er1 2.174(10) 1_545 ?
O8 C19 1.259(16) . ?
C1 C2 1.51(2) . ?
C1 O2 1.272(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.56(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.50(2) . ?
C4 C5 1.36(2) . ?
C4 C9 1.40(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.348(16) . ?
C6 H6 0.9500 . ?
C6 C7 1.38(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.36(2) . ?
C8 C7 1.350(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.50(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.51(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.55(2) . ?
C13 C14 1.36(2) . ?
C13 C18 1.390(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.39(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.37(3) . ?
C16 C17 1.373(19) . ?
C17 H17 0.9500 . ?
C17 C18 1.354(19) . ?
C18 H18 0.9500 . ?
C19 C20 1.534(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.55(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.52(2) . ?
C22 C23 1.37(2) . ?
C22 C27 1.42(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.38(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.40(2) . ?
C25 C26 1.35(3) . ?
C25 O9 1.373(19) . ?
C26 H26 0.9500 . ?
C26 C27 1.38(3) . ?
C27 H27 0.9500 . ?
O9 H9A 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Er1 O2 53.4(3) . . ?
O1Z Er1 O1 127.6(3) . . ?
O1Z Er1 O4 78.5(3) . . ?
O1Z Er1 O5 78.3(4) . . ?
O1Z Er1 O2 74.3(3) . . ?
O2Z Er1 O1 76.3(3) . . ?
O2Z Er1 O1Z 91.9(3) . . ?
O2Z Er1 O4 128.4(3) . . ?
O2Z Er1 O5 74.7(3) . . ?
O2Z Er1 O2 77.6(3) . . ?
O4 Er1 O1 146.7(3) . . ?
O4 Er1 O5 53.7(3) . . ?
O4 Er1 O2 143.0(3) . . ?
O5 Er1 O1 141.4(3) . . ?
O5 Er1 O2 140.0(3) . . ?
O7 Er1 O1 75.1(4) . . ?
O7 Er1 O1Z 157.1(4) . . ?
O7 Er1 O2Z 96.9(4) . . ?
O7 Er1 O4 79.5(4) . . ?
O7 Er1 O5 83.7(4) . . ?
O7 Er1 O2 128.2(4) . . ?
O8 Er1 O1 84.6(4) 1_565 . ?
O8 Er1 O1Z 87.3(4) 1_565 . ?
O8 Er1 O2Z 155.2(4) 1_565 . ?
O8 Er1 O4 75.7(4) 1_565 . ?
O8 Er1 O5 129.1(3) 1_565 . ?
O8 Er1 O7 93.3(4) 1_565 . ?
O8 Er1 O2 78.3(3) 1_565 . ?
C1 O1 Er1 93.9(9) . . ?
Er1 O1Z H1Z1 120.0 . . ?
Er1 O1Z H1Z2 120.0 . . ?
H1Z1 O1Z H1Z2 120.0 . . ?
Er1 O2Z H2Z1 120.0 . . ?
Er1 O2Z H2Z2 120.0 . . ?
H2Z1 O2Z H2Z2 120.0 . . ?
C7 O3 H3 109.5 . . ?
C10 O4 Er1 93.9(8) . . ?
C10 O5 Er1 93.0(9) . . ?
C16 O6 H6A 109.5 . . ?
C19 O7 Er1 145.0(10) . . ?
C19 O8 Er1 164.1(10) . 1_545 ?
O1 C1 C2 118.9(13) . . ?
O1 C1 O2 120.2(13) . . ?
O2 C1 C2 120.8(14) . . ?
C1 C2 H2A 107.8 . . ?
C1 C2 H2B 107.8 . . ?
C1 C2 C3 118.0(12) . . ?
H2A C2 H2B 107.2 . . ?
C3 C2 H2A 107.8 . . ?
C3 C2 H2B 107.8 . . ?
C2 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 C2 114.6(13) . . ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
C5 C4 C3 117.9(14) . . ?
C5 C4 C9 115.2(15) . . ?
C9 C4 C3 126.7(14) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 C4 123.2(15) . . ?
C6 C5 H5 118.4 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(14) . . ?
C7 C6 H6 119.8 . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.8(19) . . ?
C4 C9 H9 118.9 . . ?
C8 C9 C4 122.1(15) . . ?
C8 C9 H9 118.9 . . ?
O4 C10 C11 119.8(14) . . ?
O5 C10 O4 119.5(13) . . ?
O5 C10 C11 120.7(14) . . ?
C10 C11 H11A 108.2 . . ?
C10 C11 H11B 108.2 . . ?
C10 C11 C12 116.4(13) . . ?
H11A C11 H11B 107.3 . . ?
C12 C11 H11A 108.2 . . ?
C12 C11 H11B 108.2 . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C11 C12 C13 112.6(13) . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C14 C13 C12 119.8(13) . . ?
C14 C13 C18 118.3(15) . . ?
C18 C13 C12 121.9(15) . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.3(16) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.8(18) . . ?
C16 C15 H15 119.1 . . ?
O6 C16 C15 118.5(16) . . ?
O6 C16 C17 123.2(18) . . ?
C15 C16 C17 118.3(18) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.1(17) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 118.9 . . ?
C17 C18 C13 122.2(16) . . ?
C17 C18 H18 118.9 . . ?
O7 C19 O8 128.0(14) . . ?
O7 C19 C20 117.0(13) . . ?
O8 C19 C20 114.8(13) . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C19 C20 C21 113.3(12) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 108.6 . . ?
C20 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 C20 114.5(12) . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
C23 C22 C21 121.3(15) . . ?
C23 C22 C27 115.2(15) . . ?
C27 C22 C21 123.4(14) . . ?
C22 C23 H23 117.5 . . ?
C22 C23 C24 125.0(17) . . ?
C24 C23 H23 117.5 . . ?
C23 C24 H24 121.1 . . ?
C23 C24 C25 117.7(16) . . ?
C25 C24 H24 121.1 . . ?
C26 C25 C24 119.0(17) . . ?
C26 C25 O9 125.7(17) . . ?
O9 C25 C24 115.0(16) . . ?
C25 C26 H26 118.9 . . ?
C25 C26 C27 122.3(19) . . ?
C27 C26 H26 118.9 . . ?
C22 C27 H27 119.7 . . ?
C26 C27 C22 120.5(17) . . ?
C26 C27 H27 119.7 . . ?
C25 O9 H9A 109.5 . . ?
O3 C7 C6 123.1(11) . . ?
C8 C7 O3 118.7(16) . . ?
C8 C7 C6 118.2(17) . . ?
C1 O2 Er1 92.4(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1Z H1Z1 O5 0.95 1.81 2.745(15) 168.4 1_565
O1Z H1Z2 O9 0.95 2.07 2.838(15) 136.4 3_655
O6 H6A O1 0.84 1.83 2.660(15) 170.9 3_645

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.02838
2 0.97162
#=======================================================
#ALERT LEVEL B
_vrf_PLAT342                     
;
PROBLEM:Low Bond Precision on C-C Bonds ......... 0.0220 Ang
RESPONSE: The crystal was slightly twined and resulted to the 
low bond precision.
;
_vrf_PLAT420                     
;
PROBLEMS: D-H Without Acceptor O2Z - H2Z2 .. Please Check;
D-H Without Acceptor O3 - H3 .. Please Check;
D-H Without Acceptor O2Z - H2Z1 .. Please Check;
D-H Without Acceptor O9 - H9A .. Please Check
RESPONSE: The listed hydrogen bonds have been checked, but not found.
;
#=======================================================
####################################################################### 
# 
# 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_compound1.cif
_database_code_depnum_ccdc_archive 'CCDC 1055963'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_audit_creation_date             2015-05-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C108 H120 La4 O42, 4(H2 O), C H4 O'
_chemical_formula_sum            'C109 H132 La4 O47'
_chemical_formula_weight         2749.78
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.2502(9)
_cell_length_b                   16.6406(10)
_cell_length_c                   25.6709(14)
_cell_angle_alpha                89.014(2)
_cell_angle_beta                 78.289(2)
_cell_angle_gamma                64.668(3)
_cell_volume                     5747.7(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    87057
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.086
_cell_measurement_theta_min      0.813
_shelx_estimated_absorpt_T_max   0.962
_shelx_estimated_absorpt_T_min   0.747
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   0.9624
_exptl_transmission_factor_min   0.7473
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80774
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         0.813
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20184
_reflns_number_total             25932
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1500
_refine_ls_number_reflns         25932
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0814
_refine_ls_restrained_S_all      1.238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1571
_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.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6H of O6, H9H of O9, H12H of O12, H18H of O18, H11Z of
  O11Z, H3H of O3, H36H of O36, H33H of O33, H30H of O30, H27H of O27, H24H of
  O24, H21H of O21, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H15H of O15
2. Restrained distances
 O10Z-H101 = O10Z-H100 = O8Z-H80A = O8Z-H80B
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B), C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B),
  C47(H47A,H47B), C48(H48A,H48B), C56(H56A,H56B), C65(H65A,H65B), C66(H66A,
 H66B), C74(H74A,H74B), C75(H75A,H75B), C83(H83A,H83B), C84(H84A,H84B),
 C92(H92A,H92B), C93(H93A,H93B), C101(H10A,H10B), C102(H10C,H10D), C57(H57A,
 H57B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27), C32(H32), C33(H33), C35(H35), C36(H36),
  C41(H41), C42(H42), C44(H44), C45(H45), C50(H50), C51(H51), C53(H53),
 C54(H54), C59(H59), C60(H60), C62(H62), C63(H63), C68(H68), C69(H69), C71(H71),
  C72(H72), C77(H77), C78(H78), C80(H80), C81(H81), C86(H86), C87(H87),
 C89(H89), C90(H90), C95(H95), C96(H96), C98(H98), C99(H99), C104(H104),
 C105(H105), C107(H107), C108(H108)
3.c Tetrahedral OH refined with riding coordinates:
 O15(H15H)
3.d X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2), O3Z(H3Z1,H3Z2), O4Z(H4Z1,H4Z2), O5Z(H5Z1,H5Z2)
3.e Idealised Me refined as rotating group:
 C1Z(H1Z3,H1Z4,H1Z5)
3.f Idealised tetrahedral OH refined as rotating group:
 O3(H3H), O12(H12H), O18(H18H), O21(H21H), O24(H24H), O27(H27H), O33(H33H),
 O36(H36H), O11Z(H11Z)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.79839(3) 0.35922(3) 0.77819(2) 0.01493(10) Uani 1 1 d . . . . .
La2 La 0.78538(3) 0.61067(3) 0.76882(2) 0.01525(10) Uani 1 1 d . . . . .
La3 La 0.75113(3) 0.87993(3) 0.73423(2) 0.01393(10) Uani 1 1 d . . . . .
La4 La 0.72661(3) 1.14115(3) 0.72611(2) 0.01431(10) Uani 1 1 d . . . . .
O1 O 0.6076(4) 0.4308(3) 0.8091(2) 0.0228(12) Uani 1 1 d . . . . .
O1Z O 0.8186(4) 0.2405(3) 0.8443(2) 0.0241(12) Uani 1 1 d . . . . .
H1Z1 H 0.8762 0.2166 0.8591 0.029 Uiso 1 1 calc R . . . .
H1Z2 H 0.7686 0.2201 0.8544 0.029 Uiso 1 1 calc R . . . .
O2 O 0.6634(4) 0.2932(3) 0.7769(2) 0.0198(11) Uani 1 1 d . . . . .
O2Z O 0.9607(4) 0.3096(3) 0.8098(2) 0.0252(12) Uani 1 1 d . . . . .
H2Z1 H 0.9768 0.2653 0.8347 0.030 Uiso 1 1 calc R . . . .
H2Z2 H 1.0049 0.3353 0.7967 0.030 Uiso 1 1 calc R . . . .
O3 O 0.0513(4) 0.4158(3) 0.8271(3) 0.0317(14) Uani 1 1 d . . . . .
H3H H 0.0063 0.4681 0.8293 0.038 Uiso 1 1 calc GR . . . .
O3Z O 0.8221(4) 0.6198(3) 0.6699(2) 0.0251(12) Uani 1 1 d . . . . .
H3Z1 H 0.8231 0.5755 0.6467 0.030 Uiso 1 1 calc R . . . .
H3Z2 H 0.8351 0.6677 0.6556 0.030 Uiso 1 1 calc R . . . .
O4 O 0.7128(4) 0.4045(3) 0.6966(2) 0.0254(12) Uani 1 1 d . . . . .
O4Z O 0.7191(4) 0.8670(3) 0.83327(19) 0.0237(12) Uani 1 1 d . . . . .
H4Z1 H 0.6668 0.9148 0.8564 0.028 Uiso 1 1 calc R . . . .
H4Z2 H 0.7593 0.8142 0.8476 0.028 Uiso 1 1 calc R . . . .
O5 O 0.7043(4) 0.5292(4) 0.72945(19) 0.0236(12) Uani 1 1 d . . . . .
O5Z O 0.5699(4) 1.1738(4) 0.6925(2) 0.0260(12) Uani 1 1 d . . . . .
H5Z1 H 0.5115 1.1784 0.7166 0.031 Uiso 1 1 calc R . . . .
H5Z2 H 0.5697 1.1815 0.6557 0.031 Uiso 1 1 calc R . . . .
O6 O 0.2241(4) 0.8241(4) 0.5841(2) 0.0363(15) Uani 1 1 d . . . . .
H6H H 0.170(7) 0.849(6) 0.610(4) 0.044 Uiso 1 1 d R . . . .
O6Z O 0.6870(5) 1.2677(4) 0.6625(2) 0.0261(13) Uani 1 1 d . . . . .
O7 O 0.9316(4) 0.3377(4) 0.6933(2) 0.0316(14) Uani 1 1 d . . . . .
O7Z O 0.7563(5) 0.3073(4) 0.9673(3) 0.0390(17) Uani 1 1 d . . . . .
O8 O 0.9103(4) 0.4571(3) 0.73935(19) 0.0226(12) Uani 1 1 d . . . . .
O8Z O 0.4768(4) 0.6093(4) 0.8298(3) 0.0373(15) Uani 1 1 d D . . . .
O9 O 1.1829(7) 0.4734(5) 0.4126(2) 0.053(2) Uani 1 1 d . . . . .
H9H H 1.188(9) 0.517(8) 0.416(4) 0.064 Uiso 1 1 d R . . . .
O9Z O 1.0522(5) 0.8911(4) 0.6602(3) 0.0386(17) Uani 1 1 d . . . . .
O10 O 0.7310(4) 0.4160(3) 0.88760(19) 0.0238(12) Uani 1 1 d . . . . .
O10Z O 0.7403(5) 1.1831(5) 0.5361(3) 0.0456(18) Uani 1 1 d D . . . .
O11 O 0.7469(4) 0.5098(3) 0.83020(18) 0.0205(11) Uani 1 1 d . . . . .
O12 O 0.3107(7) 0.8833(4) 1.0845(3) 0.072(3) Uani 1 1 d . . . . .
H12H H 0.3307 0.8850 1.1124 0.087 Uiso 1 1 calc GR . . . .
O13 O 0.9029(4) 0.5768(3) 0.8337(2) 0.0234(12) Uani 1 1 d . . . . .
O14 O 0.7656(4) 0.6992(3) 0.85416(19) 0.0196(11) Uani 1 1 d . . . . .
O15 O 0.6917(5) 0.4960(4) 1.0787(3) 0.0449(17) Uani 1 1 d . . . . .
H15H H 0.7043 0.4427 1.0711 0.067 Uiso 1 1 calc R . . . .
O16 O 0.5951(4) 0.7019(3) 0.8032(2) 0.0235(12) Uani 1 1 d . . . . .
O17 O 0.6687(4) 0.7765(3) 0.75729(19) 0.0188(11) Uani 1 1 d . . . . .
O18 O 0.0348(5) 1.1517(5) 0.8630(3) 0.068(3) Uani 1 1 d . . . . .
H18H H 0.0036 1.1543 0.8944 0.081 Uiso 1 1 calc GR . . . .
O19 O 0.9387(4) 0.7947(3) 0.6983(2) 0.0207(11) Uani 1 1 d . . . . .
O20 O 0.8764(3) 0.7103(3) 0.74287(19) 0.0175(11) Uani 1 1 d . . . . .
O21 O 1.4970(6) 0.3885(5) 0.5604(4) 0.075(3) Uani 1 1 d . . . . .
H21H H 1.5321 0.3592 0.5816 0.090 Uiso 1 1 calc GR . . . .
O22 O 0.7754(4) 0.7888(3) 0.64701(19) 0.0188(11) Uani 1 1 d . . . . .
O23 O 0.6339(4) 0.9080(3) 0.6709(2) 0.0243(12) Uani 1 1 d . . . . .
O24 O 0.4398(4) 0.7901(4) 0.4156(2) 0.0354(14) Uani 1 1 d . . . . .
H24H H 0.3782 0.8122 0.4281 0.043 Uiso 1 1 calc GR . . . .
O25 O 0.6105(4) 1.0236(4) 0.7665(2) 0.0262(13) Uani 1 1 d . . . . .
O26 O 0.5965(4) 1.1459(4) 0.8066(2) 0.0317(14) Uani 1 1 d . . . . .
O27 O 0.2626(6) 1.0560(4) 1.0798(2) 0.0468(18) Uani 1 1 d . . . . .
H27H H 0.2945 1.0009 1.0817 0.056 Uiso 1 1 calc GR . . . .
O28 O 0.7918(4) 1.0883(3) 0.62079(19) 0.0241(12) Uani 1 1 d . . . . .
O29 O 0.7775(4) 0.9891(3) 0.67426(18) 0.0186(11) Uani 1 1 d . . . . .
O30 O 1.1936(7) 0.6267(5) 0.4118(3) 0.068(3) Uani 1 1 d . . . . .
H30H H 1.181(9) 0.640(8) 0.376(5) 0.082 Uiso 1 1 d R . . . .
O31 O 0.8044(4) 1.0975(3) 0.8106(2) 0.0233(12) Uani 1 1 d . . . . .
O32 O 0.8144(4) 0.9760(3) 0.7742(2) 0.0190(11) Uani 1 1 d . . . . .
O33 O 1.3108(4) 0.6695(4) 0.9055(2) 0.0338(14) Uani 1 1 d . . . . .
H33H H 1.3627 0.6536 0.8815 0.041 Uiso 1 1 calc GR . . . .
O34 O 0.9201(4) 1.0660(3) 0.6991(2) 0.0234(12) Uani 1 1 d . . . . .
O35 O 0.8586(4) 1.2052(3) 0.72917(19) 0.0180(11) Uani 1 1 d . . . . .
O36 O 1.4832(4) 1.0644(4) 0.6808(3) 0.0424(17) Uani 1 1 d . . . . .
H36H H 1.5258 1.0111 0.6743 0.051 Uiso 1 1 calc GR . . . .
C1 C 0.5908(5) 0.3644(5) 0.7987(3) 0.0213(17) Uani 1 1 d . . . . .
C2 C 0.4874(5) 0.3733(5) 0.8120(3) 0.0236(17) Uani 1 1 d . . . . .
H2A H 0.4498 0.4156 0.8440 0.028 Uiso 1 1 calc R . . . .
H2B H 0.4889 0.3147 0.8208 0.028 Uiso 1 1 calc R . . . .
C3 C 0.4345(6) 0.4061(6) 0.7666(3) 0.034(2) Uani 1 1 d . . . . .
H3A H 0.4295 0.4662 0.7589 0.041 Uiso 1 1 calc R . . . .
H3B H 0.4732 0.3654 0.7341 0.041 Uiso 1 1 calc R . . . .
C4 C 0.3320(6) 0.4098(6) 0.7809(3) 0.032(2) Uani 1 1 d . . . . .
C5 C 0.2490(6) 0.4898(6) 0.7993(3) 0.0306(19) Uani 1 1 d . . . . .
H5 H 0.2569 0.5431 0.8020 0.037 Uiso 1 1 calc R . . . .
C6 C 0.1546(6) 0.4928(6) 0.8137(3) 0.0290(19) Uani 1 1 d . . . . .
H6 H 0.0983 0.5483 0.8248 0.035 Uiso 1 1 calc R . . . .
C7 C 0.1423(6) 0.4169(5) 0.8122(3) 0.0267(18) Uani 1 1 d . . . . .
C8 C 0.2236(6) 0.3358(6) 0.7947(4) 0.035(2) Uani 1 1 d . . . . .
H8 H 0.2151 0.2827 0.7930 0.042 Uiso 1 1 calc R . . . .
C9 C 0.3170(6) 0.3334(6) 0.7799(4) 0.032(2) Uani 1 1 d . . . . .
H9 H 0.3727 0.2775 0.7686 0.039 Uiso 1 1 calc R . . . .
C10 C 0.6760(6) 0.4891(5) 0.7011(3) 0.0230(17) Uani 1 1 d . . . . .
C11 C 0.5910(6) 0.5403(5) 0.6746(3) 0.0263(18) Uani 1 1 d . . . . .
H11A H 0.5313 0.5348 0.6945 0.032 Uiso 1 1 calc R . . . .
H11B H 0.6073 0.5124 0.6381 0.032 Uiso 1 1 calc R . . . .
C12 C 0.5657(7) 0.6395(5) 0.6711(4) 0.036(2) Uani 1 1 d . . . . .
H12A H 0.5538 0.6670 0.7073 0.043 Uiso 1 1 calc R . . . .
H12B H 0.6234 0.6454 0.6487 0.043 Uiso 1 1 calc R . . . .
C13 C 0.4754(6) 0.6894(5) 0.6479(4) 0.030(2) Uani 1 1 d . . . . .
C14 C 0.3829(7) 0.7377(6) 0.6813(4) 0.037(2) Uani 1 1 d . . . . .
H14 H 0.3772 0.7392 0.7189 0.045 Uiso 1 1 calc R . . . .
C15 C 0.2976(7) 0.7843(6) 0.6605(4) 0.037(2) Uani 1 1 d . . . . .
H15 H 0.2352 0.8183 0.6838 0.044 Uiso 1 1 calc R . . . .
C16 C 0.3055(6) 0.7803(5) 0.6065(3) 0.0289(19) Uani 1 1 d . . . . .
C17 C 0.3972(6) 0.7342(6) 0.5727(3) 0.032(2) Uani 1 1 d . . . . .
H17 H 0.4029 0.7334 0.5352 0.038 Uiso 1 1 calc R . . . .
C18 C 0.4812(6) 0.6889(6) 0.5936(4) 0.032(2) Uani 1 1 d . . . . .
H18 H 0.5438 0.6570 0.5700 0.038 Uiso 1 1 calc R . . . .
C19 C 0.9523(6) 0.4017(5) 0.6985(3) 0.0231(17) Uani 1 1 d . . . . .
C20 C 1.0269(7) 0.4155(6) 0.6560(3) 0.032(2) Uani 1 1 d . . . . .
H20A H 1.0771 0.4209 0.6731 0.038 Uiso 1 1 calc R . . . .
H20B H 0.9924 0.4731 0.6411 0.038 Uiso 1 1 calc R . . . .
C21 C 1.0809(8) 0.3443(6) 0.6103(3) 0.041(2) Uani 1 1 d . . . . .
H21A H 1.1413 0.2980 0.6199 0.049 Uiso 1 1 calc R . . . .
H21B H 1.0376 0.3156 0.6058 0.049 Uiso 1 1 calc R . . . .
C22 C 1.1107(6) 0.3771(5) 0.5582(3) 0.0269(19) Uani 1 1 d . . . . .
C23 C 1.0807(6) 0.3631(6) 0.5135(3) 0.033(2) Uani 1 1 d . . . . .
H23 H 1.0430 0.3297 0.5159 0.040 Uiso 1 1 calc R . . . .
C24 C 1.1034(7) 0.3958(6) 0.4652(3) 0.034(2) Uani 1 1 d . . . . .
H24 H 1.0801 0.3867 0.4352 0.040 Uiso 1 1 calc R . . . .
C25 C 1.1606(7) 0.4418(6) 0.4619(3) 0.031(2) Uani 1 1 d . . . . .
C26 C 1.1959(7) 0.4548(6) 0.5047(3) 0.031(2) Uani 1 1 d . . . . .
H26 H 1.2369 0.4853 0.5013 0.038 Uiso 1 1 calc R . . . .
C27 C 1.1708(6) 0.4229(5) 0.5526(3) 0.0269(18) Uani 1 1 d . . . . .
H27 H 1.1944 0.4320 0.5824 0.032 Uiso 1 1 calc R . . . .
C28 C 0.7149(5) 0.4937(5) 0.8777(3) 0.0175(15) Uani 1 1 d . . . . .
C29 C 0.6550(6) 0.5720(5) 0.9180(3) 0.0233(17) Uani 1 1 d . . . . .
H29A H 0.6301 0.6268 0.8989 0.028 Uiso 1 1 calc R . . . .
H29B H 0.6989 0.5776 0.9398 0.028 Uiso 1 1 calc R . . . .
C30 C 0.5668(6) 0.5654(5) 0.9550(3) 0.0265(18) Uani 1 1 d . . . . .
H30A H 0.5283 0.5506 0.9332 0.032 Uiso 1 1 calc R . . . .
H30B H 0.5919 0.5161 0.9781 0.032 Uiso 1 1 calc R . . . .
C31 C 0.4989(6) 0.6497(5) 0.9894(3) 0.0220(17) Uani 1 1 d . . . . .
C32 C 0.4508(6) 0.7288(5) 0.9669(3) 0.0241(18) Uani 1 1 d . . . . .
H32 H 0.4607 0.7296 0.9292 0.029 Uiso 1 1 calc R . . . .
C33 C 0.3880(6) 0.8073(6) 0.9990(3) 0.034(2) Uani 1 1 d . . . . .
H33 H 0.3551 0.8613 0.9835 0.041 Uiso 1 1 calc R . . . .
C34 C 0.3746(7) 0.8051(6) 1.0538(3) 0.032(2) Uani 1 1 d . . . . .
C35 C 0.4221(7) 0.7285(5) 1.0769(3) 0.031(2) Uani 1 1 d . . . . .
H35 H 0.4128 0.7285 1.1147 0.037 Uiso 1 1 calc R . . . .
C36 C 0.4838(6) 0.6508(6) 1.0449(3) 0.0256(18) Uani 1 1 d . . . . .
H36 H 0.5165 0.5973 1.0610 0.031 Uiso 1 1 calc R . . . .
C37 C 0.8509(6) 0.6500(5) 0.8622(3) 0.0175(15) Uani 1 1 d . . . . .
C38 C 0.8924(6) 0.6799(5) 0.9025(3) 0.0273(18) Uani 1 1 d . . . . .
H38A H 0.8368 0.7291 0.9265 0.033 Uiso 1 1 calc R . . . .
H38B H 0.9379 0.7041 0.8834 0.033 Uiso 1 1 calc R . . . .
C39 C 0.9484(6) 0.6074(6) 0.9366(3) 0.031(2) Uani 1 1 d . . . . .
H39A H 1.0011 0.5561 0.9128 0.037 Uiso 1 1 calc R . . . .
H39B H 0.9811 0.6310 0.9577 0.037 Uiso 1 1 calc R . . . .
C40 C 0.8820(6) 0.5751(6) 0.9743(3) 0.0272(19) Uani 1 1 d . . . . .
C41 C 0.8908(6) 0.4892(5) 0.9681(3) 0.0265(18) Uani 1 1 d . . . . .
H41 H 0.9397 0.4493 0.9397 0.032 Uiso 1 1 calc R . . . .
C42 C 0.8297(6) 0.4606(6) 1.0028(3) 0.033(2) Uani 1 1 d . . . . .
H42 H 0.8374 0.4013 0.9983 0.039 Uiso 1 1 calc R . . . .
C43 C 0.7570(6) 0.5189(6) 1.0443(3) 0.031(2) Uani 1 1 d . . . . .
C44 C 0.7471(7) 0.6047(6) 1.0510(4) 0.044(3) Uani 1 1 d . . . . .
H44 H 0.6976 0.6448 1.0792 0.053 Uiso 1 1 calc R . . . .
C45 C 0.8098(7) 0.6323(6) 1.0163(4) 0.041(2) Uani 1 1 d . . . . .
H45 H 0.8033 0.6911 1.0214 0.049 Uiso 1 1 calc R . . . .
C46 C 0.5903(6) 0.7730(5) 0.7842(3) 0.0236(17) Uani 1 1 d . . . . .
C47 C 0.4929(6) 0.8544(6) 0.7893(4) 0.042(2) Uani 1 1 d . . . . .
H47A H 0.5037 0.9075 0.7960 0.050 Uiso 1 1 calc R . . . .
H47B H 0.4723 0.8595 0.7548 0.050 Uiso 1 1 calc R . . . .
C48 C 0.4136(8) 0.8560(7) 0.8301(6) 0.086(5) Uani 1 1 d . . . . .
H48A H 0.4342 0.8528 0.8646 0.104 Uiso 1 1 calc R . . . .
H48B H 0.4060 0.8009 0.8242 0.104 Uiso 1 1 calc R . . . .
C49 C 0.3122(6) 0.9341(6) 0.8363(4) 0.038(2) Uani 1 1 d . . . . .
C50 C 0.2945(7) 1.0085(6) 0.8074(3) 0.036(2) Uani 1 1 d . . . . .
H50 H 0.3469 1.0099 0.7806 0.043 Uiso 1 1 calc R . . . .
C51 C 0.2012(6) 1.0812(6) 0.8169(3) 0.032(2) Uani 1 1 d . . . . .
H51 H 0.1900 1.1320 0.7969 0.039 Uiso 1 1 calc R . . . .
C52 C 0.1276(7) 1.0785(7) 0.8546(4) 0.040(2) Uani 1 1 d . . . . .
C53 C 0.1421(7) 1.0078(6) 0.8857(4) 0.037(2) Uani 1 1 d . . . . .
H53 H 0.0892 1.0083 0.9128 0.045 Uiso 1 1 calc R . . . .
C54 C 0.2363(7) 0.9348(6) 0.8767(4) 0.038(2) Uani 1 1 d . . . . .
H54 H 0.2480 0.8859 0.8984 0.046 Uiso 1 1 calc R . . . .
C55 C 0.9485(5) 0.7186(5) 0.7124(3) 0.0182(16) Uani 1 1 d . . . . .
C56 C 1.0441(6) 0.6377(6) 0.6914(4) 0.040(2) Uani 1 1 d . . . . .
H56A H 1.0569 0.5959 0.7199 0.048 Uiso 1 1 calc R . . . .
H56B H 1.0352 0.6077 0.6613 0.048 Uiso 1 1 calc R . . . .
C58 C 1.2248(6) 0.5769(7) 0.6433(4) 0.043(2) Uani 1 1 d . . . . .
C59 C 1.2665(7) 0.4947(6) 0.6629(4) 0.040(2) Uani 1 1 d . . . . .
H59 H 1.2320 0.4812 0.6943 0.048 Uiso 1 1 calc R . . . .
C60 C 1.3602(7) 0.4308(6) 0.6362(4) 0.043(2) Uani 1 1 d . . . . .
H60 H 1.3914 0.3749 0.6502 0.052 Uiso 1 1 calc R . . . .
C61 C 1.4063(7) 0.4508(7) 0.5891(5) 0.053(3) Uani 1 1 d . . . . .
C62 C 1.3640(8) 0.5306(7) 0.5675(4) 0.055(3) Uani 1 1 d . . . . .
H62 H 1.3959 0.5415 0.5341 0.066 Uiso 1 1 calc R . . . .
C63 C 1.2750(7) 0.5943(6) 0.5948(4) 0.046(3) Uani 1 1 d . . . . .
H63 H 1.2464 0.6510 0.5812 0.055 Uiso 1 1 calc R . . . .
C64 C 0.6895(6) 0.8383(5) 0.6392(3) 0.0221(17) Uani 1 1 d . . . . .
C65 C 0.6516(7) 0.8162(5) 0.5945(3) 0.0265(18) Uani 1 1 d . . . . .
H65A H 0.5904 0.8091 0.6097 0.032 Uiso 1 1 calc R . . . .
H65B H 0.7018 0.7584 0.5757 0.032 Uiso 1 1 calc R . . . .
C66 C 0.6286(7) 0.8867(5) 0.5543(3) 0.0265(18) Uani 1 1 d . . . . .
H66A H 0.5862 0.9461 0.5736 0.032 Uiso 1 1 calc R . . . .
H66B H 0.6914 0.8873 0.5349 0.032 Uiso 1 1 calc R . . . .
C67 C 0.5775(6) 0.8703(5) 0.5154(3) 0.0258(18) Uani 1 1 d . . . . .
C68 C 0.6325(7) 0.8037(6) 0.4718(4) 0.041(2) Uani 1 1 d . . . . .
H68 H 0.7029 0.7748 0.4657 0.049 Uiso 1 1 calc R . . . .
C69 C 0.5854(6) 0.7812(7) 0.4388(3) 0.038(2) Uani 1 1 d . . . . .
H69 H 0.6231 0.7376 0.4097 0.045 Uiso 1 1 calc R . . . .
C70 C 0.4844(6) 0.8212(6) 0.4476(3) 0.0275(19) Uani 1 1 d . . . . .
C71 C 0.4277(6) 0.8886(5) 0.4882(3) 0.0260(18) Uani 1 1 d . . . . .
H71 H 0.3574 0.9185 0.4930 0.031 Uiso 1 1 calc R . . . .
C72 C 0.4758(6) 0.9108(5) 0.5214(3) 0.0258(18) Uani 1 1 d . . . . .
H72 H 0.4372 0.9559 0.5496 0.031 Uiso 1 1 calc R . . . .
C73 C 0.5746(6) 1.0822(5) 0.8062(3) 0.0270(18) Uani 1 1 d . . . . .
C74 C 0.5057(6) 1.0698(6) 0.8530(3) 0.032(2) Uani 1 1 d . . . . .
H74A H 0.5456 1.0340 0.8781 0.039 Uiso 1 1 calc R . . . .
H74B H 0.4744 1.0350 0.8401 0.039 Uiso 1 1 calc R . . . .
C75 C 0.4241(6) 1.1552(5) 0.8832(3) 0.0277(19) Uani 1 1 d . . . . .
H75A H 0.4525 1.1964 0.8903 0.033 Uiso 1 1 calc R . . . .
H75B H 0.3739 1.1851 0.8615 0.033 Uiso 1 1 calc R . . . .
C76 C 0.3754(6) 1.1332(5) 0.9355(3) 0.0246(18) Uani 1 1 d . . . . .
C77 C 0.4026(7) 1.1435(7) 0.9816(3) 0.045(3) Uani 1 1 d . . . . .
H77 H 0.4463 1.1708 0.9807 0.054 Uiso 1 1 calc R . . . .
C78 C 0.3687(8) 1.1158(7) 1.0296(4) 0.045(3) Uani 1 1 d . . . . .
H78 H 0.3912 1.1207 1.0608 0.054 Uiso 1 1 calc R . . . .
C79 C 0.3007(7) 1.0805(6) 1.0307(3) 0.035(2) Uani 1 1 d . . . . .
C80 C 0.2699(8) 1.0727(7) 0.9862(4) 0.049(3) Uani 1 1 d . . . . .
H80 H 0.2226 1.0493 0.9874 0.059 Uiso 1 1 calc R . . . .
C81 C 0.3077(7) 1.0991(6) 0.9390(3) 0.037(2) Uani 1 1 d . . . . .
H81 H 0.2856 1.0933 0.9078 0.045 Uiso 1 1 calc R . . . .
C82 C 0.8042(5) 1.0090(5) 0.6276(3) 0.0198(16) Uani 1 1 d . . . . .
C83 C 0.8516(6) 0.9385(5) 0.5818(3) 0.0266(18) Uani 1 1 d . . . . .
H83A H 0.8009 0.9440 0.5615 0.032 Uiso 1 1 calc R . . . .
H83B H 0.8746 0.8791 0.5962 0.032 Uiso 1 1 calc R . . . .
C84 C 0.9384(6) 0.9441(6) 0.5442(3) 0.031(2) Uani 1 1 d . . . . .
H84A H 0.9798 0.9559 0.5653 0.038 Uiso 1 1 calc R . . . .
H84B H 0.9131 0.9949 0.5221 0.038 Uiso 1 1 calc R . . . .
C85 C 1.0026(6) 0.8596(5) 0.5079(3) 0.0248(18) Uani 1 1 d . . . . .
C86 C 1.0126(6) 0.8580(6) 0.4531(3) 0.0270(18) Uani 1 1 d . . . . .
H86 H 0.9755 0.9106 0.4375 0.032 Uiso 1 1 calc R . . . .
C87 C 1.0748(7) 0.7820(7) 0.4210(3) 0.039(2) Uani 1 1 d . . . . .
H87 H 1.0808 0.7828 0.3835 0.047 Uiso 1 1 calc R . . . .
C88 C 1.1276(8) 0.7062(6) 0.4418(4) 0.042(3) Uani 1 1 d . . . . .
C89 C 1.1191(7) 0.7036(6) 0.4968(4) 0.038(2) Uani 1 1 d . . . . .
H89 H 1.1552 0.6500 0.5119 0.045 Uiso 1 1 calc R . . . .
C90 C 1.0560(7) 0.7819(5) 0.5291(3) 0.030(2) Uani 1 1 d . . . . .
H90 H 1.0498 0.7813 0.5666 0.036 Uiso 1 1 calc R . . . .
C91 C 0.8448(5) 1.0137(5) 0.8029(3) 0.0154(15) Uani 1 1 d . . . . .
C92 C 0.9315(6) 0.9614(5) 0.8280(3) 0.0235(17) Uani 1 1 d . . . . .
H92A H 0.9116 0.9793 0.8667 0.028 Uiso 1 1 calc R . . . .
H92B H 0.9866 0.9772 0.8127 0.028 Uiso 1 1 calc R . . . .
C93 C 0.9697(7) 0.8604(5) 0.8203(4) 0.034(2) Uani 1 1 d . . . . .
H93A H 0.9160 0.8440 0.8375 0.041 Uiso 1 1 calc R . . . .
H93B H 0.9860 0.8427 0.7816 0.041 Uiso 1 1 calc R . . . .
C94 C 1.0597(6) 0.8092(5) 0.8428(3) 0.0257(18) Uani 1 1 d . . . . .
C95 C 1.0531(6) 0.8008(5) 0.8969(3) 0.0255(18) Uani 1 1 d . . . . .
H95 H 0.9898 0.8276 0.9205 0.031 Uiso 1 1 calc R . . . .
C96 C 1.1373(6) 0.7540(5) 0.9179(3) 0.0273(18) Uani 1 1 d . . . . .
H96 H 1.1309 0.7485 0.9552 0.033 Uiso 1 1 calc R . . . .
C97 C 1.2292(6) 0.7158(5) 0.8840(3) 0.0267(18) Uani 1 1 d . . . . .
C98 C 1.2378(6) 0.7240(5) 0.8289(3) 0.031(2) Uani 1 1 d . . . . .
H98 H 1.3012 0.6978 0.8054 0.037 Uiso 1 1 calc R . . . .
C99 C 1.1536(6) 0.7703(6) 0.8090(4) 0.032(2) Uani 1 1 d . . . . .
H99 H 1.1599 0.7756 0.7717 0.038 Uiso 1 1 calc R . . . .
C100 C 0.9328(5) 1.1302(5) 0.7156(3) 0.0167(15) Uani 1 1 d . . . . .
C101 C 1.0340(5) 1.1173(6) 0.7199(3) 0.0236(17) Uani 1 1 d . . . . .
H10A H 1.0627 1.0655 0.7408 0.028 Uiso 1 1 calc R . . . .
H10B H 1.0284 1.1707 0.7394 0.028 Uiso 1 1 calc R . . . .
C102 C 1.1033(6) 1.1022(7) 0.6660(4) 0.041(2) Uani 1 1 d . . . . .
H10C H 1.1097 1.0484 0.6466 0.049 Uiso 1 1 calc R . . . .
H10D H 1.0743 1.1537 0.6449 0.049 Uiso 1 1 calc R . . . .
C103 C 1.2037(6) 1.0906(6) 0.6705(3) 0.032(2) Uani 1 1 d . . . . .
C104 C 1.2870(7) 1.0088(6) 0.6585(3) 0.035(2) Uani 1 1 d . . . . .
H104 H 1.2791 0.9587 0.6470 0.041 Uiso 1 1 calc R . . . .
C105 C 1.3808(6) 0.9973(6) 0.6624(3) 0.0291(19) Uani 1 1 d . . . . .
H105 H 1.4357 0.9401 0.6551 0.035 Uiso 1 1 calc R . . . .
C106 C 1.3924(6) 1.0705(6) 0.6771(3) 0.0275(19) Uani 1 1 d . . . . .
C107 C 1.3122(6) 1.1533(5) 0.6888(3) 0.0278(19) Uani 1 1 d . . . . .
H107 H 1.3211 1.2037 0.6986 0.033 Uiso 1 1 calc R . . . .
C108 C 1.2184(6) 1.1624(6) 0.6859(3) 0.033(2) Uani 1 1 d . . . . .
H108 H 1.1631 1.2191 0.6947 0.039 Uiso 1 1 calc R . . . .
H70A H 0.711(6) 0.327(5) 0.992(3) 0.02(2) Uiso 1 1 d . . . . .
H80B H 0.521(5) 0.632(5) 0.827(3) 0.04(3) Uiso 1 1 d D . . . .
H90A H 1.018(7) 0.859(7) 0.672(4) 0.05(3) Uiso 1 1 d . . . . .
H90B H 1.023(7) 0.946(7) 0.670(4) 0.04(3) Uiso 1 1 d . . . . .
H80A H 0.519(8) 0.552(3) 0.820(5) 0.10(5) Uiso 1 1 d D . . . .
H101 H 0.762(8) 1.181(8) 0.5004(11) 0.08(4) Uiso 1 1 d D . . . .
H70B H 0.739(8) 0.344(7) 0.944(4) 0.06(4) Uiso 1 1 d . . . . .
H100 H 0.788(7) 1.130(4) 0.541(5) 0.10(5) Uiso 1 1 d D . . . .
O11Z O -0.0954(6) 1.1454(6) 0.9468(3) 0.079(3) Uani 1 1 d . . . . .
H11Z H -0.1460 1.1946 0.9531 0.095 Uiso 1 1 calc GR . . . .
C1Z C -0.1165(10) 1.0809(10) 0.9741(6) 0.087(4) Uani 1 1 d . . . . .
H1Z3 H -0.1337 1.0971 1.0126 0.131 Uiso 1 1 calc GR . . . .
H1Z4 H -0.0581 1.0231 0.9658 0.131 Uiso 1 1 calc GR . . . .
H1Z5 H -0.1726 1.0769 0.9632 0.131 Uiso 1 1 calc GR . . . .
C57 C 1.1306(8) 0.6535(7) 0.6735(7) 0.085(5) Uani 1 1 d . . . . .
H57A H 1.1461 0.6733 0.7052 0.102 Uiso 1 1 calc R . . . .
H57B H 1.1129 0.7037 0.6504 0.102 Uiso 1 1 calc R . . . .
H6Z2 H 0.675(7) 1.331(7) 0.679(4) 0.05(3) Uiso 1 1 d . . . . .
H6Z1 H 0.718(8) 1.248(7) 0.634(4) 0.06(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O1 2.577(5) . ?
La1 O1Z 2.541(5) . ?
La1 O2 2.723(5) . ?
La1 O2Z 2.551(5) . ?
La1 O4 2.621(5) . ?
La1 O5 2.959(5) . ?
La1 O7 2.571(5) . ?
La1 O8 2.862(5) . ?
La1 O10 2.815(5) . ?
La1 O11 2.586(5) . ?
La1 O35 2.575(5) 1_545 ?
La1 C1 3.066(8) . ?
La2 O3Z 2.504(5) . ?
La2 O5 2.525(5) . ?
La2 O8 2.459(5) . ?
La2 O11 2.453(5) . ?
La2 O13 2.573(5) . ?
La2 O14 2.554(5) . ?
La2 O16 2.596(5) . ?
La2 O17 2.618(5) . ?
La2 O20 2.584(5) . ?
La2 C37 2.959(7) . ?
La2 C46 2.998(8) . ?
La3 La4 4.2057(6) . ?
La3 O4Z 2.513(5) . ?
La3 O17 2.532(5) . ?
La3 O19 2.558(5) . ?
La3 O20 2.684(5) . ?
La3 O22 2.598(5) . ?
La3 O23 2.549(5) . ?
La3 O25 2.442(5) . ?
La3 O29 2.472(5) . ?
La3 O32 2.514(5) . ?
La3 C55 3.006(7) . ?
La3 C64 2.976(8) . ?
La4 O2 2.559(5) 1_565 ?
La4 O5Z 2.543(5) . ?
La4 O6Z 2.580(5) . ?
La4 O26 2.534(5) . ?
La4 O28 2.704(5) . ?
La4 O29 2.606(5) . ?
La4 O31 2.626(5) . ?
La4 O32 2.877(5) . ?
La4 O34 2.607(5) . ?
La4 O35 2.663(5) . ?
La4 C82 3.063(7) . ?
La4 C100 3.027(7) . ?
O1 C1 1.279(9) . ?
O1Z H1Z1 0.9500 . ?
O1Z H1Z2 0.9500 . ?
O2 La4 2.559(5) 1_545 ?
O2 C1 1.262(8) . ?
O2Z H2Z1 0.9500 . ?
O2Z H2Z2 0.9500 . ?
O3 H3H 0.8400 . ?
O3 C7 1.369(9) . ?
O3Z H3Z1 0.9500 . ?
O3Z H3Z2 0.9500 . ?
O4 C10 1.270(9) . ?
O4Z H4Z1 0.9500 . ?
O4Z H4Z2 0.9500 . ?
O5 C10 1.246(9) . ?
O5Z H5Z1 0.9500 . ?
O5Z H5Z2 0.9500 . ?
O6 H6H 0.89(9) . ?
O6 C16 1.379(10) . ?
O6Z H6Z2 1.06(10) . ?
O6Z H6Z1 0.77(11) . ?
O7 C19 1.250(9) . ?
O7Z H70A 0.78(8) . ?
O7Z H70B 0.85(11) . ?
O8 C19 1.271(9) . ?
O8Z H80B 0.89(2) . ?
O8Z H80A 0.90(2) . ?
O9 H9H 0.77(11) . ?
O9 C25 1.396(10) . ?
O9Z H90A 0.90(11) . ?
O9Z H90B 0.84(10) . ?
O10 C28 1.242(8) . ?
O10Z H101 0.90(2) . ?
O10Z H100 0.90(2) . ?
O11 C28 1.286(8) . ?
O12 H12H 0.8400 . ?
O12 C34 1.378(10) . ?
O13 C37 1.270(8) . ?
O14 C37 1.264(9) . ?
O15 H15H 0.8400 . ?
O15 C43 1.368(10) . ?
O16 C46 1.249(9) . ?
O17 C46 1.278(9) . ?
O18 H18H 0.8400 . ?
O18 C52 1.394(11) . ?
O19 C55 1.265(8) . ?
O20 C55 1.272(8) . ?
O21 H21H 0.8400 . ?
O21 C61 1.385(11) . ?
O22 C64 1.269(9) . ?
O23 C64 1.279(9) . ?
O24 H24H 0.8400 . ?
O24 C70 1.395(10) . ?
O25 C73 1.281(9) . ?
O26 C73 1.241(10) . ?
O27 H27H 0.8400 . ?
O27 C79 1.407(9) . ?
O28 C82 1.264(9) . ?
O29 C82 1.272(8) . ?
O30 H30H 0.98(12) . ?
O30 C88 1.391(11) . ?
O31 C91 1.262(8) . ?
O32 C91 1.246(8) . ?
O33 H33H 0.8400 . ?
O33 C97 1.374(9) . ?
O34 C100 1.259(8) . ?
O35 La1 2.574(5) 1_565 ?
O35 C100 1.267(8) . ?
O36 H36H 0.8400 . ?
O36 C106 1.369(9) . ?
C1 C2 1.485(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.514(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.505(11) . ?
C4 C5 1.392(12) . ?
C4 C9 1.387(12) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(12) . ?
C6 H6 0.9500 . ?
C6 C7 1.356(11) . ?
C7 C8 1.387(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.380(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.503(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.531(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.510(11) . ?
C13 C14 1.391(12) . ?
C13 C18 1.377(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.408(12) . ?
C15 H15 0.9500 . ?
C15 C16 1.368(12) . ?
C16 C17 1.381(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.392(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.500(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.509(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.496(11) . ?
C22 C23 1.376(12) . ?
C22 C27 1.406(12) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(11) . ?
C24 H24 0.9500 . ?
C24 C25 1.377(12) . ?
C25 C26 1.374(12) . ?
C26 H26 0.9500 . ?
C26 C27 1.380(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.498(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.525(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.500(10) . ?
C31 C32 1.388(11) . ?
C31 C36 1.395(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.396(11) . ?
C33 H33 0.9500 . ?
C33 C34 1.382(11) . ?
C34 C35 1.364(12) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.507(11) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.528(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.517(11) . ?
C40 C41 1.385(12) . ?
C40 C45 1.392(12) . ?
C41 H41 0.9500 . ?
C41 C42 1.384(11) . ?
C42 H42 0.9500 . ?
C42 C43 1.393(12) . ?
C43 C44 1.381(13) . ?
C44 H44 0.9500 . ?
C44 C45 1.390(13) . ?
C45 H45 0.9500 . ?
C46 C47 1.504(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.420(13) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.515(13) . ?
C49 C50 1.385(12) . ?
C49 C54 1.385(12) . ?
C50 H50 0.9500 . ?
C50 C51 1.394(12) . ?
C51 H51 0.9500 . ?
C51 C52 1.342(12) . ?
C52 C53 1.374(12) . ?
C53 H53 0.9500 . ?
C53 C54 1.406(12) . ?
C54 H54 0.9500 . ?
C55 C56 1.501(11) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.437(14) . ?
C58 C59 1.374(14) . ?
C58 C63 1.417(14) . ?
C58 C57 1.518(13) . ?
C59 H59 0.9500 . ?
C59 C60 1.404(12) . ?
C60 H60 0.9500 . ?
C60 C61 1.379(14) . ?
C61 C62 1.370(15) . ?
C62 H62 0.9500 . ?
C62 C63 1.366(13) . ?
C63 H63 0.9500 . ?
C64 C65 1.502(11) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.522(11) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C67 1.479(11) . ?
C67 C68 1.432(12) . ?
C67 C72 1.376(11) . ?
C68 H68 0.9500 . ?
C68 C69 1.363(12) . ?
C69 H69 0.9500 . ?
C69 C70 1.361(12) . ?
C70 C71 1.391(11) . ?
C71 H71 0.9500 . ?
C71 C72 1.377(11) . ?
C72 H72 0.9500 . ?
C73 C74 1.500(11) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 C75 1.518(11) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75 C76 1.515(10) . ?
C76 C77 1.368(12) . ?
C76 C81 1.363(12) . ?
C77 H77 0.9500 . ?
C77 C78 1.389(12) . ?
C78 H78 0.9500 . ?
C78 C79 1.388(13) . ?
C79 C80 1.348(13) . ?
C80 H80 0.9500 . ?
C80 C81 1.383(12) . ?
C81 H81 0.9500 . ?
C82 C83 1.502(10) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C84 1.509(10) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 C85 1.516(11) . ?
C85 C86 1.384(11) . ?
C85 C90 1.373(12) . ?
C86 H86 0.9500 . ?
C86 C87 1.368(12) . ?
C87 H87 0.9500 . ?
C87 C88 1.343(14) . ?
C88 C89 1.393(13) . ?
C89 H89 0.9500 . ?
C89 C90 1.397(11) . ?
C90 H90 0.9500 . ?
C91 C92 1.505(10) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.525(11) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C93 C94 1.499(11) . ?
C94 C95 1.382(11) . ?
C94 C99 1.394(12) . ?
C95 H95 0.9500 . ?
C95 C96 1.397(11) . ?
C96 H96 0.9500 . ?
C96 C97 1.374(11) . ?
C97 C98 1.405(11) . ?
C98 H98 0.9500 . ?
C98 C99 1.380(12) . ?
C99 H99 0.9500 . ?
C100 C101 1.491(10) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C101 C102 1.511(11) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C102 C103 1.487(12) . ?
C103 C104 1.392(12) . ?
C103 C108 1.383(12) . ?
C104 H104 0.9500 . ?
C104 C105 1.384(12) . ?
C105 H105 0.9500 . ?
C105 C106 1.373(12) . ?
C106 C107 1.381(11) . ?
C107 H107 0.9500 . ?
C107 C108 1.391(11) . ?
C108 H108 0.9500 . ?
O11Z H11Z 0.8400 . ?
O11Z C1Z 1.388(15) . ?
C1Z H1Z3 0.9800 . ?
C1Z H1Z4 0.9800 . ?
C1Z H1Z5 0.9800 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O2 48.53(15) . . ?
O1 La1 O4 68.97(17) . . ?
O1 La1 O5 68.32(15) . . ?
O1 La1 O8 123.85(15) . . ?
O1 La1 O10 66.52(16) . . ?
O1 La1 O11 72.94(16) . . ?
O1 La1 C1 24.29(17) . . ?
O1Z La1 O1 92.03(16) . . ?
O1Z La1 O2 70.31(16) . . ?
O1Z La1 O2Z 68.03(17) . . ?
O1Z La1 O4 135.28(16) . . ?
O1Z La1 O5 158.92(15) . . ?
O1Z La1 O7 122.43(18) . . ?
O1Z La1 O8 133.48(16) . . ?
O1Z La1 O10 62.22(15) . . ?
O1Z La1 O11 108.56(16) . . ?
O1Z La1 O35 69.40(16) . 1_545 ?
O1Z La1 C1 79.96(18) . . ?
O2 La1 O5 99.82(14) . . ?
O2 La1 O8 155.38(15) . . ?
O2 La1 O10 94.37(15) . . ?
O2 La1 C1 24.26(17) . . ?
O2Z La1 O1 144.10(17) . . ?
O2Z La1 O2 136.30(15) . . ?
O2Z La1 O4 145.64(17) . . ?
O2Z La1 O5 123.87(15) . . ?
O2Z La1 O7 74.78(18) . . ?
O2Z La1 O8 65.68(15) . . ?
O2Z La1 O10 77.68(16) . . ?
O2Z La1 O11 85.15(17) . . ?
O2Z La1 O35 91.48(16) . 1_545 ?
O2Z La1 C1 146.64(18) . . ?
O4 La1 O2 66.87(16) . . ?
O4 La1 O5 45.83(14) . . ?
O4 La1 O8 88.51(16) . . ?
O4 La1 O10 132.56(16) . . ?
O4 La1 C1 66.24(19) . . ?
O5 La1 C1 84.19(17) . . ?
O7 La1 O1 139.24(18) . . ?
O7 La1 O2 119.21(17) . . ?
O7 La1 O4 70.98(18) . . ?
O7 La1 O5 78.64(16) . . ?
O7 La1 O8 47.32(16) . . ?
O7 La1 O10 146.12(18) . . ?
O7 La1 O11 110.31(16) . . ?
O7 La1 O35 69.35(16) . 1_545 ?
O7 La1 C1 133.6(2) . . ?
O8 La1 O5 59.92(14) . . ?
O8 La1 C1 143.94(17) . . ?
O10 La1 O5 101.30(14) . . ?
O10 La1 O8 102.91(15) . . ?
O10 La1 C1 79.35(19) . . ?
O11 La1 O2 120.75(15) . . ?
O11 La1 O4 103.89(15) . . ?
O11 La1 O5 59.55(15) . . ?
O11 La1 O8 63.43(14) . . ?
O11 La1 O10 47.47(14) . . ?
O11 La1 C1 96.78(18) . . ?
O35 La1 O1 109.66(16) 1_545 . ?
O35 La1 O2 61.53(15) 1_545 . ?
O35 La1 O4 79.31(15) 1_545 . ?
O35 La1 O5 123.29(15) 1_545 . ?
O35 La1 O8 115.75(14) 1_545 . ?
O35 La1 O10 131.04(14) 1_545 . ?
O35 La1 O11 176.56(16) 1_545 . ?
O35 La1 C1 85.65(18) 1_545 . ?
O3Z La2 La1 101.33(12) . . ?
O3Z La2 O5 73.08(16) . . ?
O3Z La2 O13 128.81(17) . . ?
O3Z La2 O14 139.02(16) . . ?
O3Z La2 O16 107.23(17) . . ?
O3Z La2 O17 76.92(16) . . ?
O3Z La2 O20 68.74(16) . . ?
O3Z La2 C37 137.57(19) . . ?
O3Z La2 C46 92.63(19) . . ?
O5 La2 La1 45.68(12) . . ?
O5 La2 O13 136.23(16) . . ?
O5 La2 O14 140.94(16) . . ?
O5 La2 O16 73.66(17) . . ?
O5 La2 O17 101.08(16) . . ?
O5 La2 O20 141.47(16) . . ?
O5 La2 C37 148.11(18) . . ?
O5 La2 C46 87.21(19) . . ?
O8 La2 La1 43.18(12) . . ?
O8 La2 O3Z 79.22(16) . . ?
O8 La2 O5 71.39(18) . . ?
O8 La2 O13 76.51(17) . . ?
O8 La2 O14 125.96(16) . . ?
O8 La2 O16 140.65(17) . . ?
O8 La2 O17 156.13(16) . . ?
O8 La2 O20 105.69(16) . . ?
O8 La2 C37 101.74(19) . . ?
O8 La2 C46 158.47(19) . . ?
O11 La2 La1 36.47(11) . . ?
O11 La2 O3Z 136.67(17) . . ?
O11 La2 O5 67.68(16) . . ?
O11 La2 O8 71.61(16) . . ?
O11 La2 O13 74.51(17) . . ?
O11 La2 O14 84.30(16) . . ?
O11 La2 O16 78.88(16) . . ?
O11 La2 O17 127.58(16) . . ?
O11 La2 O20 149.68(16) . . ?
O11 La2 C37 80.55(18) . . ?
O11 La2 C46 102.90(19) . . ?
O13 La2 La1 90.60(11) . . ?
O13 La2 O16 120.08(17) . . ?
O13 La2 O17 119.52(16) . . ?
O13 La2 O20 75.53(16) . . ?
O13 La2 C37 25.32(18) . . ?
O13 La2 C46 122.93(19) . . ?
O14 La2 La1 119.15(11) . . ?
O14 La2 O13 50.29(16) . . ?
O14 La2 O16 74.67(16) . . ?
O14 La2 O17 74.39(15) . . ?
O14 La2 O20 72.99(15) . . ?
O14 La2 C37 25.15(17) . . ?
O14 La2 C46 72.65(18) . . ?
O16 La2 La1 98.40(11) . . ?
O16 La2 O17 49.63(15) . . ?
O16 La2 C37 98.38(19) . . ?
O16 La2 C46 24.48(18) . . ?
O17 La2 La1 143.23(11) . . ?
O17 La2 C37 96.05(18) . . ?
O17 La2 C46 25.16(18) . . ?
O20 La2 La1 148.71(10) . . ?
O20 La2 O16 112.86(15) . . ?
O20 La2 O17 65.59(15) . . ?
O20 La2 C37 70.32(17) . . ?
O20 La2 C46 89.46(18) . . ?
C37 La2 La1 107.82(14) . . ?
C37 La2 C46 97.7(2) . . ?
C46 La2 La1 121.24(15) . . ?
O4Z La3 La4 101.69(12) . . ?
O4Z La3 O17 69.94(16) . . ?
O4Z La3 O19 107.13(17) . . ?
O4Z La3 O20 77.21(15) . . ?
O4Z La3 O22 138.75(16) . . ?
O4Z La3 O23 128.96(17) . . ?
O4Z La3 O32 73.14(17) . . ?
O4Z La3 C55 94.07(18) . . ?
O4Z La3 C64 138.78(19) . . ?
O17 La3 La4 149.14(11) . . ?
O17 La3 O19 112.25(16) . . ?
O17 La3 O20 65.32(15) . . ?
O17 La3 O22 72.04(15) . . ?
O17 La3 O23 73.79(16) . . ?
O17 La3 C55 88.30(17) . . ?
O17 La3 C64 70.07(18) . . ?
O19 La3 La4 98.62(11) . . ?
O19 La3 O20 49.49(15) . . ?
O19 La3 O22 73.36(16) . . ?
O19 La3 C55 24.64(17) . . ?
O19 La3 C64 96.80(19) . . ?
O20 La3 La4 143.70(10) . . ?
O20 La3 C55 25.01(16) . . ?
O20 La3 C64 94.92(18) . . ?
O22 La3 La4 119.24(11) . . ?
O22 La3 O20 72.87(15) . . ?
O22 La3 C55 69.25(18) . . ?
O22 La3 C64 25.16(18) . . ?
O23 La3 La4 91.54(12) . . ?
O23 La3 O19 119.35(16) . . ?
O23 La3 O20 117.73(16) . . ?
O23 La3 O22 50.41(16) . . ?
O23 La3 C55 119.65(18) . . ?
O23 La3 C64 25.28(18) . . ?
O25 La3 La4 49.04(13) . . ?
O25 La3 O4Z 78.27(16) . . ?
O25 La3 O17 100.28(18) . . ?
O25 La3 O19 147.00(18) . . ?
O25 La3 O20 154.71(16) . . ?
O25 La3 O22 124.34(16) . . ?
O25 La3 O23 74.20(17) . . ?
O25 La3 O29 74.14(17) . . ?
O25 La3 O32 71.95(17) . . ?
O25 La3 C55 165.58(19) . . ?
O25 La3 C64 99.4(2) . . ?
O29 La3 La4 35.13(11) . . ?
O29 La3 O4Z 136.08(16) . . ?
O29 La3 O17 148.10(16) . . ?
O29 La3 O19 80.79(16) . . ?
O29 La3 O20 129.26(15) . . ?
O29 La3 O22 85.17(15) . . ?
O29 La3 O23 74.49(17) . . ?
O29 La3 O32 66.19(16) . . ?
O29 La3 C55 104.49(18) . . ?
O29 La3 C64 79.77(18) . . ?
O32 La3 La4 41.93(11) . . ?
O32 La3 O17 143.08(16) . . ?
O32 La3 O19 78.51(16) . . ?
O32 La3 O20 106.37(16) . . ?
O32 La3 O22 142.59(16) . . ?
O32 La3 O23 133.44(16) . . ?
O32 La3 C55 94.22(18) . . ?
O32 La3 C64 145.95(18) . . ?
C55 La3 La4 122.37(13) . . ?
C64 La3 La4 107.39(14) . . ?
C64 La3 C55 94.4(2) . . ?
O2 La4 O6Z 68.72(18) 1_565 . ?
O2 La4 O28 131.83(15) 1_565 . ?
O2 La4 O29 175.79(16) 1_565 . ?
O2 La4 O31 77.97(15) 1_565 . ?
O2 La4 O32 122.42(15) 1_565 . ?
O2 La4 O34 110.61(16) 1_565 . ?
O2 La4 O35 62.56(15) 1_565 . ?
O2 La4 C82 156.09(18) 1_565 . ?
O2 La4 C100 86.28(17) 1_565 . ?
O5Z La4 O2 96.58(16) . 1_565 ?
O5Z La4 O6Z 67.05(18) . . ?
O5Z La4 O28 75.37(17) . . ?
O5Z La4 O29 79.38(17) . . ?
O5Z La4 O31 142.78(17) . . ?
O5Z La4 O32 117.89(15) . . ?
O5Z La4 O34 143.63(17) . . ?
O5Z La4 O35 141.87(16) . . ?
O5Z La4 C82 77.30(18) . . ?
O5Z La4 C100 153.47(18) . . ?
O6Z La4 O28 64.43(18) . . ?
O6Z La4 O29 110.39(17) . . ?
O6Z La4 O31 138.70(17) . . ?
O6Z La4 O32 164.97(18) . . ?
O6Z La4 O34 100.16(18) . . ?
O6Z La4 O35 75.40(17) . . ?
O6Z La4 C82 87.8(2) . . ?
O6Z La4 C100 89.86(19) . . ?
O26 La4 O2 73.98(16) . 1_565 ?
O26 La4 O5Z 73.57(18) . . ?
O26 La4 O6Z 120.7(2) . . ?
O26 La4 O28 141.69(18) . . ?
O26 La4 O29 103.54(16) . . ?
O26 La4 O31 69.52(19) . . ?
O26 La4 O32 73.88(17) . . ?
O26 La4 O34 136.06(18) . . ?
O26 La4 O35 123.59(17) . . ?
O26 La4 C82 124.61(19) . . ?
O26 La4 C100 131.97(19) . . ?
O28 La4 O32 102.16(15) . . ?
O28 La4 C82 24.31(17) . . ?
O28 La4 C100 83.08(18) . . ?
O29 La4 O28 48.50(14) . . ?
O29 La4 O31 104.49(15) . . ?
O29 La4 O32 59.28(14) . . ?
O29 La4 O34 73.57(16) . . ?
O29 La4 O35 121.45(15) . . ?
O29 La4 C82 24.24(17) . . ?
O29 La4 C100 97.87(17) . . ?
O31 La4 O28 134.93(16) . . ?
O31 La4 O32 46.29(14) . . ?
O31 La4 O35 67.77(15) . . ?
O31 La4 C82 120.73(18) . . ?
O31 La4 C100 63.65(18) . . ?
O32 La4 C82 79.97(17) . . ?
O32 La4 C100 81.40(16) . . ?
O34 La4 O28 68.55(17) . . ?
O34 La4 O31 69.06(17) . . ?
O34 La4 O32 67.23(15) . . ?
O34 La4 O35 48.84(15) . . ?
O34 La4 C82 68.02(18) . . ?
O34 La4 C100 24.40(17) . . ?
O35 La4 O28 94.71(15) . . ?
O35 La4 O32 100.13(14) . . ?
O35 La4 C82 108.40(17) . . ?
O35 La4 C100 24.69(16) . . ?
C100 La4 C82 89.42(19) . . ?
C1 O1 La1 99.8(4) . . ?
La1 O1Z H1Z1 120.0 . . ?
La1 O1Z H1Z2 120.0 . . ?
H1Z1 O1Z H1Z2 120.0 . . ?
La4 O2 La1 117.13(17) 1_545 . ?
C1 O2 La1 93.3(4) . . ?
C1 O2 La4 148.7(5) . 1_545 ?
La1 O2Z H2Z1 120.0 . . ?
La1 O2Z H2Z2 120.0 . . ?
H2Z1 O2Z H2Z2 120.0 . . ?
C7 O3 H3H 109.5 . . ?
La2 O3Z H3Z1 120.0 . . ?
La2 O3Z H3Z2 120.0 . . ?
H3Z1 O3Z H3Z2 120.0 . . ?
C10 O4 La1 102.9(5) . . ?
La3 O4Z H4Z1 120.0 . . ?
La3 O4Z H4Z2 120.0 . . ?
H4Z1 O4Z H4Z2 120.0 . . ?
La2 O5 La1 96.70(16) . . ?
C10 O5 La1 87.4(5) . . ?
C10 O5 La2 168.0(5) . . ?
La4 O5Z H5Z1 120.0 . . ?
La4 O5Z H5Z2 120.0 . . ?
H5Z1 O5Z H5Z2 120.0 . . ?
C16 O6 H6H 110(6) . . ?
La4 O6Z H6Z2 115(5) . . ?
La4 O6Z H6Z1 109(8) . . ?
H6Z2 O6Z H6Z1 123(10) . . ?
C19 O7 La1 103.0(5) . . ?
H70A O7Z H70B 103(9) . . ?
La2 O8 La1 100.81(17) . . ?
C19 O8 La1 88.5(4) . . ?
C19 O8 La2 142.3(5) . . ?
H80B O8Z H80A 99(10) . . ?
C25 O9 H9H 111(9) . . ?
H90A O9Z H90B 116(9) . . ?
C28 O10 La1 91.0(4) . . ?
H101 O10Z H100 97(10) . . ?
La2 O11 La1 109.21(17) . . ?
C28 O11 La1 100.8(4) . . ?
C28 O11 La2 149.9(5) . . ?
C34 O12 H12H 109.5 . . ?
C37 O13 La2 94.6(4) . . ?
C37 O14 La2 95.6(4) . . ?
C43 O15 H15H 109.5 . . ?
C46 O16 La2 96.1(5) . . ?
La3 O17 La2 116.54(18) . . ?
C46 O17 La2 94.3(4) . . ?
C46 O17 La3 143.0(5) . . ?
C52 O18 H18H 109.5 . . ?
C55 O19 La3 97.9(4) . . ?
La2 O20 La3 112.51(17) . . ?
C55 O20 La2 146.7(5) . . ?
C55 O20 La3 91.8(4) . . ?
C61 O21 H21H 109.5 . . ?
C64 O22 La3 94.3(4) . . ?
C64 O23 La3 96.4(4) . . ?
C70 O24 H24H 109.5 . . ?
C73 O25 La3 140.5(5) . . ?
C73 O26 La4 113.9(5) . . ?
C79 O27 H27H 109.5 . . ?
C82 O28 La4 94.0(4) . . ?
La3 O29 La4 111.80(17) . . ?
C82 O29 La3 149.7(5) . . ?
C82 O29 La4 98.4(4) . . ?
C88 O30 H30H 102(7) . . ?
C91 O31 La4 100.1(4) . . ?
La3 O32 La4 102.35(16) . . ?
C91 O32 La3 167.1(5) . . ?
C91 O32 La4 88.6(4) . . ?
C97 O33 H33H 109.5 . . ?
C100 O34 La4 96.8(4) . . ?
La1 O35 La4 118.75(18) 1_565 . ?
C100 O35 La1 143.8(5) . 1_565 ?
C100 O35 La4 94.0(4) . . ?
C106 O36 H36H 109.5 . . ?
O1 C1 La1 55.9(4) . . ?
O1 C1 C2 119.6(6) . . ?
O2 C1 La1 62.5(4) . . ?
O2 C1 O1 118.4(7) . . ?
O2 C1 C2 122.0(7) . . ?
C2 C1 La1 175.2(6) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 C3 112.3(6) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 C2 110.4(7) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C5 C4 C3 120.9(8) . . ?
C9 C4 C3 121.7(8) . . ?
C9 C4 C5 117.3(8) . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.8(8) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.5(8) . . ?
C7 C6 H6 119.8 . . ?
O3 C7 C8 117.0(7) . . ?
C6 C7 O3 122.8(7) . . ?
C6 C7 C8 120.1(8) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(8) . . ?
C9 C8 H8 120.4 . . ?
C4 C9 H9 119.0 . . ?
C8 C9 C4 122.1(8) . . ?
C8 C9 H9 119.0 . . ?
O4 C10 C11 118.0(7) . . ?
O5 C10 O4 121.5(7) . . ?
O5 C10 C11 120.3(7) . . ?
C10 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
C10 C11 C12 114.9(7) . . ?
H11A C11 H11B 107.5 . . ?
C12 C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 C11 112.9(7) . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C14 C13 C12 120.3(8) . . ?
C18 C13 C12 121.8(8) . . ?
C18 C13 C14 117.9(8) . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(8) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.4(8) . . ?
C16 C15 H15 120.3 . . ?
O6 C16 C17 118.3(8) . . ?
C15 C16 O6 121.7(8) . . ?
C15 C16 C17 120.0(8) . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(8) . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 121.3(8) . . ?
C13 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
O7 C19 La1 53.9(4) . . ?
O7 C19 O8 121.2(7) . . ?
O7 C19 C20 120.5(7) . . ?
O8 C19 La1 67.3(4) . . ?
O8 C19 C20 118.3(7) . . ?
C20 C19 La1 174.2(6) . . ?
C19 C20 H20A 108.2 . . ?
C19 C20 H20B 108.2 . . ?
C19 C20 C21 116.5(7) . . ?
H20A C20 H20B 107.3 . . ?
C21 C20 H20A 108.2 . . ?
C21 C20 H20B 108.2 . . ?
C20 C21 H21A 108.6 . . ?
C20 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 C20 114.7(7) . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
C23 C22 C21 121.0(8) . . ?
C23 C22 C27 117.3(7) . . ?
C27 C22 C21 121.7(8) . . ?
C22 C23 H23 118.7 . . ?
C22 C23 C24 122.6(8) . . ?
C24 C23 H23 118.7 . . ?
C23 C24 H24 121.0 . . ?
C25 C24 C23 118.0(8) . . ?
C25 C24 H24 121.0 . . ?
C24 C25 O9 116.7(8) . . ?
C26 C25 O9 121.4(8) . . ?
C26 C25 C24 121.9(8) . . ?
C25 C26 H26 120.6 . . ?
C25 C26 C27 118.8(8) . . ?
C27 C26 H26 120.6 . . ?
C22 C27 H27 119.4 . . ?
C26 C27 C22 121.3(8) . . ?
C26 C27 H27 119.4 . . ?
O10 C28 La1 65.3(4) . . ?
O10 C28 O11 119.5(6) . . ?
O10 C28 C29 123.1(6) . . ?
O11 C28 La1 55.1(3) . . ?
O11 C28 C29 117.3(6) . . ?
C29 C28 La1 165.4(5) . . ?
C28 C29 H29A 108.8 . . ?
C28 C29 H29B 108.8 . . ?
C28 C29 C30 113.9(6) . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
C29 C30 H30A 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C31 C30 C29 113.2(7) . . ?
C31 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
C32 C31 C30 120.8(7) . . ?
C32 C31 C36 118.3(7) . . ?
C36 C31 C30 120.8(7) . . ?
C31 C32 H32 119.6 . . ?
C31 C32 C33 120.8(7) . . ?
C33 C32 H32 119.6 . . ?
C32 C33 H33 120.6 . . ?
C34 C33 C32 118.9(8) . . ?
C34 C33 H33 120.6 . . ?
O12 C34 C33 117.5(8) . . ?
C35 C34 O12 121.0(8) . . ?
C35 C34 C33 121.5(7) . . ?
C34 C35 H35 120.3 . . ?
C34 C35 C36 119.4(8) . . ?
C36 C35 H35 120.3 . . ?
C31 C36 H36 119.5 . . ?
C35 C36 C31 121.1(8) . . ?
C35 C36 H36 119.5 . . ?
O13 C37 La2 60.1(4) . . ?
O13 C37 C38 120.7(7) . . ?
O14 C37 La2 59.2(4) . . ?
O14 C37 O13 118.6(6) . . ?
O14 C37 C38 120.6(6) . . ?
C38 C37 La2 169.0(5) . . ?
C37 C38 H38A 108.5 . . ?
C37 C38 H38B 108.5 . . ?
C37 C38 C39 115.2(7) . . ?
H38A C38 H38B 107.5 . . ?
C39 C38 H38A 108.5 . . ?
C39 C38 H38B 108.5 . . ?
C38 C39 H39A 108.9 . . ?
C38 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 C38 113.2(7) . . ?
C40 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C41 C40 C39 121.7(7) . . ?
C41 C40 C45 118.3(8) . . ?
C45 C40 C39 120.0(8) . . ?
C40 C41 H41 119.5 . . ?
C42 C41 C40 121.1(8) . . ?
C42 C41 H41 119.5 . . ?
C41 C42 H42 120.0 . . ?
C41 C42 C43 120.0(8) . . ?
C43 C42 H42 120.0 . . ?
O15 C43 C42 122.9(8) . . ?
O15 C43 C44 117.4(8) . . ?
C44 C43 C42 119.7(8) . . ?
C43 C44 H44 120.1 . . ?
C43 C44 C45 119.8(8) . . ?
C45 C44 H44 120.1 . . ?
C40 C45 H45 119.4 . . ?
C44 C45 C40 121.1(9) . . ?
C44 C45 H45 119.4 . . ?
O16 C46 La2 59.4(4) . . ?
O16 C46 O17 120.0(7) . . ?
O16 C46 C47 121.8(7) . . ?
O17 C46 La2 60.5(4) . . ?
O17 C46 C47 118.2(7) . . ?
C47 C46 La2 177.5(6) . . ?
C46 C47 H47A 108.3 . . ?
C46 C47 H47B 108.3 . . ?
H47A C47 H47B 107.4 . . ?
C48 C47 C46 115.8(8) . . ?
C48 C47 H47A 108.3 . . ?
C48 C47 H47B 108.3 . . ?
C47 C48 H48A 107.6 . . ?
C47 C48 H48B 107.6 . . ?
C47 C48 C49 118.8(9) . . ?
H48A C48 H48B 107.0 . . ?
C49 C48 H48A 107.6 . . ?
C49 C48 H48B 107.6 . . ?
C50 C49 C48 123.2(8) . . ?
C54 C49 C48 117.8(8) . . ?
C54 C49 C50 118.6(8) . . ?
C49 C50 H50 119.4 . . ?
C49 C50 C51 121.1(8) . . ?
C51 C50 H50 119.4 . . ?
C50 C51 H51 120.4 . . ?
C52 C51 C50 119.1(8) . . ?
C52 C51 H51 120.4 . . ?
C51 C52 O18 118.0(8) . . ?
C51 C52 C53 122.1(9) . . ?
C53 C52 O18 119.9(8) . . ?
C52 C53 H53 120.5 . . ?
C52 C53 C54 119.0(8) . . ?
C54 C53 H53 120.5 . . ?
C49 C54 C53 119.9(8) . . ?
C49 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
O19 C55 La3 57.4(4) . . ?
O19 C55 O20 120.0(7) . . ?
O19 C55 C56 119.9(7) . . ?
O20 C55 La3 63.2(4) . . ?
O20 C55 C56 120.1(6) . . ?
C56 C55 La3 169.6(6) . . ?
C55 C56 H56A 108.3 . . ?
C55 C56 H56B 108.3 . . ?
H56A C56 H56B 107.4 . . ?
C57 C56 C55 116.1(8) . . ?
C57 C56 H56A 108.3 . . ?
C57 C56 H56B 108.3 . . ?
C59 C58 C63 119.3(8) . . ?
C59 C58 C57 122.9(10) . . ?
C63 C58 C57 117.7(10) . . ?
C58 C59 H59 120.1 . . ?
C58 C59 C60 119.8(9) . . ?
C60 C59 H59 120.1 . . ?
C59 C60 H60 120.6 . . ?
C61 C60 C59 118.8(9) . . ?
C61 C60 H60 120.6 . . ?
C60 C61 O21 120.8(10) . . ?
C62 C61 O21 116.7(9) . . ?
C62 C61 C60 122.5(9) . . ?
C61 C62 H62 120.7 . . ?
C63 C62 C61 118.6(10) . . ?
C63 C62 H62 120.7 . . ?
C58 C63 H63 119.5 . . ?
C62 C63 C58 121.0(10) . . ?
C62 C63 H63 119.5 . . ?
O22 C64 La3 60.5(4) . . ?
O22 C64 O23 118.7(7) . . ?
O22 C64 C65 121.7(7) . . ?
O23 C64 La3 58.3(4) . . ?
O23 C64 C65 119.6(7) . . ?
C65 C64 La3 175.1(5) . . ?
C64 C65 H65A 108.9 . . ?
C64 C65 H65B 108.9 . . ?
C64 C65 C66 113.3(6) . . ?
H65A C65 H65B 107.7 . . ?
C66 C65 H65A 108.9 . . ?
C66 C65 H65B 108.9 . . ?
C65 C66 H66A 109.2 . . ?
C65 C66 H66B 109.2 . . ?
H66A C66 H66B 107.9 . . ?
C67 C66 C65 112.2(6) . . ?
C67 C66 H66A 109.2 . . ?
C67 C66 H66B 109.2 . . ?
C68 C67 C66 120.3(8) . . ?
C72 C67 C66 122.9(8) . . ?
C72 C67 C68 116.5(8) . . ?
C67 C68 H68 119.5 . . ?
C69 C68 C67 121.1(8) . . ?
C69 C68 H68 119.5 . . ?
C68 C69 H69 120.0 . . ?
C70 C69 C68 120.1(8) . . ?
C70 C69 H69 120.0 . . ?
C69 C70 O24 117.6(8) . . ?
C69 C70 C71 121.1(8) . . ?
C71 C70 O24 121.3(7) . . ?
C70 C71 H71 120.8 . . ?
C72 C71 C70 118.4(8) . . ?
C72 C71 H71 120.8 . . ?
C67 C72 C71 122.8(8) . . ?
C67 C72 H72 118.6 . . ?
C71 C72 H72 118.6 . . ?
O25 C73 C74 117.1(7) . . ?
O26 C73 O25 121.8(7) . . ?
O26 C73 C74 121.1(7) . . ?
C73 C74 H74A 108.4 . . ?
C73 C74 H74B 108.4 . . ?
C73 C74 C75 115.4(7) . . ?
H74A C74 H74B 107.5 . . ?
C75 C74 H74A 108.4 . . ?
C75 C74 H74B 108.4 . . ?
C74 C75 H75A 109.8 . . ?
C74 C75 H75B 109.8 . . ?
H75A C75 H75B 108.3 . . ?
C76 C75 C74 109.3(6) . . ?
C76 C75 H75A 109.8 . . ?
C76 C75 H75B 109.8 . . ?
C77 C76 C75 119.8(8) . . ?
C81 C76 C75 123.1(8) . . ?
C81 C76 C77 117.0(8) . . ?
C76 C77 H77 118.8 . . ?
C76 C77 C78 122.5(9) . . ?
C78 C77 H77 118.7 . . ?
C77 C78 H78 121.1 . . ?
C79 C78 C77 117.9(9) . . ?
C79 C78 H78 121.1 . . ?
C78 C79 O27 118.1(8) . . ?
C80 C79 O27 121.1(9) . . ?
C80 C79 C78 120.8(8) . . ?
C79 C80 H80 120.4 . . ?
C79 C80 C81 119.3(9) . . ?
C81 C80 H80 120.4 . . ?
C76 C81 C80 122.5(9) . . ?
C76 C81 H81 118.8 . . ?
C80 C81 H81 118.8 . . ?
O28 C82 La4 61.7(4) . . ?
O28 C82 O29 118.8(7) . . ?
O28 C82 C83 121.1(6) . . ?
O29 C82 La4 57.3(4) . . ?
O29 C82 C83 120.0(7) . . ?
C83 C82 La4 173.9(5) . . ?
C82 C83 H83A 108.9 . . ?
C82 C83 H83B 108.9 . . ?
C82 C83 C84 113.5(7) . . ?
H83A C83 H83B 107.7 . . ?
C84 C83 H83A 108.9 . . ?
C84 C83 H83B 108.9 . . ?
C83 C84 H84A 109.0 . . ?
C83 C84 H84B 109.0 . . ?
C83 C84 C85 112.8(7) . . ?
H84A C84 H84B 107.8 . . ?
C85 C84 H84A 109.0 . . ?
C85 C84 H84B 109.0 . . ?
C86 C85 C84 122.3(8) . . ?
C90 C85 C84 120.0(7) . . ?
C90 C85 C86 117.7(7) . . ?
C85 C86 H86 119.4 . . ?
C87 C86 C85 121.2(8) . . ?
C87 C86 H86 119.4 . . ?
C86 C87 H87 119.5 . . ?
C88 C87 C86 121.0(8) . . ?
C88 C87 H87 119.5 . . ?
O30 C88 C89 115.3(9) . . ?
C87 C88 O30 124.5(9) . . ?
C87 C88 C89 120.2(8) . . ?
C88 C89 H89 120.9 . . ?
C88 C89 C90 118.2(9) . . ?
C90 C89 H89 120.9 . . ?
C85 C90 C89 121.7(8) . . ?
C85 C90 H90 119.2 . . ?
C89 C90 H90 119.2 . . ?
O31 C91 La4 56.3(3) . . ?
O31 C91 C92 118.2(6) . . ?
O32 C91 La4 67.7(4) . . ?
O32 C91 O31 120.4(7) . . ?
O32 C91 C92 121.5(6) . . ?
C92 C91 La4 158.2(5) . . ?
C91 C92 H92A 108.7 . . ?
C91 C92 H92B 108.7 . . ?
C91 C92 C93 114.3(6) . . ?
H92A C92 H92B 107.6 . . ?
C93 C92 H92A 108.7 . . ?
C93 C92 H92B 108.7 . . ?
C92 C93 H93A 108.8 . . ?
C92 C93 H93B 108.8 . . ?
H93A C93 H93B 107.7 . . ?
C94 C93 C92 113.6(7) . . ?
C94 C93 H93A 108.8 . . ?
C94 C93 H93B 108.8 . . ?
C95 C94 C93 121.8(8) . . ?
C95 C94 C99 118.0(7) . . ?
C99 C94 C93 120.1(8) . . ?
C94 C95 H95 119.1 . . ?
C94 C95 C96 121.8(7) . . ?
C96 C95 H95 119.1 . . ?
C95 C96 H96 120.3 . . ?
C97 C96 C95 119.4(8) . . ?
C97 C96 H96 120.3 . . ?
O33 C97 C98 121.8(7) . . ?
C96 C97 O33 118.4(7) . . ?
C96 C97 C98 119.9(7) . . ?
C97 C98 H98 120.1 . . ?
C99 C98 C97 119.8(8) . . ?
C99 C98 H98 120.1 . . ?
C94 C99 H99 119.4 . . ?
C98 C99 C94 121.2(8) . . ?
C98 C99 H99 119.4 . . ?
O34 C100 La4 58.8(4) . . ?
O34 C100 O35 119.2(7) . . ?
O34 C100 C101 120.1(6) . . ?
O35 C100 La4 61.4(4) . . ?
O35 C100 C101 120.7(6) . . ?
C101 C100 La4 169.6(5) . . ?
C100 C101 H10A 109.1 . . ?
C100 C101 H10B 109.1 . . ?
C100 C101 C102 112.6(6) . . ?
H10A C101 H10B 107.8 . . ?
C102 C101 H10A 109.1 . . ?
C102 C101 H10B 109.1 . . ?
C101 C102 H10C 109.1 . . ?
C101 C102 H10D 109.1 . . ?
H10C C102 H10D 107.9 . . ?
C103 C102 C101 112.3(7) . . ?
C103 C102 H10C 109.1 . . ?
C103 C102 H10D 109.1 . . ?
C104 C103 C102 122.3(8) . . ?
C108 C103 C102 120.7(8) . . ?
C108 C103 C104 117.0(8) . . ?
C103 C104 H104 118.6 . . ?
C105 C104 C103 122.7(8) . . ?
C105 C104 H104 118.6 . . ?
C104 C105 H105 120.8 . . ?
C106 C105 C104 118.4(8) . . ?
C106 C105 H105 120.8 . . ?
O36 C106 C105 121.6(7) . . ?
O36 C106 C107 117.5(7) . . ?
C105 C106 C107 121.0(8) . . ?
C106 C107 H107 120.3 . . ?
C106 C107 C108 119.3(8) . . ?
C108 C107 H107 120.3 . . ?
C103 C108 C107 121.5(8) . . ?
C103 C108 H108 119.2 . . ?
C107 C108 H108 119.2 . . ?
C1Z O11Z H11Z 109.5 . . ?
O11Z C1Z H1Z3 109.5 . . ?
O11Z C1Z H1Z4 109.5 . . ?
O11Z C1Z H1Z5 109.5 . . ?
H1Z3 C1Z H1Z4 109.5 . . ?
H1Z3 C1Z H1Z5 109.5 . . ?
H1Z4 C1Z H1Z5 109.5 . . ?
C56 C57 C58 118.0(10) . . ?
C56 C57 H57A 107.8 . . ?
C56 C57 H57B 107.8 . . ?
C58 C57 H57A 107.8 . . ?
C58 C57 H57B 107.8 . . ?
H57A C57 H57B 107.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1Z H1Z1 O18 0.95 2.21 3.119(9) 159.7 1_645
O1Z H1Z2 O31 0.95 2.14 2.654(7) 112.3 1_545
O2Z H2Z1 O18 0.95 1.92 2.829(8) 160.7 1_645
O2Z H2Z2 O3 0.95 1.99 2.758(8) 136.0 1_655
O3 H3H O13 0.84 1.81 2.646(7) 175.6 1_455
O3Z H3Z1 O9 0.95 1.77 2.680(8) 158.1 2_766
O3Z H3Z2 O22 0.95 1.85 2.676(7) 143.1 .
O4Z H4Z2 O14 0.95 1.88 2.644(7) 135.6 .
O5Z H5Z2 O24 0.95 1.90 2.849(8) 173.8 2_676
O6 H6H O9Z 0.89(9) 1.84(10) 2.725(9) 173(9) 1_455
O9 H9H O30 0.77(11) 1.86(11) 2.626(9) 169(12) .
O15 H15H O33 0.84 2.04 2.791(9) 148.2 2_767
O18 H18H O11Z 0.84 1.86 2.649(10) 155.1 .
O24 H24H O10Z 0.84 1.82 2.620(9) 157.8 2_676
O27 H27H O12 0.84 1.87 2.652(9) 154.9 .
O30 H30H O4 0.98(12) 2.11(12) 2.803(9) 126(10) 2_766
O33 H33H O8Z 0.84 1.82 2.662(8) 175.1 1_655
O36 H36H O23 0.84 1.79 2.606(7) 164.1 1_655
O8Z H80B O16 0.89(2) 1.96(4) 2.819(8) 161(8) .
O9Z H90A O19 0.90(11) 1.96(11) 2.858(8) 177(9) .
O9Z H90B O34 0.84(10) 1.98(10) 2.791(8) 162(9) .
O8Z H80A O1 0.90(2) 1.87(3) 2.764(8) 172(12) .
O10Z H101 O6 0.90(2) 2.14(4) 3.018(9) 164(11) 2_676
O7Z H70B O10 0.85(11) 1.85(12) 2.683(8) 167(11) .
O10Z H100 O28 0.90(2) 2.15(12) 2.710(8) 120(10) .
O11Z H11Z O7Z 0.84 1.81 2.647(10) 172.2 1_465
O6Z H6Z2 O4 1.06(10) 1.66(10) 2.661(8) 154(8) 1_565

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_compound7
_database_code_depnum_ccdc_archive 'CCDC 1055964'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_audit_creation_date             2015-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H27 Lu O9, H2 O'
_chemical_formula_sum            'C27 H29 Lu O10'
_chemical_formula_weight         688.47
_chemical_melting_point          ?
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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.345(3)
_cell_length_b                   8.0505(16)
_cell_length_c                   24.550(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.45(3)
_cell_angle_gamma                90
_cell_volume                     2621.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26141
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      28.216
_cell_measurement_theta_min      1.536
_shelx_estimated_absorpt_T_max   0.832
_shelx_estimated_absorpt_T_min   0.251
_exptl_absorpt_coefficient_mu    3.824
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_process_details   SORTAV
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.8318
_exptl_transmission_factor_min   0.2508
_diffrn_reflns_av_R_equivalents  0.1513
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25249
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.536
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4263
_reflns_number_total             6018
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         3.640
_refine_diff_density_min         -3.885
_refine_diff_density_rms         0.379
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6018
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0714
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1857
_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.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3H = O6-H6H = O9-H9H = O1Z-H1ZA = O1Z-H1ZB
 0.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C17)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.52601(3) 0.90940(4) 0.76211(2) 0.01080(15) Uani 1 1 d . . . . .
O1 O 0.5976(5) 0.7966(8) 0.8436(2) 0.0215(15) Uani 1 1 d . . . . .
C1 C 0.5517(7) 0.6612(12) 0.8423(4) 0.017(2) Uani 1 1 d . . . . .
O1Z O 0.7950(5) 0.8479(10) 0.8910(3) 0.0291(17) Uani 1 1 d D . . . .
H1ZA H 0.731(6) 0.802(17) 0.873(5) 0.09(5) Uiso 1 1 d D . . . .
H1ZB H 0.796(9) 0.900(12) 0.927(2) 0.05(4) Uiso 1 1 d D . . . .
O2 O 0.4946(5) 0.6281(8) 0.7978(2) 0.0153(14) Uani 1 1 d . . . . .
C2 C 0.5629(7) 0.5449(12) 0.8895(4) 0.017(2) Uani 1 1 d . . . . .
H2A H 0.6209 0.4707 0.8857 0.021 Uiso 1 1 calc R . . . .
H2B H 0.5017 0.4747 0.8878 0.021 Uiso 1 1 calc R . . . .
O3 O 0.2396(5) 0.9183(9) 1.0309(3) 0.035(2) Uani 1 1 d D . . . .
H3H H 0.181(5) 0.872(14) 1.010(4) 0.042 Uiso 1 1 d DR . . . .
C3 C 0.5789(7) 0.6281(13) 0.9461(4) 0.020(2) Uani 1 1 d . . . . .
H3A H 0.6036 0.5430 0.9735 0.024 Uiso 1 1 calc R . . . .
H3B H 0.6326 0.7128 0.9456 0.024 Uiso 1 1 calc R . . . .
O4 O 0.3846(5) 0.8421(9) 0.7115(2) 0.0224(15) Uani 1 1 d . . . . .
C4 C 0.4869(7) 0.7106(11) 0.9650(4) 0.0157(19) Uani 1 1 d . . . . .
O5 O 0.3451(5) 0.5722(8) 0.7089(3) 0.0230(16) Uani 1 1 d . . . . .
C5 C 0.4958(7) 0.7804(13) 1.0172(4) 0.022(2) Uani 1 1 d . . . . .
H5 H 0.5600 0.7799 1.0384 0.027 Uiso 1 1 calc R . . . .
O6 O -0.0273(4) 0.7119(9) 0.8855(2) 0.0210(15) Uani 1 1 d D . . . .
H6H H -0.090(4) 0.771(11) 0.890(4) 0.025 Uiso 1 1 d DR . . . .
C6 C 0.4148(7) 0.8508(13) 1.0395(4) 0.022(2) Uani 1 1 d . . . . .
H6 H 0.4232 0.8969 1.0753 0.027 Uiso 1 1 calc R . . . .
O7 O 0.6193(5) 0.7805(8) 0.7081(3) 0.0229(15) Uani 1 1 d . . . . .
C7 C 0.3203(7) 0.8526(12) 1.0082(4) 0.021(2) Uani 1 1 d . . . . .
O8 O 0.5767(5) 0.5214(9) 0.6848(3) 0.0230(15) Uani 1 1 d . . . . .
C8 C 0.3111(7) 0.7884(12) 0.9559(4) 0.021(2) Uani 1 1 d . . . . .
H8 H 0.2474 0.7907 0.9343 0.025 Uiso 1 1 calc R . . . .
O9 O 1.0606(5) 0.7178(9) 0.4886(3) 0.0217(15) Uani 1 1 d D . . . .
H9H H 1.040(7) 0.766(12) 0.453(2) 0.026 Uiso 1 1 d DR . . . .
C9 C 0.3941(7) 0.7199(13) 0.9343(4) 0.021(2) Uani 1 1 d . . . . .
H9 H 0.3865 0.6789 0.8978 0.025 Uiso 1 1 calc R . . . .
C10 C 0.3239(7) 0.7220(12) 0.7003(3) 0.0145(19) Uani 1 1 d . . . . .
C11 C 0.2189(6) 0.7633(12) 0.6725(4) 0.018(2) Uani 1 1 d . . . . .
H11A H 0.1764 0.6625 0.6726 0.021 Uiso 1 1 calc R . . . .
H11B H 0.2244 0.7926 0.6338 0.021 Uiso 1 1 calc R . . . .
C12 C 0.1656(7) 0.9060(11) 0.6992(4) 0.020(2) Uani 1 1 d . . . . .
H12A H 0.2155 0.9935 0.7109 0.024 Uiso 1 1 calc R . . . .
H12B H 0.1142 0.9552 0.6716 0.024 Uiso 1 1 calc R . . . .
C13 C 0.1143(6) 0.8495(12) 0.7490(4) 0.0151(19) Uani 1 1 d . . . . .
C14 C 0.1636(6) 0.7580(11) 0.7920(4) 0.0154(19) Uani 1 1 d . . . . .
H14 H 0.2318 0.7261 0.7905 0.019 Uiso 1 1 calc R . . . .
C15 C 0.1161(7) 0.7120(12) 0.8371(4) 0.017(2) Uani 1 1 d . . . . .
H15 H 0.1514 0.6499 0.8660 0.021 Uiso 1 1 calc R . . . .
C16 C 0.0165(6) 0.7577(11) 0.8394(4) 0.0161(13) Uani 1 1 d . . . . .
C17 C -0.0353(6) 0.8461(12) 0.7969(4) 0.0161(13) Uani 1 1 d . . . . .
H17 H -0.1039 0.8756 0.7983 0.019 Uiso 1 1 calc R . . . .
C18 C 0.0140(7) 0.8912(12) 0.7523(4) 0.017(2) Uani 1 1 d . . . . .
H18 H -0.0217 0.9523 0.7232 0.021 Uiso 1 1 calc R . . . .
C19 C 0.6307(6) 0.6482(12) 0.6817(4) 0.016(2) Uani 1 1 d . . . . .
C20 C 0.7127(6) 0.6425(11) 0.6442(4) 0.0159(19) Uani 1 1 d . . . . .
H20A H 0.6826 0.6045 0.6076 0.019 Uiso 1 1 calc R . . . .
H20B H 0.7630 0.5583 0.6585 0.019 Uiso 1 1 calc R . . . .
C21 C 0.7672(7) 0.8044(12) 0.6372(4) 0.020(2) Uani 1 1 d . . . . .
H21A H 0.8001 0.8415 0.6733 0.024 Uiso 1 1 calc R . . . .
H21B H 0.7177 0.8903 0.6234 0.024 Uiso 1 1 calc R . . . .
C22 C 0.8464(7) 0.7876(12) 0.5976(4) 0.018(2) Uani 1 1 d . . . . .
C23 C 0.8353(6) 0.8642(12) 0.5480(4) 0.018(2) Uani 1 1 d . . . . .
H23 H 0.7780 0.9327 0.5386 0.022 Uiso 1 1 calc R . . . .
C24 C 0.9048(7) 0.8456(12) 0.5108(4) 0.019(2) Uani 1 1 d . . . . .
H24 H 0.8955 0.9007 0.4764 0.022 Uiso 1 1 calc R . . . .
C25 C 0.9883(6) 0.7454(12) 0.5244(4) 0.018(2) Uani 1 1 d . . . . .
C26 C 1.0024(7) 0.6679(12) 0.5752(4) 0.018(2) Uani 1 1 d . . . . .
H26 H 1.0597 0.5994 0.5848 0.022 Uiso 1 1 calc R . . . .
C27 C 0.9325(7) 0.6917(13) 0.6116(4) 0.024(2) Uani 1 1 d . . . . .
H27 H 0.9430 0.6419 0.6469 0.029 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O1 2.305(6) . ?
Lu1 O2 2.481(6) . ?
Lu1 O2 2.292(6) 2_656 ?
Lu1 O4 2.207(6) . ?
Lu1 O5 2.215(7) 2_656 ?
Lu1 O7 2.181(6) . ?
Lu1 O8 2.190(6) 2_656 ?
O1 C1 1.249(11) . ?
C1 O2 1.286(11) . ?
C1 C2 1.484(13) . ?
O1Z H1ZA 0.98(2) . ?
O1Z H1ZB 0.98(2) . ?
O2 Lu1 2.292(6) 2_646 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.537(13) . ?
O3 H3H 0.97(2) . ?
O3 C7 1.374(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.515(13) . ?
O4 C10 1.272(11) . ?
C4 C5 1.391(13) . ?
C4 C9 1.378(13) . ?
O5 Lu1 2.215(7) 2_646 ?
O5 C10 1.252(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(14) . ?
O6 H6H 0.98(2) . ?
O6 C16 1.381(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.401(13) . ?
O7 C19 1.264(11) . ?
C7 C8 1.376(13) . ?
O8 Lu1 2.190(6) 2_646 ?
O8 C19 1.257(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(13) . ?
O9 H9H 0.97(2) . ?
O9 C25 1.393(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.524(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.537(12) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.535(12) . ?
C13 C14 1.392(12) . ?
C13 C18 1.391(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(12) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(12) . ?
C16 C17 1.382(13) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.508(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.512(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.519(12) . ?
C22 C23 1.359(13) . ?
C22 C27 1.395(14) . ?
C23 H23 0.9500 . ?
C23 C24 1.381(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(13) . ?
C25 C26 1.390(13) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(13) . ?
C27 H27 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Lu1 O2 53.4(2) . . ?
O2 Lu1 O1 150.3(2) 2_656 . ?
O2 Lu1 O2 156.28(11) 2_656 . ?
O4 Lu1 O1 129.6(2) . . ?
O4 Lu1 O2 78.1(2) . 2_656 ?
O4 Lu1 O2 78.9(2) . . ?
O4 Lu1 O5 155.5(3) . 2_656 ?
O5 Lu1 O1 73.9(2) 2_656 . ?
O5 Lu1 O2 77.6(2) 2_656 2_656 ?
O5 Lu1 O2 125.6(2) 2_656 . ?
O7 Lu1 O1 97.5(2) . . ?
O7 Lu1 O2 84.9(2) . . ?
O7 Lu1 O2 90.6(2) . 2_656 ?
O7 Lu1 O4 92.9(2) . . ?
O7 Lu1 O5 90.1(2) . 2_656 ?
O7 Lu1 O8 175.2(3) . 2_656 ?
O8 Lu1 O1 82.6(2) 2_656 . ?
O8 Lu1 O2 91.6(2) 2_656 2_656 ?
O8 Lu1 O2 91.3(2) 2_656 . ?
O8 Lu1 O4 83.3(2) 2_656 . ?
O8 Lu1 O5 94.6(3) 2_656 2_656 ?
C1 O1 Lu1 99.6(5) . . ?
O1 C1 O2 116.4(8) . . ?
O1 C1 C2 121.6(8) . . ?
O2 C1 C2 122.0(9) . . ?
H1ZA O1Z H1ZB 119(10) . . ?
Lu1 O2 Lu1 119.1(2) 2_646 . ?
C1 O2 Lu1 90.2(5) . . ?
C1 O2 Lu1 136.1(6) . 2_646 ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
C1 C2 C3 115.0(8) . . ?
H2A C2 H2B 107.5 . . ?
C3 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
C7 O3 H3H 105(7) . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 C2 115.7(8) . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C10 O4 Lu1 142.4(6) . . ?
C5 C4 C3 118.0(8) . . ?
C9 C4 C3 124.4(8) . . ?
C9 C4 C5 117.5(9) . . ?
C10 O5 Lu1 141.0(6) . 2_646 ?
C4 C5 H5 118.7 . . ?
C6 C5 C4 122.5(9) . . ?
C6 C5 H5 118.7 . . ?
C16 O6 H6H 114(6) . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.8(9) . . ?
C7 C6 H6 120.6 . . ?
C19 O7 Lu1 145.3(6) . . ?
O3 C7 C6 118.7(9) . . ?
O3 C7 C8 122.1(9) . . ?
C8 C7 C6 119.2(9) . . ?
C19 O8 Lu1 140.4(6) . 2_646 ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.8(9) . . ?
C9 C8 H8 119.6 . . ?
C25 O9 H9H 111(6) . . ?
C4 C9 C8 121.0(9) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
O4 C10 C11 117.6(8) . . ?
O5 C10 O4 124.7(9) . . ?
O5 C10 C11 117.7(8) . . ?
C10 C11 H11A 108.6 . . ?
C10 C11 H11B 108.6 . . ?
C10 C11 C12 114.7(8) . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 C11 112.8(7) . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C14 C13 C12 123.1(8) . . ?
C18 C13 C12 119.5(8) . . ?
C18 C13 C14 117.4(8) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.9(8) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.3(8) . . ?
C16 C15 H15 120.4 . . ?
O6 C16 C15 117.3(8) . . ?
O6 C16 C17 122.3(7) . . ?
C17 C16 C15 120.4(8) . . ?
C16 C17 H17 120.3 . . ?
C16 C17 C18 119.3(8) . . ?
C18 C17 H17 120.3 . . ?
C13 C18 H18 119.1 . . ?
C17 C18 C13 121.8(9) . . ?
C17 C18 H18 119.1 . . ?
O7 C19 C20 118.4(8) . . ?
O8 C19 O7 123.5(8) . . ?
O8 C19 C20 118.1(9) . . ?
C19 C20 H20A 108.3 . . ?
C19 C20 H20B 108.3 . . ?
C19 C20 C21 115.8(8) . . ?
H20A C20 H20B 107.4 . . ?
C21 C20 H20A 108.3 . . ?
C21 C20 H20B 108.3 . . ?
C20 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C20 C21 C22 112.0(7) . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
C23 C22 C21 121.3(8) . . ?
C23 C22 C27 118.4(8) . . ?
C27 C22 C21 120.3(8) . . ?
C22 C23 H23 119.0 . . ?
C22 C23 C24 122.0(9) . . ?
C24 C23 H23 119.0 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.1(9) . . ?
C25 C24 H24 120.4 . . ?
C24 C25 O9 122.5(8) . . ?
C24 C25 C26 120.1(8) . . ?
C26 C25 O9 117.5(8) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.2(9) . . ?
C27 C26 H26 120.4 . . ?
C22 C27 H27 119.4 . . ?
C26 C27 C22 121.2(9) . . ?
C26 C27 H27 119.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1Z H1ZA O1 0.98(2) 1.85(6) 2.788(9) 159(13) .
O1Z H1ZB O3 0.98(2) 1.88(6) 2.763(10) 149(10) 3_677
O3 H3H O9 0.97(2) 1.78(4) 2.725(10) 164(10) 4_476
O6 H6H O1Z 0.98(2) 1.66(3) 2.629(9) 170(9) 1_455
O9 H9H O6 0.97(2) 1.80(4) 2.727(9) 159(9) 4_675

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_compound2b
_database_code_depnum_ccdc_archive 'CCDC 1055965'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_audit_creation_date             2015-05-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C63 H67 Ce2 Na O23, 3(H2 O)'
_chemical_formula_sum            'C63 H73 Ce2 Na O26'
_chemical_formula_weight         1549.44
_chemical_melting_point          ?
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'
Na Na 0.0362 0.0249 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.0063(7)
_cell_length_b                   15.3267(7)
_cell_length_c                   16.4093(7)
_cell_angle_alpha                103.726(2)
_cell_angle_beta                 107.053(2)
_cell_angle_gamma                94.662(2)
_cell_volume                     3458.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    40363
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.190
_cell_measurement_theta_min      1.350
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.819
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1414
_diffrn_reflns_av_unetI/netI     0.2013
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29745
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.350
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9547
_reflns_number_total             11923
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         6.454
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.397
_refine_ls_extinction_coef       13241(92)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         11923
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.1257
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3033
_refine_ls_wR_factor_ref         0.3247
_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.
 
 After refinement of the primary molecule including part of lattice solvent
 molecule, attempts to model the residual electron density in the lattice 
 voids as solvent molecules gave unsatisfactory refinements. Subsequently,
 the electron density in voids was accounted for using PLATON/SQUEEZE
 (see below). 
;
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 0.500 0.500 90 30
2 0.000 0.500 0.000 141 44
3 0.252 0.457 0.752 31 9
4 0.748 0.543 0.248 31 9
_platon_squeeze_details          
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 18.82316 -17.82316
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H15H of O15, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  H3 of O3
3. Restrained distances
 C31-C32 = C32-C33 = C33-C34 = C34-C35 = C35-C36 = C36-C31
 1.39 with sigma of 0.02
 C40-C41 = C44-C45
 1.4 with sigma of 0.02
 C43-C44 = C45-C40
 1.39 with sigma of 0.02
 C58-C59 = C60-C61 = C62-C63
 1.39 with sigma of 0.02
 C59-C60 = C61-C62 = C63-C58
 1.39 with sigma of 0.02
 C52-C53 = C53-C54
 1.4 with sigma of 0.02
 C49-C50
 1.39 with sigma of 0.02
 C47-C48 = C46-C47 = C48-C49
 1.4 with sigma of 0.002
 C41-C42 = C42-C43 = C39-C40
 1.4 with sigma of 0.002
 C49-C54
 1.4 with sigma of 0.002
 C29-C30
 1.57 with sigma of 0.02
 C31-C33 = C32-C34 = C33-C35 = C34-C36 = C35-C31 = C36-C32
 2.39 with sigma of 0.02
4. Restrained planarity
 C40, C41, C42, C43, C44, C45
 with sigma of 0.1
5. Rigid bond restraints
 C30, C31
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C46, C47
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C56, C57
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C61, C62
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C7, C8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C24, C25
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C34, C35
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C47, C48
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C60, C61
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O20, C55
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C11, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C16, C17
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C22, C23
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C13, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C62, C63
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C29, C30
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A
with sigma of 0.05 and sigma for terminal atoms of 0.01
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 1.7A with sigma
of 0.05 and sigma for terminal atoms of 0.01
C47 \\sim C48 \\sim C49 \\sim C52 \\sim C53: within 1.7A with sigma of 0.05 and
sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C63) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) = Uanis(C39)
Uanis(C50) = Uanis(C51)
Uanis(C57) = Uanis(C56)
Uanis(C30) = Uanis(C29)
Uanis(C34) = Uanis(C33)
Uanis(C58) = Uanis(C59)
Uanis(C55) = Uanis(O19)
7. Others
 Fixed k1: basf(-17.82316)
8.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B), C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B),
  C47(H47A,H47B), C48(H48A,H48B), C56(H56A,H56B), C57(H57A,H57B)
8.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27), C41(H41), C42(H42), C44(H44), C45(H45),
  C50(H50), C51(H51), C53(H53), C54(H54), C59(H59), C60(H60), C62(H62),
 C63(H63), C33(H33), C35(H35), C36(H36)
8.c Tetrahedral OH refined with riding coordinates:
 O3(H3)
8.d X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2)
8.e Idealised tetrahedral OH refined as rotating group:
 O15(H15H)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.56172(8) 0.01785(8) 0.14252(7) 0.0511(5) Uani 1 1 d . . . . .
Ce2 Ce 0.53198(8) 0.04323(8) 0.39350(7) 0.0520(5) Uani 1 1 d . . . . .
Na2 Na 0.3269(6) -0.1150(5) 0.0313(6) 0.061(2) Uani 1 1 d . . . . .
O1 O 0.4734(9) 0.0874(12) 0.2528(8) 0.061(4) Uani 1 1 d . . . . .
O1Z O 0.6449(13) -0.0571(12) 0.4492(11) 0.077(5) Uani 1 1 d . . . . .
H1Z1 H 0.7096 -0.0439 0.4542 0.092 Uiso 1 1 calc R . . . .
H1Z2 H 0.6232 -0.1083 0.4653 0.092 Uiso 1 1 calc R . . . .
O2 O 0.3901(9) 0.0282(12) 0.1109(8) 0.068(5) Uani 1 1 d . . . . .
O2Z O 0.2752(16) -0.2617(11) -0.0597(12) 0.088(6) Uani 1 1 d . . . . .
H2Z1 H 0.3052 -0.2852 -0.1019 0.105 Uiso 1 1 calc R . . . .
H2Z2 H 0.2239 -0.2986 -0.0550 0.105 Uiso 1 1 calc R . . . .
O3 O -0.0216(17) 0.3402(12) 0.2619(18) 0.112(8) Uani 1 1 d . . . . .
H3 H -0.0737 0.3072 0.2505 0.168 Uiso 1 1 calc R . . . .
O3Z O 0.7025(14) -0.2254(13) 0.1905(12) 0.087(5) Uani 1 1 d . . . . .
O4 O 0.5690(10) -0.0634(9) 0.2678(9) 0.060(4) Uani 1 1 d . . . . .
O4Z O -0.2056(11) 0.2607(11) 0.2353(11) 0.071(4) Uani 1 1 d . . . . .
O5 O 0.4650(10) -0.1302(9) 0.1369(11) 0.061(4) Uani 1 1 d . . . . .
O5Z O 0.4255(14) 0.7131(10) 0.6886(11) 0.072(4) Uani 1 1 d . . . . .
O6 O 0.4274(15) -0.6117(12) 0.3101(14) 0.089(5) Uani 1 1 d . . . . .
O7 O 0.6935(10) -0.0733(11) 0.1372(9) 0.063(4) Uani 1 1 d . . . . .
O8 O 0.7027(11) 0.0468(11) 0.0872(9) 0.065(4) Uani 1 1 d . . . . .
O9 O 1.2509(11) -0.1189(14) 0.1378(10) 0.074(5) Uani 1 1 d . . . . .
O10 O 0.5485(10) 0.1870(9) 0.1456(9) 0.053(3) Uani 1 1 d . . . . .
O11 O 0.5131(10) 0.0919(9) 0.0135(8) 0.053(3) Uani 1 1 d . . . . .
O12 O 0.231(3) 0.545(2) -0.093(3) 0.187(16) Uani 1 1 d . . . . .
O13 O 0.7019(12) 0.1128(11) 0.2635(10) 0.070(4) Uani 1 1 d . . . . .
O14 O 0.6724(12) 0.1128(11) 0.3887(9) 0.070(4) Uani 1 1 d . . . . .
O15 O 1.2576(13) 0.1681(17) 0.6341(12) 0.094(6) Uani 1 1 d . . . . .
H15H H 1.2634 0.1657 0.6860 0.113 Uiso 1 1 calc GR . . . .
O16 O 0.3694(11) -0.0696(8) 0.3066(8) 0.061(4) Uani 1 1 d . . . . .
O17 O 0.4336(9) -0.0768(9) 0.4389(9) 0.054(3) Uani 1 1 d . . . . .
O18 O -0.0506(15) -0.5061(16) 0.216(3) 0.172(16) Uani 1 1 d . . . . .
O19 O 0.3987(12) 0.1246(10) 0.4296(9) 0.061(3) Uani 1 1 d . . . . .
O20 O 0.5364(12) 0.2172(10) 0.4456(10) 0.066(4) Uani 1 1 d . U . . .
O21 O 0.2510(14) 0.6377(11) 0.6231(11) 0.081(5) Uani 1 1 d . . . . .
C1 C 0.3940(14) 0.0831(17) 0.1925(11) 0.058(6) Uani 1 1 d . . . . .
C2 C 0.3245(17) 0.1352(15) 0.2119(12) 0.065(6) Uani 1 1 d . . . . .
H2A H 0.3545 0.1999 0.2355 0.078 Uiso 1 1 calc R . . . .
H2B H 0.3074 0.1172 0.2601 0.078 Uiso 1 1 calc R . . . .
C3 C 0.2336(18) 0.1290(18) 0.1378(17) 0.073(7) Uani 1 1 d . . . . .
H3A H 0.2035 0.0644 0.1117 0.087 Uiso 1 1 calc R . . . .
H3B H 0.2487 0.1513 0.0907 0.087 Uiso 1 1 calc R . . . .
C4 C 0.1639(14) 0.1844(15) 0.1697(14) 0.056(5) Uani 1 1 d . . . . .
C5 C 0.191(2) 0.2730(19) 0.215(2) 0.093(9) Uani 1 1 d . . . . .
H5 H 0.2548 0.2987 0.2277 0.111 Uiso 1 1 calc R . . . .
C6 C 0.1304(15) 0.3329(18) 0.248(2) 0.090(9) Uani 1 1 d . . . . .
H6 H 0.1509 0.3960 0.2765 0.108 Uiso 1 1 calc R . . . .
C7 C 0.0389(15) 0.2883(15) 0.2321(14) 0.059(5) Uani 1 1 d . U . . .
C8 C 0.0104(18) 0.1982(14) 0.1821(15) 0.065(6) Uani 1 1 d . U . . .
H8 H -0.0541 0.1718 0.1648 0.078 Uiso 1 1 calc R . . . .
C9 C 0.0748(15) 0.1449(13) 0.1563(17) 0.064(6) Uani 1 1 d . . . . .
H9 H 0.0558 0.0813 0.1294 0.077 Uiso 1 1 calc R . . . .
C10 C 0.5127(13) -0.1324(11) 0.2148(11) 0.041(4) Uani 1 1 d . U . . .
C11 C 0.5061(15) -0.2199(15) 0.2425(14) 0.058(5) Uani 1 1 d . U . . .
H11A H 0.4870 -0.2076 0.2965 0.070 Uiso 1 1 calc R . . . .
H11B H 0.5699 -0.2370 0.2586 0.070 Uiso 1 1 calc R . . . .
C12 C 0.4364(19) -0.3027(19) 0.1720(16) 0.081(8) Uani 1 1 d . U . . .
H12A H 0.3718 -0.2874 0.1554 0.098 Uiso 1 1 calc R . . . .
H12B H 0.4554 -0.3177 0.1181 0.098 Uiso 1 1 calc R . . . .
C13 C 0.4375(15) -0.3856(14) 0.2111(17) 0.066(6) Uani 1 1 d . U . . .
C14 C 0.3514(16) -0.427(2) 0.2218(17) 0.079(7) Uani 1 1 d . U . . .
H14 H 0.2933 -0.4063 0.2004 0.094 Uiso 1 1 calc R . . . .
C15 C 0.355(2) -0.496(2) 0.2629(19) 0.083(7) Uani 1 1 d . U . . .
H15 H 0.3044 -0.5132 0.2825 0.100 Uiso 1 1 calc R . . . .
C16 C 0.428(2) -0.5375(14) 0.2750(18) 0.074(7) Uani 1 1 d . U . . .
C17 C 0.5152(17) -0.4977(13) 0.2703(15) 0.060(5) Uani 1 1 d . U . . .
H17 H 0.5707 -0.5235 0.2882 0.073 Uiso 1 1 calc R . . . .
C18 C 0.5185(17) -0.4183(14) 0.2382(19) 0.074(7) Uani 1 1 d . . . . .
H18 H 0.5762 -0.3898 0.2363 0.088 Uiso 1 1 calc R . . . .
C19 C 0.7373(11) -0.0188(12) 0.1108(12) 0.042(4) Uani 1 1 d . . . . .
C20 C 0.8388(13) -0.0301(15) 0.1190(14) 0.054(5) Uani 1 1 d . . . . .
H20A H 0.8500 -0.0209 0.0649 0.065 Uiso 1 1 calc R . . . .
H20B H 0.8799 0.0202 0.1694 0.065 Uiso 1 1 calc R . . . .
C21 C 0.8700(16) -0.110(2) 0.1309(18) 0.076(7) Uani 1 1 d . . . . .
H21A H 0.8269 -0.1617 0.0830 0.092 Uiso 1 1 calc R . . . .
H21B H 0.8647 -0.1175 0.1877 0.092 Uiso 1 1 calc R . . . .
C22 C 0.9724(15) -0.1181(18) 0.1315(17) 0.066(6) Uani 1 1 d . U . . .
C23 C 1.0490(18) -0.068(2) 0.2034(15) 0.080(8) Uani 1 1 d . U . . .
H23 H 1.0336 -0.0313 0.2514 0.096 Uiso 1 1 calc R . . . .
C24 C 1.1413(18) -0.0634(14) 0.2143(14) 0.065(6) Uani 1 1 d . U . . .
H24 H 1.1887 -0.0285 0.2672 0.078 Uiso 1 1 calc R . . . .
C25 C 1.1634(14) -0.1165(16) 0.1383(12) 0.054(5) Uani 1 1 d . U . . .
C26 C 1.084(2) -0.168(2) 0.0623(16) 0.086(9) Uani 1 1 d . . . . .
H26 H 1.0932 -0.2065 0.0116 0.103 Uiso 1 1 calc R . . . .
C27 C 0.9922(17) -0.1584(16) 0.0677(15) 0.069(6) Uani 1 1 d . . . . .
H27 H 0.9407 -0.1866 0.0155 0.083 Uiso 1 1 calc R . . . .
C28 C 0.5091(14) 0.1673(13) 0.0628(12) 0.053(4) Uani 1 1 d . U . . .
C29 C 0.477(3) 0.240(2) 0.022(2) 0.119(9) Uani 1 1 d D U . . .
H29A H 0.4338 0.2120 -0.0389 0.143 Uiso 1 1 calc R . . . .
H29B H 0.5320 0.2771 0.0189 0.143 Uiso 1 1 calc R . . . .
C30 C 0.425(3) 0.302(2) 0.073(2) 0.119(9) Uani 1 1 d D U . . .
H30A H 0.4712 0.3383 0.1309 0.143 Uiso 1 1 calc R . . . .
H30B H 0.3768 0.2646 0.0856 0.143 Uiso 1 1 calc R . . . .
C37 C 0.7276(16) 0.1207(19) 0.3447(14) 0.069(6) Uani 1 1 d . . . . .
C38 C 0.838(3) 0.141(4) 0.390(2) 0.154(15) Uani 1 1 d . . . . .
H38A H 0.8676 0.1407 0.3438 0.185 Uiso 1 1 calc R . . . .
H38B H 0.8547 0.2037 0.4308 0.185 Uiso 1 1 calc R . . . .
C39 C 0.879(2) 0.079(4) 0.441(2) 0.154(15) Uani 1 1 d D . . . .
H39A H 0.8418 0.0692 0.4796 0.185 Uiso 1 1 calc R . . . .
H39B H 0.8768 0.0197 0.3995 0.185 Uiso 1 1 calc R . . . .
C40 C 0.9720(18) 0.118(3) 0.491(2) 0.206(19) Uani 1 1 d D U . . .
C41 C 1.0362(19) 0.089(3) 0.448(3) 0.156(14) Uani 1 1 d D U . . .
H41 H 1.0154 0.0544 0.3872 0.187 Uiso 1 1 calc R . . . .
C42 C 1.132(2) 0.112(3) 0.4972(17) 0.169(16) Uani 1 1 d D U . . .
H42 H 1.1773 0.0961 0.4682 0.203 Uiso 1 1 calc R . . . .
C43 C 1.165(2) 0.158(2) 0.5877(17) 0.135(14) Uani 1 1 d D U . . .
C44 C 1.1013(16) 0.191(3) 0.628(2) 0.153(15) Uani 1 1 d D U . . .
H44 H 1.1223 0.2273 0.6885 0.184 Uiso 1 1 calc R . . . .
C45 C 1.0056(19) 0.171(3) 0.579(3) 0.195(18) Uani 1 1 d D U . . .
H45 H 0.9614 0.1946 0.6064 0.234 Uiso 1 1 calc R . . . .
C46 C 0.3676(16) -0.1083(14) 0.3608(15) 0.063(5) Uani 1 1 d D U . . .
C47 C 0.3046(16) -0.1902(16) 0.3328(19) 0.095(8) Uani 1 1 d D U . . .
H47A H 0.2818 -0.2089 0.2672 0.114 Uiso 1 1 calc R . . . .
H47B H 0.3406 -0.2371 0.3522 0.114 Uiso 1 1 calc R . . . .
C48 C 0.225(2) -0.1918(19) 0.362(2) 0.141(12) Uani 1 1 d D U . . .
H48A H 0.1885 -0.1457 0.3418 0.170 Uiso 1 1 calc R . . . .
H48B H 0.2475 -0.1738 0.4271 0.170 Uiso 1 1 calc R . . . .
C49 C 0.166(3) -0.276(2) 0.331(2) 0.148(15) Uani 1 1 d D U . . .
C50 C 0.166(3) -0.346(2) 0.373(2) 0.112(8) Uani 1 1 d D . . . .
H50 H 0.2192 -0.3448 0.4228 0.135 Uiso 1 1 calc R . . . .
C51 C 0.093(2) -0.417(3) 0.344(2) 0.112(8) Uani 1 1 d . . . . .
H51 H 0.0901 -0.4567 0.3794 0.135 Uiso 1 1 calc R . . . .
C52 C 0.019(3) -0.432(2) 0.260(2) 0.111(10) Uani 1 1 d D U . . .
C53 C 0.020(3) -0.369(3) 0.212(3) 0.143(14) Uani 1 1 d D U . . .
H53 H -0.0256 -0.3766 0.1554 0.172 Uiso 1 1 calc R . . . .
C54 C 0.092(2) -0.292(2) 0.2508(18) 0.109(10) Uani 1 1 d D U . . .
H54 H 0.0913 -0.2466 0.2196 0.131 Uiso 1 1 calc R . . . .
C55 C 0.4497(18) 0.2000(15) 0.4512(13) 0.061(3) Uani 1 1 d . U . . .
C56 C 0.416(2) 0.2817(19) 0.500(2) 0.094(6) Uani 1 1 d . U . . .
H56A H 0.4133 0.2727 0.5571 0.113 Uiso 1 1 calc R . . . .
H56B H 0.4620 0.3372 0.5132 0.113 Uiso 1 1 calc R . . . .
C57 C 0.322(2) 0.2958(19) 0.449(2) 0.094(6) Uani 1 1 d . U . . .
H57A H 0.2742 0.2438 0.4415 0.113 Uiso 1 1 calc R . . . .
H57B H 0.3224 0.2999 0.3901 0.113 Uiso 1 1 calc R . . . .
C58 C 0.299(2) 0.3833(14) 0.4992(16) 0.087(6) Uani 1 1 d D . . . .
C59 C 0.336(2) 0.4611(12) 0.4823(16) 0.087(6) Uani 1 1 d D . . . .
H59 H 0.3711 0.4564 0.4419 0.105 Uiso 1 1 calc R . . . .
C60 C 0.3216(19) 0.5450(15) 0.5257(13) 0.085(9) Uani 1 1 d D U . . .
H60 H 0.3539 0.5986 0.5210 0.102 Uiso 1 1 calc R . . . .
C61 C 0.2613(19) 0.5529(18) 0.576(2) 0.099(9) Uani 1 1 d D U . . .
C62 C 0.216(3) 0.4707(17) 0.577(3) 0.136(15) Uani 1 1 d D U . . .
H62 H 0.1668 0.4741 0.6030 0.163 Uiso 1 1 calc R . . . .
C63 C 0.235(2) 0.3843(18) 0.545(2) 0.104(9) Uani 1 1 d D U . . .
H63 H 0.2064 0.3310 0.5538 0.124 Uiso 1 1 calc R . . . .
C31 C 0.378(2) 0.367(2) 0.022(3) 0.143(11) Uani 1 1 d D U . . .
C34 C 0.284(2) 0.483(2) -0.062(3) 0.144(10) Uani 1 1 d D U . . .
C32 C 0.429(2) 0.433(3) 0.000(3) 0.143(12) Uani 1 1 d D U . . .
C33 C 0.379(2) 0.487(2) -0.049(3) 0.144(10) Uani 1 1 d D U . . .
H33 H 0.4109 0.5260 -0.0720 0.173 Uiso 1 1 calc R . . . .
C35 C 0.239(2) 0.433(3) -0.022(3) 0.149(12) Uani 1 1 d D U . . .
H35 H 0.1751 0.4364 -0.0258 0.179 Uiso 1 1 calc R . . . .
C36 C 0.287(2) 0.378(2) 0.024(3) 0.158(14) Uani 1 1 d D U . . .
H36 H 0.2593 0.3470 0.0567 0.189 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 Na2 4.190(8) 2_655 ?
Ce1 O1 2.625(14) . ?
Ce1 O2 2.499(15) . ?
Ce1 O4 2.626(13) . ?
Ce1 O5 2.559(14) . ?
Ce1 O7 2.522(12) . ?
Ce1 O8 2.582(16) . ?
Ce1 O10 2.606(12) . ?
Ce1 O11 2.570(13) 2_655 ?
Ce1 O11 2.583(13) . ?
Ce1 O13 2.483(16) . ?
Ce2 O1 2.492(12) . ?
Ce2 O1Z 2.500(15) . ?
Ce2 O4 2.541(16) . ?
Ce2 O14 2.314(16) . ?
Ce2 O16 2.661(15) . ?
Ce2 O17 2.560(13) 2_656 ?
Ce2 O17 2.640(14) . ?
Ce2 O19 2.580(15) . ?
Ce2 O20 2.589(15) . ?
Na2 Ce1 4.190(8) 2_655 ?
Na2 O2 2.236(18) . ?
Na2 O2Z 2.309(18) . ?
Na2 O5 2.349(17) . ?
Na2 O8 2.367(16) 2_655 ?
Na2 O9 2.360(16) 1_455 ?
Na2 O11 2.729(16) 2_655 ?
O1 C1 1.29(2) . ?
O1Z H1Z1 0.9500 . ?
O1Z H1Z2 0.9500 . ?
O2 C1 1.38(2) . ?
O2Z H2Z1 0.9500 . ?
O2Z H2Z2 0.9500 . ?
O3 H3 0.8400 . ?
O3 C7 1.37(3) . ?
O4 C10 1.25(2) . ?
O5 C10 1.28(2) . ?
O6 C16 1.39(3) . ?
O7 C19 1.25(2) . ?
O8 Na2 2.367(16) 2_655 ?
O8 C19 1.26(2) . ?
O9 Na2 2.360(16) 1_655 ?
O9 C25 1.32(2) . ?
O10 C28 1.26(2) . ?
O11 Ce1 2.570(13) 2_655 ?
O11 Na2 2.729(16) 2_655 ?
O11 C28 1.26(2) . ?
O12 C34 1.39(3) . ?
O13 C37 1.25(3) . ?
O14 C37 1.26(3) . ?
O15 H15H 0.8400 . ?
O15 C43 1.35(3) . ?
O16 C46 1.19(3) . ?
O17 Ce2 2.559(13) 2_656 ?
O17 C46 1.32(3) . ?
O18 C52 1.37(4) . ?
O19 C55 1.25(3) . ?
O20 C55 1.34(3) . ?
O21 C61 1.39(3) . ?
C1 C2 1.43(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.52(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.53(3) . ?
C4 C5 1.35(4) . ?
C4 C9 1.35(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.46(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.41(3) . ?
C7 C8 1.39(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.41(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.52(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.56(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.55(3) . ?
C13 C14 1.47(3) . ?
C13 C18 1.35(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.38(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.30(4) . ?
C16 C17 1.43(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.44(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.52(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.39(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.55(3) . ?
C22 C23 1.39(4) . ?
C22 C27 1.21(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.34(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.46(3) . ?
C25 C26 1.45(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.43(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.47(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.522(18) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.54(3) . ?
C37 C38 1.57(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.46(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.400(2) . ?
C40 C41 1.402(19) . ?
C40 C45 1.396(19) . ?
C41 H41 0.9500 . ?
C41 C42 1.400(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.400(2) . ?
C43 C44 1.387(19) . ?
C44 H44 0.9500 . ?
C44 C45 1.393(19) . ?
C45 H45 0.9500 . ?
C46 C47 1.400(2) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.400(2) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.400(2) . ?
C49 C50 1.410(18) . ?
C49 C54 1.400(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.36(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.44(4) . ?
C52 C53 1.396(19) . ?
C53 H53 0.9500 . ?
C53 C54 1.416(19) . ?
C54 H54 0.9500 . ?
C55 C56 1.53(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.46(4) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.52(3) . ?
C58 C59 1.396(19) . ?
C58 C63 1.388(19) . ?
C59 H59 0.9500 . ?
C59 C60 1.383(17) . ?
C60 H60 0.9500 . ?
C60 C61 1.382(19) . ?
C61 C62 1.393(19) . ?
C62 H62 0.9500 . ?
C62 C63 1.389(19) . ?
C63 H63 0.9500 . ?
C31 C32 1.392(17) . ?
C31 C36 1.389(17) . ?
C34 C33 1.379(17) . ?
C34 C35 1.375(17) . ?
C32 C33 1.391(16) . ?
C33 H33 0.9500 . ?
C35 H35 0.9500 . ?
C35 C36 1.378(17) . ?
C36 H36 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ce1 Na2 134.4(4) . 2_655 ?
O1 Ce1 O4 65.5(5) . . ?
O2 Ce1 Na2 111.9(3) . 2_655 ?
O2 Ce1 O1 51.2(4) . . ?
O2 Ce1 O4 94.1(4) . . ?
O2 Ce1 O5 67.9(5) . . ?
O2 Ce1 O7 151.1(6) . . ?
O2 Ce1 O8 142.5(4) . . ?
O2 Ce1 O10 74.3(5) . . ?
O2 Ce1 O11 72.8(4) . . ?
O2 Ce1 O11 77.4(5) . 2_655 ?
O4 Ce1 Na2 153.7(4) . 2_655 ?
O5 Ce1 Na2 136.1(4) . 2_655 ?
O5 Ce1 O1 81.8(5) . . ?
O5 Ce1 O4 50.1(5) . . ?
O5 Ce1 O8 131.3(5) . . ?
O5 Ce1 O10 141.6(4) . . ?
O5 Ce1 O11 120.5(5) . . ?
O5 Ce1 O11 65.4(5) . 2_655 ?
O7 Ce1 Na2 77.9(4) . 2_655 ?
O7 Ce1 O1 139.7(4) . . ?
O7 Ce1 O4 77.3(5) . . ?
O7 Ce1 O5 86.0(5) . . ?
O7 Ce1 O8 50.9(5) . . ?
O7 Ce1 O10 132.3(5) . . ?
O7 Ce1 O11 80.5(4) . 2_655 ?
O7 Ce1 O11 113.3(5) . . ?
O8 Ce1 Na2 30.6(3) . 2_655 ?
O8 Ce1 O1 145.0(5) . . ?
O8 Ce1 O4 123.2(4) . . ?
O8 Ce1 O10 83.9(5) . . ?
O8 Ce1 O11 69.8(4) . . ?
O10 Ce1 Na2 65.1(3) . 2_655 ?
O10 Ce1 O1 69.4(5) . . ?
O10 Ce1 O4 129.2(4) . . ?
O11 Ce1 Na2 39.2(3) . 2_655 ?
O11 Ce1 Na2 71.8(3) 2_655 2_655 ?
O11 Ce1 O1 126.9(4) 2_655 . ?
O11 Ce1 O1 105.9(4) . . ?
O11 Ce1 O4 112.3(4) 2_655 . ?
O11 Ce1 O4 166.7(5) . . ?
O11 Ce1 O8 83.7(5) 2_655 . ?
O11 Ce1 O10 112.8(4) 2_655 . ?
O11 Ce1 O10 50.0(4) . . ?
O11 Ce1 O11 63.8(5) 2_655 . ?
O13 Ce1 Na2 86.5(4) . 2_655 ?
O13 Ce1 O1 82.4(5) . . ?
O13 Ce1 O2 130.3(5) . . ?
O13 Ce1 O4 79.0(5) . . ?
O13 Ce1 O5 128.7(5) . . ?
O13 Ce1 O7 75.7(5) . . ?
O13 Ce1 O8 68.0(5) . . ?
O13 Ce1 O10 73.1(5) . . ?
O13 Ce1 O11 110.7(5) . . ?
O13 Ce1 O11 150.6(5) . 2_655 ?
O1 Ce2 O1Z 135.6(5) . . ?
O1 Ce2 O4 68.7(4) . . ?
O1 Ce2 O16 76.6(5) . . ?
O1 Ce2 O17 150.5(5) . 2_656 ?
O1 Ce2 O17 123.7(5) . . ?
O1 Ce2 O19 82.7(4) . . ?
O1 Ce2 O20 76.1(5) . . ?
O1Z Ce2 O4 68.4(5) . . ?
O1Z Ce2 O16 104.2(5) . . ?
O1Z Ce2 O17 72.0(5) . 2_656 ?
O1Z Ce2 O17 74.4(5) . . ?
O1Z Ce2 O19 140.8(5) . . ?
O1Z Ce2 O20 131.3(6) . . ?
O4 Ce2 O16 77.0(4) . . ?
O4 Ce2 O17 99.3(4) . . ?
O4 Ce2 O17 140.3(4) . 2_656 ?
O4 Ce2 O19 141.9(4) . . ?
O4 Ce2 O20 135.1(5) . . ?
O14 Ce2 O1 79.9(5) . . ?
O14 Ce2 O1Z 78.1(6) . . ?
O14 Ce2 O4 74.2(5) . . ?
O14 Ce2 O16 147.8(5) . . ?
O14 Ce2 O17 152.2(5) . . ?
O14 Ce2 O17 100.6(5) . 2_656 ?
O14 Ce2 O19 126.0(6) . . ?
O14 Ce2 O20 72.9(6) . . ?
O17 Ce2 O16 47.5(4) . . ?
O17 Ce2 O16 110.7(5) 2_656 . ?
O17 Ce2 O17 66.8(5) 2_656 . ?
O17 Ce2 O19 73.2(4) 2_656 . ?
O17 Ce2 O20 75.9(5) 2_656 . ?
O19 Ce2 O16 72.2(4) . . ?
O19 Ce2 O17 75.7(4) . . ?
O19 Ce2 O20 53.4(5) . . ?
O20 Ce2 O16 121.1(4) . . ?
O20 Ce2 O17 123.6(4) . . ?
O2 Na2 Ce1 78.3(4) . 2_655 ?
O2 Na2 O2Z 172.9(7) . . ?
O2 Na2 O5 76.1(6) . . ?
O2 Na2 O8 82.1(6) . 2_655 ?
O2 Na2 O9 86.3(7) . 1_455 ?
O2 Na2 O11 78.7(5) . 2_655 ?
O2Z Na2 Ce1 95.3(5) . 2_655 ?
O2Z Na2 O5 102.4(7) . . ?
O2Z Na2 O8 94.4(7) . 2_655 ?
O2Z Na2 O9 100.5(8) . 1_455 ?
O2Z Na2 O11 94.4(6) . 2_655 ?
O5 Na2 Ce1 101.3(4) . 2_655 ?
O5 Na2 O8 133.8(6) . 2_655 ?
O5 Na2 O9 86.8(6) . 1_455 ?
O5 Na2 O11 65.6(5) . 2_655 ?
O8 Na2 Ce1 33.8(4) 2_655 2_655 ?
O8 Na2 O11 70.5(5) 2_655 2_655 ?
O9 Na2 Ce1 160.2(6) 1_455 2_655 ?
O9 Na2 O8 132.1(7) 1_455 2_655 ?
O9 Na2 O11 151.0(6) 1_455 2_655 ?
O11 Na2 Ce1 36.7(3) 2_655 2_655 ?
Ce2 O1 Ce1 110.4(5) . . ?
C1 O1 Ce1 95.8(10) . . ?
C1 O1 Ce2 138.5(14) . . ?
Ce2 O1Z H1Z1 120.0 . . ?
Ce2 O1Z H1Z2 120.0 . . ?
H1Z1 O1Z H1Z2 120.0 . . ?
Na2 O2 Ce1 100.0(8) . . ?
C1 O2 Ce1 98.9(10) . . ?
C1 O2 Na2 135.9(13) . . ?
Na2 O2Z H2Z1 120.0 . . ?
Na2 O2Z H2Z2 120.0 . . ?
H2Z1 O2Z H2Z2 120.0 . . ?
C7 O3 H3 109.5 . . ?
Ce2 O4 Ce1 108.8(5) . . ?
C10 O4 Ce1 92.8(10) . . ?
C10 O4 Ce2 123.6(13) . . ?
Na2 O5 Ce1 95.4(5) . . ?
C10 O5 Ce1 95.3(11) . . ?
C10 O5 Na2 152.7(13) . . ?
C19 O7 Ce1 94.6(11) . . ?
Na2 O8 Ce1 115.6(6) 2_655 . ?
C19 O8 Ce1 91.7(11) . . ?
C19 O8 Na2 141.5(12) . 2_655 ?
C25 O9 Na2 134.1(12) . 1_655 ?
C28 O10 Ce1 92.7(11) . . ?
Ce1 O11 Ce1 116.2(5) 2_655 . ?
Ce1 O11 Na2 86.5(4) 2_655 2_655 ?
Ce1 O11 Na2 104.1(5) . 2_655 ?
C28 O11 Ce1 93.8(11) . . ?
C28 O11 Ce1 143.4(12) . 2_655 ?
C28 O11 Na2 106.9(13) . 2_655 ?
C37 O13 Ce1 130.3(16) . . ?
C37 O14 Ce2 148.3(15) . . ?
C43 O15 H15H 109.5 . . ?
C46 O16 Ce2 98.9(12) . . ?
Ce2 O17 Ce2 113.2(5) 2_656 . ?
C46 O17 Ce2 96.2(12) . . ?
C46 O17 Ce2 144.7(13) . 2_656 ?
C55 O19 Ce2 90.6(14) . . ?
C55 O20 Ce2 88.2(11) . . ?
O1 C1 O2 111.8(15) . . ?
O1 C1 C2 121.0(17) . . ?
O2 C1 C2 127.1(15) . . ?
C1 C2 H2A 107.7 . . ?
C1 C2 H2B 107.7 . . ?
C1 C2 C3 118.5(16) . . ?
H2A C2 H2B 107.1 . . ?
C3 C2 H2A 107.7 . . ?
C3 C2 H2B 107.7 . . ?
C2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
C2 C3 C4 112(2) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C5 C4 C3 121(2) . . ?
C5 C4 C9 118(2) . . ?
C9 C4 C3 121(2) . . ?
C4 C5 H5 117.2 . . ?
C4 C5 C6 126(2) . . ?
C6 C5 H5 117.2 . . ?
C5 C6 H6 123.2 . . ?
C7 C6 C5 114(2) . . ?
C7 C6 H6 123.2 . . ?
O3 C7 C6 117(2) . . ?
O3 C7 C8 123(2) . . ?
C8 C7 C6 120(2) . . ?
C7 C8 H8 119.2 . . ?
C7 C8 C9 122(2) . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C8 120.0(19) . . ?
C4 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
O4 C10 O5 120.2(16) . . ?
O4 C10 C11 119.2(16) . . ?
O5 C10 C11 120.5(15) . . ?
C10 C11 H11A 108.3 . . ?
C10 C11 H11B 108.3 . . ?
C10 C11 C12 115.8(16) . . ?
H11A C11 H11B 107.4 . . ?
C12 C11 H11A 108.3 . . ?
C12 C11 H11B 108.3 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C13 C12 C11 109.2(17) . . ?
C13 C12 H12A 109.8 . . ?
C13 C12 H12B 109.8 . . ?
C14 C13 C12 120(2) . . ?
C18 C13 C12 120(2) . . ?
C18 C13 C14 119(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 120(2) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120(3) . . ?
C16 C15 H15 120.0 . . ?
O6 C16 C17 119(2) . . ?
C15 C16 O6 119(2) . . ?
C15 C16 C17 121(2) . . ?
C16 C17 H17 120.1 . . ?
C16 C17 C18 120(2) . . ?
C18 C17 H17 120.1 . . ?
C13 C18 C17 118(2) . . ?
C13 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
O7 C19 O8 122.1(15) . . ?
O7 C19 C20 115.9(16) . . ?
O8 C19 C20 121.7(17) . . ?
C19 C20 H20A 107.3 . . ?
C19 C20 H20B 107.3 . . ?
H20A C20 H20B 106.9 . . ?
C21 C20 C19 120.1(19) . . ?
C21 C20 H20A 107.3 . . ?
C21 C20 H20B 107.3 . . ?
C20 C21 H21A 108.2 . . ?
C20 C21 H21B 108.2 . . ?
C20 C21 C22 116(2) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
C23 C22 C21 121(2) . . ?
C27 C22 C21 124(3) . . ?
C27 C22 C23 115(2) . . ?
C22 C23 H23 115.6 . . ?
C24 C23 C22 129(2) . . ?
C24 C23 H23 115.6 . . ?
C23 C24 H24 122.6 . . ?
C23 C24 C25 115(2) . . ?
C25 C24 H24 122.6 . . ?
O9 C25 C24 122.5(19) . . ?
O9 C25 C26 120.6(19) . . ?
C26 C25 C24 117.0(18) . . ?
C25 C26 H26 121.8 . . ?
C27 C26 C25 116.4(19) . . ?
C27 C26 H26 121.8 . . ?
C22 C27 C26 127(2) . . ?
C22 C27 H27 116.3 . . ?
C26 C27 H27 116.3 . . ?
O10 C28 C29 119(2) . . ?
O11 C28 O10 120.6(18) . . ?
O11 C28 C29 119.2(19) . . ?
C28 C29 H29A 108.9 . . ?
C28 C29 H29B 108.9 . . ?
C28 C29 C30 113.3(19) . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C29 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
C29 C30 C31 113(2) . . ?
H30A C30 H30B 107.8 . . ?
C31 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
O13 C37 O14 125(2) . . ?
O13 C37 C38 114(2) . . ?
O14 C37 C38 121(2) . . ?
C37 C38 H38A 108.3 . . ?
C37 C38 H38B 108.3 . . ?
H38A C38 H38B 107.4 . . ?
C39 C38 C37 116(4) . . ?
C39 C38 H38A 108.3 . . ?
C39 C38 H38B 108.3 . . ?
C38 C39 H39A 110.1 . . ?
C38 C39 H39B 110.1 . . ?
H39A C39 H39B 108.4 . . ?
C40 C39 C38 108(4) . . ?
C40 C39 H39A 110.1 . . ?
C40 C39 H39B 110.1 . . ?
C39 C40 C41 112(3) . . ?
C45 C40 C39 128(3) . . ?
C45 C40 C41 120(3) . . ?
C40 C41 H41 121.5 . . ?
C42 C41 C40 117(3) . . ?
C42 C41 H41 121.5 . . ?
C41 C42 H42 118.5 . . ?
C43 C42 C41 123(3) . . ?
C43 C42 H42 118.5 . . ?
O15 C43 C42 120(2) . . ?
O15 C43 C44 121(2) . . ?
C44 C43 C42 119(3) . . ?
C43 C44 H44 120.9 . . ?
C43 C44 C45 118(3) . . ?
C45 C44 H44 120.9 . . ?
C40 C45 H45 118.7 . . ?
C44 C45 C40 123(3) . . ?
C44 C45 H45 118.7 . . ?
O16 C46 O17 116.8(18) . . ?
O16 C46 C47 117(2) . . ?
O17 C46 C47 125(2) . . ?
C46 C47 H47A 107.8 . . ?
C46 C47 H47B 107.8 . . ?
H47A C47 H47B 107.1 . . ?
C48 C47 C46 118(2) . . ?
C48 C47 H47A 107.8 . . ?
C48 C47 H47B 107.8 . . ?
C47 C48 H48A 108.5 . . ?
C47 C48 H48B 108.5 . . ?
C47 C48 C49 115(3) . . ?
H48A C48 H48B 107.5 . . ?
C49 C48 H48A 108.5 . . ?
C49 C48 H48B 108.5 . . ?
C48 C49 C50 128(3) . . ?
C54 C49 C48 117(2) . . ?
C54 C49 C50 115(3) . . ?
C49 C50 H50 119.4 . . ?
C51 C50 C49 121(3) . . ?
C51 C50 H50 119.4 . . ?
C50 C51 H51 119.0 . . ?
C50 C51 C52 122(3) . . ?
C52 C51 H51 119.0 . . ?
O18 C52 C51 129(3) . . ?
O18 C52 C53 113(3) . . ?
C53 C52 C51 118(3) . . ?
C52 C53 H53 121.6 . . ?
C52 C53 C54 117(3) . . ?
C54 C53 H53 121.6 . . ?
C49 C54 C53 126(3) . . ?
C49 C54 H54 117.1 . . ?
C53 C54 H54 117.1 . . ?
O19 C55 O20 127.6(19) . . ?
O19 C55 C56 117(2) . . ?
O20 C55 C56 115(2) . . ?
C55 C56 H56A 108.9 . . ?
C55 C56 H56B 108.9 . . ?
H56A C56 H56B 107.7 . . ?
C57 C56 C55 113(2) . . ?
C57 C56 H56A 108.9 . . ?
C57 C56 H56B 108.9 . . ?
C56 C57 H57A 109.8 . . ?
C56 C57 H57B 109.8 . . ?
C56 C57 C58 109(3) . . ?
H57A C57 H57B 108.3 . . ?
C58 C57 H57A 109.8 . . ?
C58 C57 H57B 109.8 . . ?
C59 C58 C57 113(2) . . ?
C63 C58 C57 123(2) . . ?
C63 C58 C59 123(2) . . ?
C58 C59 H59 120.7 . . ?
C60 C59 C58 119(2) . . ?
C60 C59 H59 120.7 . . ?
C59 C60 H60 119.1 . . ?
C61 C60 C59 122(3) . . ?
C61 C60 H60 119.1 . . ?
C60 C61 O21 121(2) . . ?
C60 C61 C62 115(2) . . ?
C62 C61 O21 124(2) . . ?
C61 C62 H62 116.6 . . ?
C63 C62 C61 127(3) . . ?
C63 C62 H62 116.6 . . ?
C58 C63 C62 113(3) . . ?
C58 C63 H63 123.3 . . ?
C62 C63 H63 123.3 . . ?
C32 C31 C30 123(3) . . ?
C36 C31 C30 115(2) . . ?
C36 C31 C32 118.6(16) . . ?
C33 C34 O12 124(3) . . ?
C35 C34 O12 112(3) . . ?
C35 C34 C33 120.7(14) . . ?
C33 C32 C31 118.8(15) . . ?
C34 C33 C32 119.1(14) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.8(14) . . ?
C36 C35 H35 120.1 . . ?
C31 C36 H36 120.5 . . ?
C35 C36 C31 119.0(15) . . ?
C35 C36 H36 120.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1Z H1Z2 O19 0.95 1.91 2.66(2) 133.8 2_656
O3 H3 O4Z 0.84 1.97 2.79(3) 165.0 .
O15 H15H O3Z 0.84 1.91 2.67(3) 149.8 2_756

_olex2_submission_special_instructions 'No special instructions were received'

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 18.82316
2 -17.82316
#=========================================
#ALERT LEVEL B
_vrf_DIFMX01                     
;
PROBLEM:The maximum difference density is > 0.1*ZMAX*1.00
_refine_diff_density_max given = 6.454,Test value = 5.800
RESPONSE: The highest peak 6.45 is at 0.5628 0.0202 0.1419
[0.04 A from CE1] and is not assignable to other atoms. 
There is limitation to the quality of data and the structure
might be twinned.
;
_vrf_PLAT094                     
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .. 4.10 Report
RESPONSE: as above
;
_vrf_PLAT097                     
;
PROBLEM:Large Reported Max. (Positive) Residual Density 6.45 eA-3
RESPONSE: as above
;
_vrf_PLAT342                     
;
PROBLEM:Low Bond Precision on C-C Bonds .. 0.0430 Ang.
RESPONSE: as above
;
_vrf_PLAT306                     
;
PROBLEMS:Isolated Oxygen Atom (H-atoms Missing ?) ..O3Z Check;
Isolated Oxygen Atom (H-atoms Missing ?) ....... O4Z Check;
Isolated Oxygen Atom (H-atoms Missing ?) ....... O5Z Check.
RESPONSE: The relevant protons are not able to be located 
and modelled properly.
;
_vrf_PLAT430                     
;
PROBLEMS:Short Inter D...A Contact O3Z .. O7 .. 2.68 Ang.
Short Inter D...A Contact O4Z .. O13 .. 2.77 Ang.
Short Inter D...A Contact O4Z .. O21 .. 2.77 Ang.
Short Inter D...A Contact O5Z .. O21 .. 2.57 Ang.
Short Inter D...A Contact O5Z .. O10 .. 2.68 Ang.
Short Inter D...A Contact O5Z .. O6 .. 2.80 Ang.
Short Inter D...A Contact O5Z .. O20 .. 2.84 Ang.
RESPONSE: as above
;
#==========================================
####################################################################### 
# 
# 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_compound4.cif
_database_code_depnum_ccdc_archive 'CCDC 1055966'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_audit_creation_date             2015-05-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H69 Na Nd2 O23, H2 O, 3(C H4 O)'
_chemical_formula_sum            'C67 H83 Na Nd2 O27'
_chemical_formula_weight         1631.80
_chemical_melting_point          ?
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.328(3)
_cell_length_b                   15.480(3)
_cell_length_c                   16.300(3)
_cell_angle_alpha                78.16(3)
_cell_angle_beta                 70.63(3)
_cell_angle_gamma                86.33(3)
_cell_volume                     3571.0(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    43827
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.046
_cell_measurement_theta_min      1.344
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.702
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_process_details   SORTAV
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.9277
_exptl_transmission_factor_min   0.7018
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_unetI/netI     0.1473
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31950
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.344
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7672
_reflns_number_total             12470
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         2.174
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         12470
_refine_ls_number_restraints     214
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0687
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1896
_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.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, {H14H,H2ZD,H4Z} of C4Z, All C(H) groups, All C(H,H) groups,
   All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  {H4Z1,H4Z2,H4Z3} of C4Z, {H6ZA,H6ZB,H6ZC} of C6Z, {H2ZA,H2ZB,H2ZC} of C2Z,
  {H5ZA,H5ZB,H5ZC} of C5Z
2. Restrained distances
 C22-C23 = C23-C24 = C24-C25 = C25-C26 = C26-C27 = C27-C22
 1.4 with sigma of 0.02
 C16-C17 = C13-C18
 1.4 with sigma of 0.02
 O2Z-H2ZD = O12-H14H
 0.9 with sigma of 0.02
 O9-H9H = O4Z-H4Z = O18-H18H = O3Z-H3ZA = O3Z-H3ZB
 0.92 with sigma of 0.02
 C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C18 = C18-C13
 1.4 with sigma of 0.02
 Na1-H2ZD
 2.39 with sigma of 0.02
3. Rigid bond restraints
 C13, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C47, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim O9:
within 1.7A with sigma of 0.05 and sigma for terminal atoms of 0.01
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A
with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(O4Z) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, : with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(C28)
Uiso(C4Z) = Uiso(C6Z)
Uanis(O4Z) = Uanis(O5Z)
Uanis(O7) = Uanis(O8)
Uanis(C37) = Uanis(C38)
Uanis(O5) = Uanis(O10)
Uanis(C4) = Uanis(C5)
Uanis(C21) = Uanis(C20)
Uanis(O9) = Uanis(O21)
Uiso(H3ZA) = Uiso(H1Z1)
Uiso(H4Z) = Uiso(H5ZD)
Uanis(C14) = Uanis(C12)
Uanis(C13) = Uanis(C12)
Uanis(C16) = Uanis(C15)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B), C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B),
  C47(H47A,H47B), C48(H48A,H48B), C56(H56A,H56B), C57(H57A,H57B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27), C32(H32), C33(H33), C35(H35), C36(H36),
  C41(H41), C42(H42), C44(H44), C45(H45), C50(H50), C51(H51), C53(H53),
 C54(H54), C59(H59), C60(H60), C62(H62), C63(H63)
5.c X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2)
5.d Idealised Me refined as rotating group:
 C2Z(H2ZA,H2ZB,H2ZC), C5Z(H5ZA,H5ZB,H5ZC), C6Z(H6ZA,H6ZB,H6ZC), C4Z(H4Z1,H4Z2,
 H4Z3)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3H), O5Z(H5ZD), O6(H6H), O6Z(H6ZD), O9(H9H), O15(H15H), O21(H21)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.56064(4) 0.50599(3) 0.85781(3) 0.01339(17) Uani 1 1 d . . . . .
Nd2 Nd 0.53747(4) 0.53445(3) 0.60604(3) 0.01401(17) Uani 1 1 d . . . . .
Na1 Na 0.3339(3) 0.4091(2) 0.9714(3) 0.0210(9) Uani 1 1 d D . . . .
O1 O 0.5681(4) 0.4245(3) 0.7300(4) 0.0138(15) Uani 1 1 d . . . . .
O1Z O 0.6359(5) 0.4174(4) 0.5446(4) 0.0252(17) Uani 1 1 d . . . . .
H1Z1 H 0.7003 0.4176 0.5362 0.030 Uiso 1 1 calc R . . . .
H1Z2 H 0.6099 0.3716 0.5291 0.030 Uiso 1 1 calc R . . . .
O2 O 0.4677(4) 0.3725(4) 0.8606(4) 0.0157(15) Uani 1 1 d . . . . .
O2Z O 0.2798(6) 0.2752(5) 1.0646(5) 0.037(2) Uani 1 1 d D . . . .
O3 O 0.4502(6) -0.1033(4) 0.6814(5) 0.036(2) Uani 1 1 d . . . . .
H3H H 0.4830 -0.1414 0.7021 0.043 Uiso 1 1 calc GR . . . .
O3Z O 0.5911(5) 0.7716(4) 0.6861(5) 0.0223(17) Uani 1 1 d D . . . .
O4 O 0.4822(4) 0.5870(4) 0.7464(4) 0.0144(15) Uani 1 1 d . . . . .
O5 O 0.3885(4) 0.5534(4) 0.8845(4) 0.0202(11) Uani 1 1 d . . . . .
O5Z O 0.7185(7) 0.2543(6) 0.7801(7) 0.0619(19) Uani 1 1 d . . . . .
H5ZD H 0.7244 0.3013 0.7960 0.074 Uiso 1 1 calc GR . . . .
O6 O 0.0332(6) 0.9214(4) 0.6837(6) 0.052(3) Uani 1 1 d . . . . .
H6H H 0.0036 0.8944 0.6616 0.062 Uiso 1 1 calc GR . . . .
O6Z O 0.9388(5) 0.8427(5) 0.6150(6) 0.043(2) Uani 1 1 d . . . . .
H6ZD H 0.8815 0.8383 0.6260 0.052 Uiso 1 1 calc GR . . . .
O7 O 0.5072(5) 0.5878(4) 0.9907(4) 0.0182(11) Uani 1 1 d . . . . .
O8 O 0.5477(5) 0.6721(4) 0.8583(4) 0.0182(11) Uani 1 1 d . . . . .
O9 O 0.2324(6) 1.1001(5) 1.0589(6) 0.0563(18) Uani 1 1 d D U . . .
H9H H 0.2107 1.1287 1.0203 0.068 Uiso 1 1 calc DGR . . . .
O10 O 0.6877(4) 0.3974(4) 0.8556(4) 0.0202(11) Uani 1 1 d . . . . .
O11 O 0.6968(4) 0.5087(4) 0.9165(4) 0.0171(15) Uani 1 1 d . . . . .
O12 O 1.2610(5) 0.4017(4) 0.8655(5) 0.0256(17) Uani 1 1 d D . . . .
O13 O 0.6883(5) 0.5757(4) 0.7394(4) 0.0244(17) Uani 1 1 d . . . . .
O14 O 0.6804(4) 0.5779(4) 0.6052(4) 0.0221(16) Uani 1 1 d . . . . .
O15 O 1.2475(5) 0.6994(4) 0.3922(4) 0.0259(17) Uani 1 1 d . . . . .
H15H H 1.2594 0.6989 0.3382 0.031 Uiso 1 1 calc GR . . . .
O16 O 0.3796(5) 0.4529(4) 0.6973(4) 0.0232(17) Uani 1 1 d . . . . .
O17 O 0.4317(5) 0.4408(4) 0.5584(4) 0.0200(16) Uani 1 1 d . . . . .
O18 O -0.0075(6) 0.0607(5) 0.7592(7) 0.061(3) Uani 1 1 d D . . . .
O19 O 0.5522(5) 0.7009(4) 0.5570(4) 0.0189(16) Uani 1 1 d . . . . .
O20 O 0.4192(5) 0.6410(4) 0.5720(4) 0.0198(16) Uani 1 1 d . . . . .
O21 O 0.2446(6) 1.1460(5) 0.3742(7) 0.0563(18) Uani 1 1 d . . . . .
H21 H 0.2918 1.1785 0.3525 0.068 Uiso 1 1 calc GR . . . .
C1 C 0.5136(7) 0.3642(6) 0.7835(7) 0.0146(15) Uani 1 1 d . U . . .
C2 C 0.5068(7) 0.2800(5) 0.7522(6) 0.017(2) Uani 1 1 d . . . . .
H2A H 0.4922 0.2962 0.6963 0.021 Uiso 1 1 calc R . . . .
H2B H 0.5684 0.2518 0.7383 0.021 Uiso 1 1 calc R . . . .
C2Z C 0.2412(9) 0.2639(8) 1.1572(8) 0.049(4) Uani 1 1 d . . . . .
H2ZA H 0.2577 0.3144 1.1769 0.074 Uiso 1 1 calc GR . . . .
H2ZB H 0.2653 0.2096 1.1849 0.074 Uiso 1 1 calc GR . . . .
H2ZC H 0.1738 0.2597 1.1745 0.074 Uiso 1 1 calc GR . . . .
C3 C 0.4369(8) 0.2125(6) 0.8151(7) 0.028(3) Uani 1 1 d . . . . .
H3A H 0.3741 0.2378 0.8252 0.034 Uiso 1 1 calc R . . . .
H3B H 0.4481 0.1983 0.8728 0.034 Uiso 1 1 calc R . . . .
C4 C 0.4413(7) 0.1270(6) 0.7795(7) 0.0240(18) Uani 1 1 d . . . . .
O4Z O 0.0598(7) 0.0640(6) 1.0709(6) 0.0619(19) Uani 1 1 d D U . . .
C5 C 0.3705(7) 0.1041(6) 0.7543(7) 0.0240(18) Uani 1 1 d . . . . .
H5 H 0.3170 0.1401 0.7613 0.029 Uiso 1 1 calc R . . . .
C5Z C 0.7739(12) 0.1849(10) 0.8144(11) 0.088(5) Uiso 1 1 d . U . . .
H5ZA H 0.7563 0.1787 0.8789 0.132 Uiso 1 1 calc GR . . . .
H5ZB H 0.8396 0.2005 0.7871 0.132 Uiso 1 1 calc GR . . . .
H5ZC H 0.7630 0.1289 0.8001 0.132 Uiso 1 1 calc GR . . . .
C6 C 0.3756(8) 0.0288(7) 0.7184(8) 0.035(3) Uani 1 1 d . . . . .
H6 H 0.3273 0.0151 0.6987 0.042 Uiso 1 1 calc R . . . .
C6Z C 0.9847(12) 0.8505(10) 0.5221(11) 0.090(4) Uiso 1 1 d . U . . .
H6ZA H 0.9804 0.9116 0.4921 0.135 Uiso 1 1 calc GR . . . .
H6ZB H 0.9553 0.8110 0.4991 0.135 Uiso 1 1 calc GR . . . .
H6ZC H 1.0498 0.8345 0.5113 0.135 Uiso 1 1 calc GR . . . .
C7 C 0.4512(7) -0.0252(6) 0.7120(7) 0.024(3) Uani 1 1 d . . . . .
C8 C 0.5231(8) -0.0031(6) 0.7353(7) 0.027(3) Uani 1 1 d . . . . .
H8 H 0.5765 -0.0394 0.7282 0.032 Uiso 1 1 calc R . . . .
C9 C 0.5178(7) 0.0738(6) 0.7699(7) 0.023(2) Uani 1 1 d . . . . .
H9 H 0.5675 0.0891 0.7869 0.027 Uiso 1 1 calc R . . . .
C10 C 0.4056(7) 0.5959(6) 0.8053(7) 0.018(2) Uani 1 1 d . . . . .
C11 C 0.3392(6) 0.6623(6) 0.7767(6) 0.018(2) Uani 1 1 d . . . . .
H11A H 0.3227 0.6421 0.7299 0.021 Uiso 1 1 calc R . . . .
H11B H 0.3725 0.7191 0.7494 0.021 Uiso 1 1 calc R . . . .
C12 C 0.2490(7) 0.6798(7) 0.8483(8) 0.0360(17) Uani 1 1 d . U . . .
H12A H 0.2148 0.6236 0.8770 0.043 Uiso 1 1 calc R . . . .
H12B H 0.2640 0.7030 0.8944 0.043 Uiso 1 1 calc R . . . .
C13 C 0.1894(7) 0.7440(6) 0.8107(8) 0.0360(17) Uani 1 1 d D U . . .
C14 C 0.2109(8) 0.8334(6) 0.7803(7) 0.0360(17) Uani 1 1 d D U . . .
H14 H 0.2624 0.8552 0.7902 0.043 Uiso 1 1 calc R . . . .
C15 C 0.1611(8) 0.8931(7) 0.7359(9) 0.049(3) Uani 1 1 d D U . . .
H15 H 0.1796 0.9532 0.7145 0.058 Uiso 1 1 calc R . . . .
C16 C 0.0841(9) 0.8626(6) 0.7238(9) 0.049(3) Uani 1 1 d D U . . .
C17 C 0.0672(9) 0.7754(6) 0.7461(10) 0.062(5) Uani 1 1 d D U . . .
H17 H 0.0180 0.7528 0.7332 0.074 Uiso 1 1 calc R . . . .
C18 C 0.1188(9) 0.7179(7) 0.7870(10) 0.064(5) Uani 1 1 d D U . . .
H18 H 0.1049 0.6567 0.7997 0.076 Uiso 1 1 calc R . . . .
C19 C 0.5078(7) 0.6621(6) 0.9401(7) 0.018(2) Uani 1 1 d . . . . .
C20 C 0.4579(10) 0.7387(7) 0.9798(8) 0.059(3) Uani 1 1 d . . . . .
H20A H 0.3934 0.7200 1.0144 0.071 Uiso 1 1 calc R . . . .
H20B H 0.4872 0.7504 1.0222 0.071 Uiso 1 1 calc R . . . .
C21 C 0.4550(10) 0.8220(7) 0.9192(8) 0.059(3) Uani 1 1 d . U . . .
H21A H 0.4308 0.8098 0.8734 0.071 Uiso 1 1 calc R . . . .
H21B H 0.5191 0.8442 0.8887 0.071 Uiso 1 1 calc R . . . .
C22 C 0.3980(11) 0.8939(10) 0.9602(10) 0.077(4) Uani 1 1 d D U . . .
C23 C 0.4161(12) 0.9365(9) 1.0192(10) 0.087(5) Uani 1 1 d D U . . .
H23 H 0.4689 0.9196 1.0367 0.105 Uiso 1 1 calc R . . . .
C24 C 0.3593(11) 1.0038(10) 1.0545(11) 0.080(5) Uani 1 1 d D U . . .
H24 H 0.3716 1.0302 1.0973 0.096 Uiso 1 1 calc R . . . .
C25 C 0.2866(10) 1.0303(8) 1.0259(10) 0.060(3) Uani 1 1 d D U . . .
C26 C 0.2658(11) 0.9846(9) 0.9713(10) 0.080(5) Uani 1 1 d D U . . .
H26 H 0.2115 0.9997 0.9557 0.096 Uiso 1 1 calc R . . . .
C27 C 0.3215(11) 0.9167(9) 0.9375(10) 0.079(5) Uani 1 1 d D U . . .
H27 H 0.3056 0.8868 0.8990 0.095 Uiso 1 1 calc R . . . .
C28 C 0.7325(6) 0.4426(6) 0.8855(6) 0.0146(15) Uani 1 1 d . . . . .
C29 C 0.8313(7) 0.4163(6) 0.8786(7) 0.022(2) Uani 1 1 d . . . . .
H29A H 0.8673 0.4166 0.8156 0.027 Uiso 1 1 calc R . . . .
H29B H 0.8314 0.3551 0.9119 0.027 Uiso 1 1 calc R . . . .
C30 C 0.8789(7) 0.4761(7) 0.9136(8) 0.031(3) Uani 1 1 d . U . . .
H30A H 0.8466 0.4716 0.9780 0.037 Uiso 1 1 calc R . . . .
H30B H 0.8742 0.5380 0.8840 0.037 Uiso 1 1 calc R . . . .
C31 C 0.9812(7) 0.4532(6) 0.8984(7) 0.025(3) Uani 1 1 d . . . . .
C32 C 1.0089(7) 0.3913(7) 0.9597(7) 0.030(3) Uani 1 1 d . U . . .
H32 H 0.9629 0.3605 1.0104 0.036 Uiso 1 1 calc R . . . .
C33 C 1.1007(7) 0.3729(7) 0.9497(7) 0.029(3) Uani 1 1 d . . . . .
H33 H 1.1177 0.3304 0.9927 0.034 Uiso 1 1 calc R . . . .
C34 C 1.1680(7) 0.4184(6) 0.8749(6) 0.015(2) Uani 1 1 d . . . . .
C35 C 1.1413(7) 0.4778(6) 0.8118(7) 0.023(2) Uani 1 1 d . . . . .
H35 H 1.1867 0.5076 0.7600 0.028 Uiso 1 1 calc R . . . .
C36 C 1.0497(8) 0.4937(7) 0.8240(7) 0.029(3) Uani 1 1 d . . . . .
H36 H 1.0326 0.5341 0.7796 0.035 Uiso 1 1 calc R . . . .
C37 C 0.7225(7) 0.5907(7) 0.6562(7) 0.0255(18) Uani 1 1 d . . . . .
C38 C 0.8189(7) 0.6334(6) 0.6139(7) 0.0255(18) Uani 1 1 d . U . . .
H38A H 0.8202 0.6809 0.5625 0.031 Uiso 1 1 calc R . . . .
H38B H 0.8358 0.6590 0.6575 0.031 Uiso 1 1 calc R . . . .
C39 C 0.8833(8) 0.5628(8) 0.5852(9) 0.051(4) Uani 1 1 d . U . . .
H39A H 0.8616 0.5334 0.5470 0.061 Uiso 1 1 calc R . . . .
H39B H 0.8850 0.5181 0.6377 0.061 Uiso 1 1 calc R . . . .
C40 C 0.9830(9) 0.6014(8) 0.5326(9) 0.050(3) Uani 1 1 d . U . . .
C41 C 1.0490(9) 0.6034(9) 0.5732(9) 0.058(4) Uani 1 1 d . U . . .
H41 H 1.0334 0.5808 0.6351 0.069 Uiso 1 1 calc R . . . .
C42 C 1.1369(8) 0.6372(8) 0.5267(8) 0.047(3) Uani 1 1 d . U . . .
H42 H 1.1812 0.6373 0.5560 0.057 Uiso 1 1 calc R . . . .
C43 C 1.1588(7) 0.6703(7) 0.4380(7) 0.028(2) Uani 1 1 d . U . . .
C44 C 1.0953(8) 0.6696(7) 0.3945(8) 0.040(3) Uani 1 1 d . U . . .
H44 H 1.1117 0.6912 0.3324 0.048 Uiso 1 1 calc R . . . .
C45 C 1.0065(8) 0.6365(8) 0.4436(9) 0.047(3) Uani 1 1 d . U . . .
H45 H 0.9616 0.6383 0.4148 0.056 Uiso 1 1 calc R . . . .
C46 C 0.3761(8) 0.4181(7) 0.6352(7) 0.028(2) Uani 1 1 d . U . . .
C47 C 0.3100(8) 0.3377(7) 0.6599(8) 0.040(3) Uani 1 1 d . U . . .
H47A H 0.3452 0.2875 0.6357 0.048 Uiso 1 1 calc R . . . .
H47B H 0.2853 0.3194 0.7252 0.048 Uiso 1 1 calc R . . . .
C48 C 0.2335(8) 0.3587(7) 0.6251(8) 0.043(3) Uani 1 1 d . U . . .
H48A H 0.2567 0.3703 0.5594 0.052 Uiso 1 1 calc R . . . .
H48B H 0.2008 0.4119 0.6446 0.052 Uiso 1 1 calc R . . . .
C49 C 0.1669(10) 0.2783(8) 0.6610(9) 0.051(4) Uani 1 1 d . . . . .
C50 C 0.1825(9) 0.2072(8) 0.6180(8) 0.047(3) Uani 1 1 d . . . . .
H50 H 0.2337 0.2091 0.5653 0.056 Uiso 1 1 calc R . . . .
C51 C 0.1246(8) 0.1331(7) 0.6505(8) 0.035(3) Uani 1 1 d . . . . .
H51 H 0.1368 0.0849 0.6204 0.041 Uiso 1 1 calc R . . . .
C52 C 0.0501(8) 0.1308(6) 0.7261(8) 0.032(3) Uani 1 1 d . U . . .
C53 C 0.0379(8) 0.1987(7) 0.7712(8) 0.041(3) Uani 1 1 d . . . . .
H53 H -0.0119 0.1962 0.8251 0.049 Uiso 1 1 calc R . . . .
C54 C 0.0964(9) 0.2699(8) 0.7397(9) 0.046(3) Uani 1 1 d . . . . .
H54 H 0.0877 0.3148 0.7736 0.055 Uiso 1 1 calc R . . . .
C55 C 0.4746(7) 0.7083(6) 0.5467(7) 0.019(2) Uani 1 1 d . . . . .
C56 C 0.4431(7) 0.7956(6) 0.5072(7) 0.022(2) Uani 1 1 d . . . . .
H56A H 0.4612 0.8000 0.4423 0.026 Uiso 1 1 calc R . . . .
H56B H 0.4762 0.8429 0.5178 0.026 Uiso 1 1 calc R . . . .
C57 C 0.3391(7) 0.8126(6) 0.5430(8) 0.039(3) Uani 1 1 d . . . . .
H57A H 0.3052 0.7661 0.5323 0.047 Uiso 1 1 calc R . . . .
H57B H 0.3203 0.8092 0.6078 0.047 Uiso 1 1 calc R . . . .
C58 C 0.3133(7) 0.9013(6) 0.4999(8) 0.033(3) Uani 1 1 d . U . . .
C59 C 0.3473(7) 0.9788(6) 0.5083(7) 0.027(2) Uani 1 1 d . U . . .
H59 H 0.3871 0.9753 0.5429 0.033 Uiso 1 1 calc R . . . .
C60 C 0.3249(7) 1.0613(6) 0.4678(7) 0.021(2) Uani 1 1 d . U . . .
H60 H 0.3494 1.1137 0.4738 0.025 Uiso 1 1 calc R . . . .
C61 C 0.2666(7) 1.0652(6) 0.4188(7) 0.025(2) Uani 1 1 d . U . . .
C62 C 0.2307(7) 0.9899(6) 0.4098(8) 0.032(3) Uani 1 1 d . U . . .
H62 H 0.1906 0.9944 0.3755 0.039 Uiso 1 1 calc R . . . .
C63 C 0.2523(8) 0.9080(6) 0.4501(8) 0.037(3) Uani 1 1 d . U . . .
H63 H 0.2264 0.8562 0.4445 0.044 Uiso 1 1 calc R . . . .
H3ZA H 0.558(6) 0.746(6) 0.742(3) 0.044 Uiso 1 1 d DR . . . .
H3ZB H 0.567(9) 0.742(7) 0.656(8) 0.09(5) Uiso 1 1 d D . . . .
H18H H -0.030(11) 0.039(9) 0.721(9) 0.110 Uiso 1 1 d DR . . . .
C4Z C -0.0039(12) 0.1197(10) 1.0350(11) 0.090(4) Uiso 1 1 d . U . . .
H4Z1 H -0.0467 0.1478 1.0815 0.135 Uiso 1 1 calc GR . . . .
H4Z2 H -0.0390 0.0838 1.0138 0.135 Uiso 1 1 calc GR . . . .
H4Z3 H 0.0309 0.1653 0.9857 0.135 Uiso 1 1 calc GR . . . .
H14H H 1.263(10) 0.344(2) 0.865(10) 0.108 Uiso 1 1 d DR . . . .
H2ZD H 0.305(9) 0.2536(18) 1.015(3) 0.108 Uiso 1 1 d DR . . . .
H4Z H 0.083(10) 0.012(5) 1.100(9) 0.108 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 Na1 4.104(3) 2_667 ?
Nd1 O1 2.617(6) . ?
Nd1 O2 2.568(6) . ?
Nd1 O4 2.577(5) . ?
Nd1 O5 2.610(6) . ?
Nd1 O7 2.511(6) 2_667 ?
Nd1 O7 2.605(6) . ?
Nd1 O8 2.568(5) . ?
Nd1 O10 2.486(6) . ?
Nd1 O11 2.574(6) . ?
Nd1 O13 2.372(7) . ?
Nd2 O1 2.513(6) . ?
Nd2 O1Z 2.440(6) . ?
Nd2 O4 2.450(6) . ?
Nd2 O14 2.328(6) . ?
Nd2 O16 2.627(7) . ?
Nd2 O17 2.513(6) 2_666 ?
Nd2 O17 2.633(6) . ?
Nd2 O19 2.537(6) . ?
Nd2 O20 2.495(6) . ?
Na1 Nd1 4.104(3) 2_667 ?
Na1 O2 2.367(8) . ?
Na1 O2Z 2.321(8) . ?
Na1 O5 2.418(7) . ?
Na1 O7 2.709(7) 2_667 ?
Na1 O11 2.342(7) 2_667 ?
Na1 O12 2.369(7) 1_455 ?
Na1 H2ZD 2.39(2) . ?
O1 C1 1.270(11) . ?
O1Z H1Z1 0.9500 . ?
O1Z H1Z2 0.9500 . ?
O2 C1 1.250(11) . ?
O2Z C2Z 1.404(13) . ?
O2Z H2ZD 0.90(2) . ?
O3 H3H 0.8400 . ?
O3 C7 1.402(10) . ?
O3Z H3ZA 0.91(2) . ?
O3Z H3ZB 0.91(2) . ?
O4 C10 1.267(11) . ?
O5 C10 1.271(11) . ?
O5Z H5ZD 0.8400 . ?
O5Z C5Z 1.463(15) . ?
O6 H6H 0.8400 . ?
O6 C16 1.367(11) . ?
O6Z H6ZD 0.8400 . ?
O6Z C6Z 1.425(17) . ?
O7 Nd1 2.511(6) 2_667 ?
O7 Na1 2.709(7) 2_667 ?
O7 C19 1.269(10) . ?
O8 C19 1.250(11) . ?
O9 H9H 0.8400 . ?
O9 C25 1.405(14) . ?
O10 C28 1.273(10) . ?
O11 Na1 2.342(7) 2_667 ?
O11 C28 1.249(10) . ?
O12 Na1 2.369(7) 1_655 ?
O12 C34 1.396(11) . ?
O12 H14H 0.90(2) . ?
O13 C37 1.258(12) . ?
O14 C37 1.260(11) . ?
O15 H15H 0.8400 . ?
O15 C43 1.369(12) . ?
O16 C46 1.256(11) . ?
O17 Nd2 2.513(6) 2_666 ?
O17 C46 1.252(12) . ?
O18 C52 1.346(13) . ?
O18 H18H 0.92(2) . ?
O19 C55 1.250(11) . ?
O20 C55 1.296(11) . ?
O21 H21 0.8400 . ?
O21 C61 1.393(11) . ?
C1 C2 1.514(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.506(13) . ?
C2Z H2ZA 0.9800 . ?
C2Z H2ZB 0.9800 . ?
C2Z H2ZC 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.539(12) . ?
C4 C5 1.370(13) . ?
C4 C9 1.373(13) . ?
O4Z C4Z 1.451(15) . ?
O4Z H4Z 0.95(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(13) . ?
C5Z H5ZA 0.9800 . ?
C5Z H5ZB 0.9800 . ?
C5Z H5ZC 0.9800 . ?
C6 H6 0.9500 . ?
C6 C7 1.372(14) . ?
C6Z H6ZA 0.9800 . ?
C6Z H6ZB 0.9800 . ?
C6Z H6ZC 0.9800 . ?
C7 C8 1.363(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.406(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.514(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.536(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.484(13) . ?
C13 C14 1.393(12) . ?
C13 C18 1.372(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.401(11) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(12) . ?
C16 C17 1.343(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.370(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.510(14) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.463(15) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.496(17) . ?
C22 C23 1.376(14) . ?
C22 C27 1.348(14) . ?
C23 H23 0.9500 . ?
C23 C24 1.405(13) . ?
C24 H24 0.9500 . ?
C24 C25 1.353(13) . ?
C25 C26 1.368(13) . ?
C26 H26 0.9500 . ?
C26 C27 1.395(14) . ?
C27 H27 0.9500 . ?
C28 C29 1.517(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.516(12) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.533(13) . ?
C31 C32 1.390(14) . ?
C31 C36 1.377(15) . ?
C32 H32 0.9500 . ?
C32 C33 1.379(14) . ?
C33 H33 0.9500 . ?
C33 C34 1.398(14) . ?
C34 C35 1.384(12) . ?
C35 H35 0.9500 . ?
C35 C36 1.365(14) . ?
C36 H36 0.9500 . ?
C37 C38 1.535(14) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.467(14) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.570(16) . ?
C40 C41 1.386(16) . ?
C40 C45 1.372(17) . ?
C41 H41 0.9500 . ?
C41 C42 1.384(17) . ?
C42 H42 0.9500 . ?
C42 C43 1.365(15) . ?
C43 C44 1.383(14) . ?
C44 H44 0.9500 . ?
C44 C45 1.398(16) . ?
C45 H45 0.9500 . ?
C46 C47 1.558(15) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.456(14) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.549(16) . ?
C49 C50 1.389(15) . ?
C49 C54 1.364(17) . ?
C50 H50 0.9500 . ?
C50 C51 1.397(15) . ?
C51 H51 0.9500 . ?
C51 C52 1.371(15) . ?
C52 C53 1.371(14) . ?
C53 H53 0.9500 . ?
C53 C54 1.369(15) . ?
C54 H54 0.9500 . ?
C55 C56 1.496(12) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.530(14) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.501(13) . ?
C58 C59 1.387(13) . ?
C58 C63 1.413(14) . ?
C59 H59 0.9500 . ?
C59 C60 1.391(12) . ?
C60 H60 0.9500 . ?
C60 C61 1.374(13) . ?
C61 C62 1.374(13) . ?
C62 H62 0.9500 . ?
C62 C63 1.378(13) . ?
C63 H63 0.9500 . ?
C4Z H4Z1 0.9800 . ?
C4Z H4Z2 0.9800 . ?
C4Z H4Z3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nd1 Na1 154.41(14) . 2_667 ?
O2 Nd1 Na1 136.78(14) . 2_667 ?
O2 Nd1 O1 50.16(19) . . ?
O2 Nd1 O4 83.88(19) . . ?
O2 Nd1 O5 71.55(19) . . ?
O2 Nd1 O7 119.6(2) . . ?
O2 Nd1 O11 128.58(18) . . ?
O4 Nd1 Na1 132.77(14) . 2_667 ?
O4 Nd1 O1 64.84(17) . . ?
O4 Nd1 O5 50.4(2) . . ?
O4 Nd1 O7 105.64(18) . . ?
O5 Nd1 Na1 111.35(14) . 2_667 ?
O5 Nd1 O1 94.23(19) . . ?
O7 Nd1 Na1 40.36(15) . 2_667 ?
O7 Nd1 Na1 71.63(14) 2_667 2_667 ?
O7 Nd1 O1 165.0(2) . . ?
O7 Nd1 O1 112.97(18) 2_667 . ?
O7 Nd1 O2 66.01(19) 2_667 . ?
O7 Nd1 O4 130.6(2) 2_667 . ?
O7 Nd1 O5 71.06(19) . . ?
O7 Nd1 O5 82.3(2) 2_667 . ?
O7 Nd1 O7 63.4(2) 2_667 . ?
O7 Nd1 O8 113.1(2) 2_667 . ?
O7 Nd1 O11 80.7(2) 2_667 . ?
O8 Nd1 Na1 64.01(14) . 2_667 ?
O8 Nd1 O1 128.81(18) . . ?
O8 Nd1 O2 142.38(19) . . ?
O8 Nd1 O4 68.76(18) . . ?
O8 Nd1 O5 71.1(2) . . ?
O8 Nd1 O7 50.16(19) . . ?
O8 Nd1 O11 85.74(19) . . ?
O10 Nd1 Na1 80.76(15) . 2_667 ?
O10 Nd1 O1 75.49(18) . . ?
O10 Nd1 O2 84.26(19) . . ?
O10 Nd1 O4 136.4(2) . . ?
O10 Nd1 O5 154.5(2) . . ?
O10 Nd1 O7 116.64(19) . . ?
O10 Nd1 O7 80.6(2) . 2_667 ?
O10 Nd1 O8 133.4(2) . . ?
O10 Nd1 O11 51.27(19) . . ?
O11 Nd1 Na1 31.65(15) . 2_667 ?
O11 Nd1 O1 122.78(19) . . ?
O11 Nd1 O4 145.1(2) . . ?
O11 Nd1 O5 142.88(19) . . ?
O11 Nd1 O7 71.8(2) . . ?
O13 Nd1 Na1 87.95(16) . 2_667 ?
O13 Nd1 O1 77.5(2) . . ?
O13 Nd1 O2 127.3(2) . . ?
O13 Nd1 O4 78.0(2) . . ?
O13 Nd1 O5 124.7(2) . . ?
O13 Nd1 O7 112.9(2) . . ?
O13 Nd1 O7 151.4(2) . 2_667 ?
O13 Nd1 O8 72.9(2) . . ?
O13 Nd1 O10 76.5(2) . . ?
O13 Nd1 O11 71.8(2) . . ?
O1 Nd2 O16 74.1(2) . . ?
O1 Nd2 O17 101.05(18) . . ?
O1 Nd2 O19 134.49(18) . . ?
O1Z Nd2 O1 70.9(2) . . ?
O1Z Nd2 O4 138.24(19) . . ?
O1Z Nd2 O16 103.0(2) . . ?
O1Z Nd2 O17 69.9(2) . 2_666 ?
O1Z Nd2 O17 74.3(2) . . ?
O1Z Nd2 O19 130.4(2) . . ?
O1Z Nd2 O20 139.16(19) . . ?
O4 Nd2 O1 68.26(19) . . ?
O4 Nd2 O16 74.0(2) . . ?
O4 Nd2 O17 121.9(2) . . ?
O4 Nd2 O17 150.74(19) . 2_666 ?
O4 Nd2 O19 76.8(2) . . ?
O4 Nd2 O20 81.64(19) . . ?
O14 Nd2 O1 76.3(2) . . ?
O14 Nd2 O1Z 79.4(2) . . ?
O14 Nd2 O4 82.8(2) . . ?
O14 Nd2 O16 147.5(2) . . ?
O14 Nd2 O17 152.8(2) . . ?
O14 Nd2 O17 99.0(2) . 2_666 ?
O14 Nd2 O19 71.1(2) . . ?
O14 Nd2 O20 123.2(2) . . ?
O16 Nd2 O17 49.0(2) . . ?
O17 Nd2 O1 140.74(19) 2_666 . ?
O17 Nd2 O16 112.4(2) 2_666 . ?
O17 Nd2 O17 65.6(3) 2_666 . ?
O17 Nd2 O19 76.3(2) 2_666 . ?
O19 Nd2 O16 123.3(2) . . ?
O19 Nd2 O17 122.28(18) . . ?
O20 Nd2 O1 142.2(2) . . ?
O20 Nd2 O16 76.1(2) . . ?
O20 Nd2 O17 75.50(19) . . ?
O20 Nd2 O17 72.9(2) . 2_666 ?
O20 Nd2 O19 52.1(2) . . ?
Nd1 Na1 H2ZD 110(3) 2_667 . ?
O2 Na1 Nd1 103.28(17) . 2_667 ?
O2 Na1 O5 78.5(2) . . ?
O2 Na1 O7 65.7(2) . 2_667 ?
O2 Na1 O12 83.3(3) . 1_455 ?
O2 Na1 H2ZD 85.6(18) . . ?
O2Z Na1 Nd1 95.1(2) . 2_667 ?
O2Z Na1 O2 104.7(3) . . ?
O2Z Na1 O5 175.5(3) . . ?
O2Z Na1 O7 96.4(3) . 2_667 ?
O2Z Na1 O11 96.3(3) . 2_667 ?
O2Z Na1 O12 97.2(3) . 1_455 ?
O2Z Na1 H2ZD 21.9(5) . . ?
O5 Na1 Nd1 81.01(16) . 2_667 ?
O5 Na1 O7 82.0(2) . 2_667 ?
O5 Na1 H2ZD 162.4(7) . . ?
O7 Na1 Nd1 38.52(14) 2_667 2_667 ?
O7 Na1 H2ZD 98(4) 2_667 . ?
O11 Na1 Nd1 35.22(15) 2_667 2_667 ?
O11 Na1 O2 135.6(3) 2_667 . ?
O11 Na1 O5 79.3(2) 2_667 . ?
O11 Na1 O7 73.5(2) 2_667 2_667 ?
O11 Na1 O12 132.7(3) 2_667 1_455 ?
O11 Na1 H2ZD 117.8(9) 2_667 . ?
O12 Na1 Nd1 164.1(2) 1_455 2_667 ?
O12 Na1 O5 86.3(3) 1_455 . ?
O12 Na1 O7 148.4(3) 1_455 2_667 ?
O12 Na1 H2ZD 85(3) 1_455 . ?
Nd2 O1 Nd1 108.63(19) . . ?
C1 O1 Nd1 91.9(5) . . ?
C1 O1 Nd2 126.7(5) . . ?
Nd2 O1Z H1Z1 120.0 . . ?
Nd2 O1Z H1Z2 120.0 . . ?
H1Z1 O1Z H1Z2 120.0 . . ?
Na1 O2 Nd1 93.8(2) . . ?
C1 O2 Nd1 94.7(5) . . ?
C1 O2 Na1 154.2(6) . . ?
Na1 O2Z H2ZD 83.6(15) . . ?
C2Z O2Z Na1 124.1(6) . . ?
C2Z O2Z H2ZD 151(3) . . ?
C7 O3 H3H 109.5 . . ?
H3ZA O3Z H3ZB 99(10) . . ?
Nd2 O4 Nd1 112.0(2) . . ?
C10 O4 Nd1 94.5(5) . . ?
C10 O4 Nd2 137.8(6) . . ?
Na1 O5 Nd1 91.6(2) . . ?
C10 O5 Nd1 92.8(6) . . ?
C10 O5 Na1 139.1(5) . . ?
C5Z O5Z H5ZD 109.5 . . ?
C16 O6 H6H 109.5 . . ?
C6Z O6Z H6ZD 109.5 . . ?
Nd1 O7 Nd1 116.6(2) 2_667 . ?
Nd1 O7 Na1 101.1(2) . 2_667 ?
Nd1 O7 Na1 87.3(2) 2_667 2_667 ?
C19 O7 Nd1 147.0(6) . 2_667 ?
C19 O7 Nd1 92.2(6) . . ?
C19 O7 Na1 103.1(5) . 2_667 ?
C19 O8 Nd1 94.4(5) . . ?
C25 O9 H9H 109.5 . . ?
C28 O10 Nd1 95.3(5) . . ?
Na1 O11 Nd1 113.1(3) 2_667 . ?
C28 O11 Nd1 91.8(5) . . ?
C28 O11 Na1 149.2(6) . 2_667 ?
Na1 O12 H14H 102(9) 1_655 . ?
C34 O12 Na1 126.3(6) . 1_655 ?
C34 O12 H14H 100(10) . . ?
C37 O13 Nd1 142.1(7) . . ?
C37 O14 Nd2 141.9(7) . . ?
C43 O15 H15H 109.5 . . ?
C46 O16 Nd2 94.7(6) . . ?
Nd2 O17 Nd2 114.4(3) 2_666 . ?
C46 O17 Nd2 94.6(6) . . ?
C46 O17 Nd2 148.4(7) . 2_666 ?
C52 O18 H18H 118(10) . . ?
C55 O19 Nd2 92.9(5) . . ?
C55 O20 Nd2 93.7(5) . . ?
C61 O21 H21 109.5 . . ?
O1 C1 C2 118.3(9) . . ?
O2 C1 O1 121.5(8) . . ?
O2 C1 C2 120.2(9) . . ?
C1 C2 H2A 108.1 . . ?
C1 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
C3 C2 C1 116.9(8) . . ?
C3 C2 H2A 108.1 . . ?
C3 C2 H2B 108.1 . . ?
O2Z C2Z H2ZA 109.5 . . ?
O2Z C2Z H2ZB 109.5 . . ?
O2Z C2Z H2ZC 109.5 . . ?
H2ZA C2Z H2ZB 109.5 . . ?
H2ZA C2Z H2ZC 109.5 . . ?
H2ZB C2Z H2ZC 109.5 . . ?
C2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
C2 C3 C4 112.3(9) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C5 C4 C3 120.8(9) . . ?
C5 C4 C9 118.8(9) . . ?
C9 C4 C3 120.4(9) . . ?
C4Z O4Z H4Z 159(9) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(9) . . ?
C6 C5 H5 119.4 . . ?
O5Z C5Z H5ZA 109.5 . . ?
O5Z C5Z H5ZB 109.5 . . ?
O5Z C5Z H5ZC 109.5 . . ?
H5ZA C5Z H5ZB 109.5 . . ?
H5ZA C5Z H5ZC 109.5 . . ?
H5ZB C5Z H5ZC 109.5 . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.2(9) . . ?
C7 C6 H6 120.4 . . ?
O6Z C6Z H6ZA 109.5 . . ?
O6Z C6Z H6ZB 109.5 . . ?
O6Z C6Z H6ZC 109.5 . . ?
H6ZA C6Z H6ZB 109.5 . . ?
H6ZA C6Z H6ZC 109.5 . . ?
H6ZB C6Z H6ZC 109.5 . . ?
C6 C7 O3 117.1(9) . . ?
C8 C7 O3 122.2(9) . . ?
C8 C7 C6 120.7(9) . . ?
C7 C8 H8 120.3 . . ?
C7 C8 C9 119.4(9) . . ?
C9 C8 H8 120.3 . . ?
C4 C9 C8 120.6(9) . . ?
C4 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
O4 C10 O5 120.8(8) . . ?
O4 C10 C11 116.3(9) . . ?
O5 C10 C11 122.8(9) . . ?
C10 C11 H11A 107.9 . . ?
C10 C11 H11B 107.9 . . ?
C10 C11 C12 117.5(8) . . ?
H11A C11 H11B 107.2 . . ?
C12 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
C13 C12 C11 111.8(9) . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C14 C13 C12 123.0(9) . . ?
C18 C13 C12 122.3(9) . . ?
C18 C13 C14 113.5(9) . . ?
C13 C14 H14 118.1 . . ?
C13 C14 C15 123.7(10) . . ?
C15 C14 H14 118.1 . . ?
C14 C15 H15 120.7 . . ?
C16 C15 C14 118.6(10) . . ?
C16 C15 H15 120.7 . . ?
O6 C16 C15 118.6(9) . . ?
C17 C16 O6 123.1(9) . . ?
C17 C16 C15 118.1(10) . . ?
C16 C17 H17 119.1 . . ?
C16 C17 C18 121.9(10) . . ?
C18 C17 H17 119.1 . . ?
C13 C18 H18 118.2 . . ?
C17 C18 C13 123.5(10) . . ?
C17 C18 H18 118.2 . . ?
O7 C19 C20 119.0(10) . . ?
O8 C19 O7 121.0(8) . . ?
O8 C19 C20 119.9(9) . . ?
C19 C20 H20A 107.8 . . ?
C19 C20 H20B 107.8 . . ?
H20A C20 H20B 107.2 . . ?
C21 C20 C19 117.8(11) . . ?
C21 C20 H20A 107.8 . . ?
C21 C20 H20B 107.8 . . ?
C20 C21 H21A 108.2 . . ?
C20 C21 H21B 108.2 . . ?
C20 C21 C22 116.2(12) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
C23 C22 C21 126.0(13) . . ?
C27 C22 C21 115.8(13) . . ?
C27 C22 C23 118.2(14) . . ?
C22 C23 H23 118.7 . . ?
C22 C23 C24 122.6(15) . . ?
C24 C23 H23 118.7 . . ?
C23 C24 H24 120.8 . . ?
C25 C24 C23 118.3(14) . . ?
C25 C24 H24 120.8 . . ?
C24 C25 O9 118.0(11) . . ?
C24 C25 C26 118.9(13) . . ?
C26 C25 O9 123.0(12) . . ?
C25 C26 H26 118.8 . . ?
C25 C26 C27 122.3(14) . . ?
C27 C26 H26 118.8 . . ?
C22 C27 C26 119.4(14) . . ?
C22 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
O10 C28 C29 118.1(8) . . ?
O11 C28 O10 120.6(8) . . ?
O11 C28 C29 121.2(8) . . ?
C28 C29 H29A 108.8 . . ?
C28 C29 H29B 108.8 . . ?
C28 C29 C30 113.7(8) . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
C29 C30 H30A 109.0 . . ?
C29 C30 H30B 109.0 . . ?
C29 C30 C31 112.7(8) . . ?
H30A C30 H30B 107.8 . . ?
C31 C30 H30A 109.0 . . ?
C31 C30 H30B 109.0 . . ?
C32 C31 C30 121.5(10) . . ?
C36 C31 C30 121.4(10) . . ?
C36 C31 C32 117.1(10) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 C31 122.5(11) . . ?
C33 C32 H32 118.7 . . ?
C32 C33 H33 120.8 . . ?
C32 C33 C34 118.4(10) . . ?
C34 C33 H33 120.8 . . ?
C33 C34 O12 118.7(8) . . ?
C35 C34 O12 121.7(9) . . ?
C35 C34 C33 119.6(9) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.1(10) . . ?
C36 C35 H35 120.0 . . ?
C31 C36 H36 118.9 . . ?
C35 C36 C31 122.2(10) . . ?
C35 C36 H36 118.9 . . ?
O13 C37 O14 124.0(10) . . ?
O13 C37 C38 118.1(9) . . ?
O14 C37 C38 117.8(9) . . ?
C37 C38 H38A 110.5 . . ?
C37 C38 H38B 110.5 . . ?
H38A C38 H38B 108.7 . . ?
C39 C38 C37 106.3(9) . . ?
C39 C38 H38A 110.5 . . ?
C39 C38 H38B 110.5 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
C38 C39 C40 110.4(10) . . ?
H39A C39 H39B 108.1 . . ?
C40 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
C41 C40 C39 122.3(13) . . ?
C45 C40 C39 120.0(11) . . ?
C45 C40 C41 117.8(13) . . ?
C40 C41 H41 118.9 . . ?
C42 C41 C40 122.3(13) . . ?
C42 C41 H41 118.9 . . ?
C41 C42 H42 120.7 . . ?
C43 C42 C41 118.6(11) . . ?
C43 C42 H42 120.7 . . ?
O15 C43 C42 117.8(9) . . ?
O15 C43 C44 120.8(10) . . ?
C42 C43 C44 121.2(11) . . ?
C43 C44 H44 120.6 . . ?
C43 C44 C45 118.8(11) . . ?
C45 C44 H44 120.6 . . ?
C40 C45 C44 121.3(11) . . ?
C40 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
O16 C46 C47 117.5(9) . . ?
O17 C46 O16 120.8(10) . . ?
O17 C46 C47 121.2(9) . . ?
C46 C47 H47A 109.3 . . ?
C46 C47 H47B 109.3 . . ?
H47A C47 H47B 108.0 . . ?
C48 C47 C46 111.6(10) . . ?
C48 C47 H47A 109.3 . . ?
C48 C47 H47B 109.3 . . ?
C47 C48 H48A 110.2 . . ?
C47 C48 H48B 110.2 . . ?
C47 C48 C49 107.5(10) . . ?
H48A C48 H48B 108.5 . . ?
C49 C48 H48A 110.2 . . ?
C49 C48 H48B 110.2 . . ?
C50 C49 C48 120.7(12) . . ?
C54 C49 C48 122.1(11) . . ?
C54 C49 C50 116.9(12) . . ?
C49 C50 H50 119.2 . . ?
C49 C50 C51 121.7(12) . . ?
C51 C50 H50 119.2 . . ?
C50 C51 H51 120.4 . . ?
C52 C51 C50 119.2(11) . . ?
C52 C51 H51 120.4 . . ?
O18 C52 C51 121.0(10) . . ?
O18 C52 C53 120.0(12) . . ?
C53 C52 C51 118.9(10) . . ?
C52 C53 H53 119.5 . . ?
C52 C53 C54 121.1(12) . . ?
C54 C53 H53 119.5 . . ?
C49 C54 C53 121.8(12) . . ?
C49 C54 H54 119.1 . . ?
C53 C54 H54 119.1 . . ?
O19 C55 O20 120.6(8) . . ?
O19 C55 C56 120.5(8) . . ?
O20 C55 C56 118.9(9) . . ?
C55 C56 H56A 108.5 . . ?
C55 C56 H56B 108.5 . . ?
C55 C56 C57 115.3(9) . . ?
H56A C56 H56B 107.5 . . ?
C57 C56 H56A 108.5 . . ?
C57 C56 H56B 108.5 . . ?
C56 C57 H57A 109.2 . . ?
C56 C57 H57B 109.2 . . ?
H57A C57 H57B 107.9 . . ?
C58 C57 C56 111.9(9) . . ?
C58 C57 H57A 109.2 . . ?
C58 C57 H57B 109.2 . . ?
C59 C58 C57 121.4(10) . . ?
C59 C58 C63 118.1(9) . . ?
C63 C58 C57 120.5(10) . . ?
C58 C59 H59 119.0 . . ?
C58 C59 C60 121.9(9) . . ?
C60 C59 H59 119.0 . . ?
C59 C60 H60 120.8 . . ?
C61 C60 C59 118.3(9) . . ?
C61 C60 H60 120.8 . . ?
C60 C61 O21 120.6(9) . . ?
C62 C61 O21 118.1(9) . . ?
C62 C61 C60 121.3(9) . . ?
C61 C62 H62 119.7 . . ?
C61 C62 C63 120.6(10) . . ?
C63 C62 H62 119.7 . . ?
C58 C63 H63 120.2 . . ?
C62 C63 C58 119.7(10) . . ?
C62 C63 H63 120.2 . . ?
O4Z C4Z H4Z1 109.5 . . ?
O4Z C4Z H4Z2 109.5 . . ?
O4Z C4Z H4Z3 109.5 . . ?
H4Z1 C4Z H4Z2 109.5 . . ?
H4Z1 C4Z H4Z3 109.5 . . ?
H4Z2 C4Z H4Z3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1Z H1Z1 O15 0.95 2.20 2.751(9) 115.7 2_766
O1Z H1Z2 O20 0.95 1.89 2.647(8) 134.7 2_666
O3 H3H O3Z 0.84 2.05 2.816(10) 151.5 1_545
O5Z H5ZD O10 0.84 1.90 2.692(10) 157.4 .
O6 H6H O6Z 0.84 1.75 2.588(10) 177.3 1_455
O6Z H6ZD O21 0.84 1.93 2.755(11) 165.0 2_676
O9 H9H O4Z 0.84 2.39 2.674(13) 100.3 1_565
O15 H15H O5Z 0.84 1.84 2.631(12) 156.8 2_766
O21 H21 O3Z 0.84 1.86 2.682(12) 167.3 2_676
O3Z H3ZA O8 0.91(2) 1.96(5) 2.794(9) 152(10) .
O3Z H3ZB O19 0.91(2) 1.93(5) 2.800(9) 159(13) .
O18 H18H O6 0.92(2) 2.12(13) 2.637(11) 115(11) 1_545
O4Z H4Z O9 0.95(2) 2.56(15) 2.674(13) 87(9) 1_545

_olex2_submission_special_instructions 'No special instructions were received'

#=======================================================
#ALERT LEVEL B
_vrf_PLAT420                     
;
PROBLEMS: D-H Without Acceptor O12 - H14H .. Please Check;
RESPONSE: The listed hydrogen bonds have been checked, but not found.
;
_vrf_PLAT482                     
;
PROBLEM:Small D-H..A Angle Rep for O4Z .. O9 .. 87.00 Degree
RESPONSE: Probably the listed weak hydrogen bond of the small angle 
subjects to the effects of other stronger chemical bonds in the proximity.
;
#=======================================================
