Electronic Supplementary Material for CrystEngComm
This Journal is (c) The Royal Society of Chemistry 2007

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Peter Junk'
'Phil Andrews'
'Benjamin Fraser'
'Massimiliano Massi'
'Morry Silberstein'

_publ_contact_author_name        'Peter Junk'
_publ_contact_author_address     
;
School of Chemistry
Monash University
PO Box 23
Clayton
Victoria
3800
AUSTRALIA
;

_publ_contact_author_email       PETER.JUNK@SCI.MONASH.EDU.AU

_publ_requested_journal          'Cryst Eng. Comm.'

_publ_section_title              
;
Diol-functionalised Benzoates as Novel Linkers for the
Formation of Coordination Polymers
;

# Attachment 'DBAH.CIF'

data_D:\DBAH\ORTHO.CIF
_database_code_depnum_ccdc_archive 'CCDC 628107'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(R)-4-(2,3-dihydroxypropoxy) benzoic acid
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H12 O5'
_chemical_formula_sum            'C10 H12 O5'
_chemical_formula_weight         212.20

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   7.7901(3)
_cell_length_b                   10.8098(4)
_cell_length_c                   23.0523(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1941.22(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24115
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2547
_reflns_number_gt                2485
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius Collect'
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        Nonius
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+0.5572P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_chemical_absolute_configuration syn
_refine_ls_number_reflns         2547
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1130
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.9164(2) 0.78400(17) 0.87998(6) 0.0224(4) Uani 1 1 d . . .
O2 O 0.7586(3) 0.95462(17) 0.86518(7) 0.0242(4) Uani 1 1 d . . .
O3 O 1.0085(2) 0.86737(15) 0.60905(6) 0.0168(4) Uani 1 1 d . . .
O4 O 1.2349(2) 0.72318(13) 0.49141(6) 0.0145(3) Uani 1 1 d . . .
O5 O 1.3352(2) 0.97475(16) 0.47422(7) 0.0202(4) Uani 1 1 d . . .
O6 O 0.6038(2) 0.72142(16) 0.61683(6) 0.0220(4) Uani 1 1 d . . .
O7 O 0.7405(2) 0.54302(16) 0.63489(7) 0.0224(4) Uani 1 1 d . . .
O8 O 0.4891(2) 0.64740(15) 0.88879(6) 0.0165(3) Uani 1 1 d . . .
O9 O 0.47299(19) 0.67555(14) 1.00837(6) 0.0116(3) Uani 1 1 d . . .
O10 O 0.1960(2) 0.51337(15) 1.02357(7) 0.0162(3) Uani 1 1 d . . .
C1 C 0.8576(3) 0.8621(2) 0.84747(9) 0.0152(4) Uani 1 1 d . . .
C2 C 0.8921(3) 0.8623(2) 0.78431(8) 0.0138(4) Uani 1 1 d . . .
C3 C 0.9953(3) 0.7688(2) 0.76168(8) 0.0152(4) Uani 1 1 d . . .
H3 H 1.0378 0.7077 0.7862 0.018 Uiso 1 1 calc R . .
C4 C 1.0358(3) 0.7658(2) 0.70273(9) 0.0148(4) Uani 1 1 d . . .
H4 H 1.1042 0.7029 0.6878 0.018 Uiso 1 1 calc R . .
C5 C 0.9727(3) 0.8579(2) 0.66678(8) 0.0140(4) Uani 1 1 d . . .
C6 C 0.8651(3) 0.9499(2) 0.68867(9) 0.0158(4) Uani 1 1 d . . .
H6 H 0.8205 1.0097 0.6639 0.019 Uiso 1 1 calc R . .
C7 C 0.8246(3) 0.9524(2) 0.74717(9) 0.0151(4) Uani 1 1 d . . .
H7 H 0.7528 1.0138 0.7617 0.018 Uiso 1 1 calc R . .
C8 C 1.1124(3) 0.7735(2) 0.58256(8) 0.0140(4) Uani 1 1 d . . .
H8A H 1.0479 0.6973 0.5784 0.017 Uiso 1 1 calc R . .
H8B H 1.2135 0.7572 0.6059 0.017 Uiso 1 1 calc R . .
C9 C 1.1630(3) 0.8239(2) 0.52357(8) 0.0121(4) Uani 1 1 d . . .
H9 H 1.0610 0.8554 0.5035 0.014 Uiso 1 1 calc R . .
C10 C 1.2940(3) 0.9265(2) 0.52992(9) 0.0161(4) Uani 1 1 d . . .
H10A H 1.2479 0.9917 0.5542 0.019 Uiso 1 1 calc R . .
H10B H 1.3969 0.8945 0.5483 0.019 Uiso 1 1 calc R . .
C11 C 0.6481(3) 0.6406(2) 0.65055(9) 0.0152(4) Uani 1 1 d . . .
C12 C 0.6071(3) 0.6432(2) 0.71348(9) 0.0143(4) Uani 1 1 d . . .
C13 C 0.5021(3) 0.7367(2) 0.73487(8) 0.0149(4) Uani 1 1 d . . .
H13 H 0.4591 0.7960 0.7095 0.018 Uiso 1 1 calc R . .
C14 C 0.4603(3) 0.7432(2) 0.79345(9) 0.0144(4) Uani 1 1 d . . .
H14 H 0.3906 0.8066 0.8073 0.017 Uiso 1 1 calc R . .
C15 C 0.5242(3) 0.6534(2) 0.83120(8) 0.0133(4) Uani 1 1 d . . .
C16 C 0.6338(3) 0.5608(2) 0.81019(9) 0.0150(4) Uani 1 1 d . . .
H16 H 0.6792 0.5026 0.8356 0.018 Uiso 1 1 calc R . .
C17 C 0.6744(3) 0.5558(2) 0.75199(9) 0.0148(4) Uani 1 1 d . . .
H17 H 0.7469 0.4939 0.7383 0.018 Uiso 1 1 calc R . .
C18 C 0.3743(3) 0.7368(2) 0.91372(8) 0.0146(4) Uani 1 1 d . . .
H18A H 0.2736 0.7468 0.8894 0.018 Uiso 1 1 calc R . .
H18B H 0.4310 0.8164 0.9172 0.018 Uiso 1 1 calc R . .
C19 C 0.3230(3) 0.68878(19) 0.97326(8) 0.0110(4) Uani 1 1 d . . .
H19 H 0.2456 0.7487 0.9916 0.013 Uiso 1 1 calc R . .
C20 C 0.2302(3) 0.5657(2) 0.96736(9) 0.0139(4) Uani 1 1 d . . .
H20A H 0.1229 0.5779 0.9468 0.017 Uiso 1 1 calc R . .
H20B H 0.3002 0.5089 0.9450 0.017 Uiso 1 1 calc R . .
H2O H 0.740(5) 0.950(3) 0.9015(16) 0.044(10) Uiso 1 1 d . . .
H4O H 1.202(4) 0.741(3) 0.4565(14) 0.034(9) Uiso 1 1 d . . .
H5O H 1.405(4) 1.038(3) 0.4808(13) 0.023(8) Uiso 1 1 d . . .
H7O H 0.752(6) 0.544(4) 0.5977(18) 0.059(12) Uiso 1 1 d . . .
H9O H 0.452(3) 0.693(2) 1.0407(12) 0.009(6) Uiso 1 1 d . . .
H10O H 0.202(5) 0.440(3) 1.0188(15) 0.040(10) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0317(9) 0.0250(8) 0.0106(7) -0.0007(7) 0.0001(7) 0.0048(8)
O2 0.0365(10) 0.0262(8) 0.0099(7) -0.0035(6) 0.0047(7) 0.0084(9)
O3 0.0230(9) 0.0182(8) 0.0091(6) 0.0021(5) 0.0044(6) 0.0073(7)
O4 0.0216(8) 0.0141(7) 0.0078(6) -0.0009(5) 0.0022(6) 0.0023(6)
O5 0.0254(9) 0.0240(8) 0.0112(7) 0.0016(6) -0.0011(6) -0.0136(8)
O6 0.0326(9) 0.0225(8) 0.0109(6) 0.0024(6) 0.0034(7) 0.0038(8)
O7 0.0334(10) 0.0234(8) 0.0105(7) 0.0001(6) 0.0034(7) 0.0082(8)
O8 0.0205(8) 0.0195(8) 0.0094(6) 0.0024(6) 0.0044(6) 0.0078(7)
O9 0.0104(6) 0.0161(7) 0.0085(6) -0.0016(5) -0.0014(5) 0.0012(6)
O10 0.0238(8) 0.0152(8) 0.0098(7) -0.0003(6) 0.0014(6) -0.0048(7)
C1 0.0179(10) 0.0168(10) 0.0110(8) -0.0047(8) 0.0000(8) -0.0034(9)
C2 0.0155(10) 0.0162(10) 0.0096(9) -0.0031(8) 0.0013(8) -0.0017(9)
C3 0.0165(10) 0.0163(10) 0.0127(9) 0.0025(8) 0.0005(9) -0.0006(9)
C4 0.0156(10) 0.0156(10) 0.0133(9) -0.0011(8) 0.0025(8) 0.0026(9)
C5 0.0131(9) 0.0178(10) 0.0113(9) -0.0007(8) 0.0006(7) -0.0013(9)
C6 0.0184(10) 0.0156(9) 0.0135(9) 0.0010(8) -0.0005(8) 0.0026(9)
C7 0.0178(10) 0.0137(9) 0.0139(9) -0.0026(8) 0.0015(8) 0.0025(9)
C8 0.0158(10) 0.0154(9) 0.0108(8) -0.0001(8) 0.0021(8) 0.0008(9)
C9 0.0120(9) 0.0144(9) 0.0099(8) -0.0013(7) 0.0002(7) 0.0011(9)
C10 0.0205(10) 0.0193(10) 0.0083(8) -0.0007(8) -0.0001(8) -0.0075(10)
C11 0.0178(10) 0.0146(10) 0.0132(9) -0.0018(8) 0.0001(8) -0.0025(9)
C12 0.0144(10) 0.0154(10) 0.0130(9) 0.0006(8) -0.0015(8) -0.0025(9)
C13 0.0169(10) 0.0150(10) 0.0128(9) 0.0013(7) -0.0026(8) 0.0007(9)
C14 0.0166(10) 0.0135(9) 0.0132(9) 0.0022(8) 0.0013(8) 0.0035(9)
C15 0.0133(9) 0.0149(10) 0.0116(9) 0.0012(7) 0.0026(7) -0.0014(9)
C16 0.0170(10) 0.0151(9) 0.0128(9) 0.0028(8) 0.0001(8) 0.0011(9)
C17 0.0155(10) 0.0136(10) 0.0152(10) -0.0016(8) 0.0018(8) -0.0003(9)
C18 0.0169(10) 0.0165(9) 0.0106(8) 0.0022(8) 0.0043(8) 0.0064(9)
C19 0.0119(9) 0.0123(9) 0.0087(8) 0.0008(7) -0.0007(7) 0.0018(8)
C20 0.0168(10) 0.0168(9) 0.0081(8) -0.0007(7) -0.0002(8) -0.0007(9)

_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
O1 C1 1.219(3) . ?
O2 C1 1.327(3) . ?
O2 H2O 0.85(4) . ?
O3 C5 1.363(2) . ?
O3 C8 1.434(3) . ?
O4 C9 1.432(2) . ?
O4 H4O 0.87(3) . ?
O5 C10 1.423(3) . ?
O5 H5O 0.89(3) . ?
O6 C11 1.219(3) . ?
O7 C11 1.327(3) . ?
O7 H7O 0.86(4) . ?
O8 C15 1.357(2) . ?
O8 C18 1.437(3) . ?
O9 C19 1.429(2) . ?
O9 H9O 0.79(3) . ?
O10 C20 1.439(2) . ?
O10 H10O 0.80(4) . ?
C1 C2 1.481(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.400(3) . ?
C3 C4 1.395(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(3) . ?
C6 C7 1.385(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.517(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.514(3) . ?
C9 H9 0.9800 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.486(3) . ?
C12 C13 1.390(3) . ?
C12 C17 1.399(3) . ?
C13 C14 1.391(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.396(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.402(3) . ?
C16 C17 1.380(3) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.521(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.520(3) . ?
C19 H19 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O2 H2O 111(3) . . ?
C5 O3 C8 118.55(16) . . ?
C9 O4 H4O 101(2) . . ?
C10 O5 H5O 105(2) . . ?
C11 O7 H7O 109(3) . . ?
C15 O8 C18 118.98(16) . . ?
C19 O9 H9O 110.1(19) . . ?
C20 O10 H10O 105(3) . . ?
O1 C1 O2 123.46(19) . . ?
O1 C1 C2 122.5(2) . . ?
O2 C1 C2 114.04(19) . . ?
C3 C2 C7 119.53(18) . . ?
C3 C2 C1 118.19(19) . . ?
C7 C2 C1 122.3(2) . . ?
C2 C3 C4 120.8(2) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.0(2) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
O3 C5 C4 124.4(2) . . ?
O3 C5 C6 114.99(19) . . ?
C4 C5 C6 120.60(19) . . ?
C7 C6 C5 120.2(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C2 119.7(2) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
O3 C8 C9 105.91(16) . . ?
O3 C8 H8A 110.6 . . ?
C9 C8 H8A 110.6 . . ?
O3 C8 H8B 110.6 . . ?
C9 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
O4 C9 C10 110.04(17) . . ?
O4 C9 C8 107.02(16) . . ?
C10 C9 C8 110.57(16) . . ?
O4 C9 H9 109.7 . . ?
C10 C9 H9 109.7 . . ?
C8 C9 H9 109.7 . . ?
O5 C10 C9 109.47(16) . . ?
O5 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
O6 C11 O7 123.36(19) . . ?
O6 C11 C12 123.2(2) . . ?
O7 C11 C12 113.42(18) . . ?
C13 C12 C17 119.13(19) . . ?
C13 C12 C11 119.12(19) . . ?
C17 C12 C11 121.7(2) . . ?
C12 C13 C14 121.26(19) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C15 119.1(2) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
O8 C15 C14 124.8(2) . . ?
O8 C15 C16 115.25(19) . . ?
C14 C15 C16 119.90(18) . . ?
C17 C16 C15 120.28(19) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C12 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
C12 C17 H17 119.9 . . ?
O8 C18 C19 107.14(16) . . ?
O8 C18 H18A 110.3 . . ?
C19 C18 H18A 110.3 . . ?
O8 C18 H18B 110.3 . . ?
C19 C18 H18B 110.3 . . ?
H18A C18 H18B 108.5 . . ?
O9 C19 C20 110.61(16) . . ?
O9 C19 C18 109.28(17) . . ?
C20 C19 C18 110.07(16) . . ?
O9 C19 H19 108.9 . . ?
C20 C19 H19 108.9 . . ?
C18 C19 H19 108.9 . . ?
O10 C20 C19 110.57(16) . . ?
O10 C20 H20A 109.5 . . ?
C19 C20 H20A 109.5 . . ?
O10 C20 H20B 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?

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
O2 H2O O10 0.85(4) 1.80(4) 2.633(2) 164(4) 3_567

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.053

# Attachment 'LaDBAH3.CIF'

data_D:\LaDBA3\NEW.CIF
_database_code_depnum_ccdc_archive 'CCDC 628108'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Lanthanum (R)-4-(2,3-dihydroxypropoxy) benzoate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H74 La2 O34, 3(H2 O)'
_chemical_formula_sum            'C60 H80 La2 O37'
_chemical_formula_weight         1671.0808

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P1
_symmetry_space_group_name_Hall  P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   11.2283(3)
_cell_length_b                   12.8350(3)
_cell_length_c                   13.7238(4)
_cell_angle_alpha                66.370(1)
_cell_angle_beta                 88.669(1)
_cell_angle_gamma                65.326(1)
_cell_volume                     1621.69(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block-shaped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             850
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7206
_exptl_absorpt_correction_T_max  0.8172
_exptl_absorpt_process_details   DENZO-SMN

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25214
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.50
_reflns_number_total             12244
_reflns_number_gt                12085
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius Collect'
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        Nonius
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+0.2153P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12244
_refine_ls_number_parameters     982
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0163
_refine_ls_wR_factor_ref         0.0403
_refine_ls_wR_factor_gt          0.0401
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.727400(8) 0.969193(8) 0.956764(7) 0.00890(4) Uani 1 1 d . . .
La2 La 0.274339(8) 1.028787(8) 1.043867(7) 0.00899(4) Uani 1 1 d . . .
O1 O 0.8980(2) 1.0607(2) 0.85415(19) 0.0177(5) Uani 1 1 d . . .
O2 O 0.6836(2) 1.1890(2) 0.81368(19) 0.0166(5) Uani 1 1 d . . .
O3 O 0.82887(16) 1.40174(16) 0.35223(13) 0.0182(3) Uani 1 1 d . . .
O4 O 0.82414(19) 1.57215(16) 0.15167(14) 0.0238(4) Uani 1 1 d D . .
O5 O 0.8952(3) 1.4022(3) 0.0382(2) 0.0359(6) Uani 1 1 d . . .
O6 O 0.7735(2) 0.9306(2) 0.79201(19) 0.0147(5) Uani 1 1 d . . .
O7 O 0.6833(2) 0.8127(2) 0.77375(19) 0.0214(5) Uani 1 1 d . . .
O8 O 0.72434(18) 1.10999(19) 0.28643(15) 0.0156(4) Uani 1 1 d . . .
O9 O 0.60675(19) 1.1357(2) 0.03093(18) 0.0136(4) Uani 1 1 d D . .
O10 O 0.8632(2) 0.9954(2) 0.08600(18) 0.0124(4) Uani 1 1 d . . .
O11 O 0.4995(2) 1.0701(2) 0.86645(18) 0.0155(5) Uani 1 1 d . . .
O12 O 0.2800(2) 1.1576(2) 0.85463(19) 0.0159(5) Uani 1 1 d . . .
O13 O 0.29692(18) 1.4112(2) 0.35897(16) 0.0174(4) Uani 1 1 d . . .
O14 O 0.22240(19) 1.46423(19) 0.15126(15) 0.0201(4) Uani 1 1 d . . .
O15 O 0.55256(19) 1.4495(2) 0.12049(18) 0.0345(5) Uani 1 1 d . . .
H15O H 0.5419 1.5100 0.1353 0.041 Uiso 1 1 calc R . .
O16 O 0.3227(2) 0.8072(2) 1.20030(19) 0.0151(5) Uani 1 1 d . . .
O17 O 0.1108(2) 0.9385(2) 1.14283(18) 0.0156(5) Uani 1 1 d . . .
O18 O 0.08437(18) 0.61307(18) 1.62643(14) 0.0255(4) Uani 1 1 d . . .
O19 O 0.29886(17) 0.44605(16) 1.88903(14) 0.0204(3) Uani 1 1 d D . .
O20 O 0.1038(3) 0.6377(2) 1.9294(2) 0.0340(6) Uani 1 1 d . . .
O21 O 0.2200(2) 1.0822(2) 1.1995(2) 0.0171(5) Uani 1 1 d . . .
O22 O 0.2922(2) 1.2103(2) 1.22056(19) 0.0197(5) Uani 1 1 d . . .
O23 O 0.2236(2) 0.9088(2) 1.69968(17) 0.0247(5) Uani 1 1 d . . .
O24 O 0.1596(2) 0.9721(2) 1.91719(19) 0.0196(5) Uani 1 1 d . . .
O25 O 0.4149(2) 0.8558(2) 1.98777(19) 0.0172(5) Uani 1 1 d . . .
O26 O 0.5057(2) 0.9352(2) 1.12980(19) 0.0163(5) Uani 1 1 d . . .
O27 O 0.7244(2) 0.8272(2) 1.14778(18) 0.0146(5) Uani 1 1 d . . .
O28 O 0.66348(19) 0.6041(2) 1.63921(17) 0.0175(4) Uani 1 1 d . . .
O29 O 0.7034(2) 0.5763(2) 1.85060(16) 0.0310(5) Uani 1 1 d . . .
O30 O 0.52666(17) 0.41426(16) 1.81196(16) 0.0249(4) Uani 1 1 d . . .
H30O H 0.5579 0.3430 1.8106 0.030 Uiso 1 1 calc R . .
O31 O 0.6677(2) 0.7861(2) 0.9689(2) 0.0154(5) Uani 1 1 d D . .
O32 O 0.9520(2) 0.7827(3) 1.0226(2) 0.0211(5) Uani 1 1 d D . .
O33 O 0.3428(2) 1.2079(2) 1.0321(2) 0.0134(5) Uani 1 1 d . . .
O34 O 0.0522(2) 1.2251(2) 0.9658(2) 0.0188(5) Uani 1 1 d . . .
O35 O -0.0618(3) 1.3994(3) 0.7503(2) 0.0333(6) Uani 1 1 d D . .
O36 O 1.0350(2) 0.6259(2) 1.2410(2) 0.0229(5) Uani 1 1 d D . .
O37 O 0.54763(19) 1.58752(18) 0.22885(17) 0.0297(4) Uani 1 1 d D . .
C1 C 0.8005(3) 1.1567(3) 0.7885(3) 0.0131(7) Uani 1 1 d . . .
C2 C 0.8142(3) 1.2328(3) 0.6765(3) 0.0143(6) Uani 1 1 d . . .
C3 C 0.9363(3) 1.2009(3) 0.6434(3) 0.0207(7) Uani 1 1 d . . .
H3 H 1.0146 1.1389 0.6952 0.025 Uiso 1 1 calc R . .
C4 C 0.9466(3) 1.2580(3) 0.5354(2) 0.0156(6) Uani 1 1 d . . .
H4 H 1.0312 1.2359 0.5135 0.019 Uiso 1 1 calc R . .
C5 C 0.8320(3) 1.3473(3) 0.4607(2) 0.0135(5) Uani 1 1 d . . .
C6 C 0.7090(3) 1.3836(3) 0.4935(2) 0.0165(6) Uani 1 1 d . . .
H6 H 0.6311 1.4476 0.4420 0.020 Uiso 1 1 calc R . .
C7 C 0.6994(3) 1.3273(3) 0.6003(3) 0.0146(6) Uani 1 1 d . . .
H7 H 0.6151 1.3525 0.6224 0.018 Uiso 1 1 calc R . .
C8 C 0.9516(2) 1.3829(2) 0.3142(2) 0.0183(5) Uani 1 1 d . . .
H8A H 1.0116 1.2909 0.3418 0.022 Uiso 1 1 calc R . .
H8B H 0.9958 1.4220 0.3400 0.022 Uiso 1 1 calc R . .
C9 C 0.9229(2) 1.4439(2) 0.19215(19) 0.0189(5) Uani 1 1 d . . .
H9 H 1.0066 1.4434 0.1653 0.023 Uiso 1 1 calc R . .
C10 C 0.8782(3) 1.3726(3) 0.1482(2) 0.0235(6) Uani 1 1 d . . .
H10A H 0.9304 1.2801 0.1926 0.028 Uiso 1 1 calc R . .
H10B H 0.7833 1.3951 0.1531 0.028 Uiso 1 1 calc R . .
C11 C 0.7325(3) 0.8911(3) 0.7355(3) 0.0137(6) Uani 1 1 d . . .
C12 C 0.7366(3) 0.9428(3) 0.6176(2) 0.0113(6) Uani 1 1 d . . .
C13 C 0.6693(3) 0.9214(3) 0.5501(3) 0.0132(6) Uani 1 1 d . . .
H13 H 0.6264 0.8686 0.5807 0.016 Uiso 1 1 calc R . .
C14 C 0.6627(3) 0.9746(3) 0.4392(3) 0.0143(6) Uani 1 1 d . . .
H14 H 0.6156 0.9590 0.3943 0.017 Uiso 1 1 calc R . .
C15 C 0.7261(3) 1.0512(3) 0.3947(2) 0.0125(6) Uani 1 1 d . . .
C16 C 0.7966(3) 1.0724(3) 0.4617(2) 0.0158(6) Uani 1 1 d . . .
H16 H 0.8411 1.1237 0.4314 0.019 Uiso 1 1 calc R . .
C17 C 0.8012(3) 1.0186(3) 0.5715(3) 0.0167(6) Uani 1 1 d . . .
H17 H 0.8490 1.0333 0.6166 0.020 Uiso 1 1 calc R . .
C18 C 0.6618(2) 1.0808(2) 0.21811(19) 0.0126(5) Uani 1 1 d . . .
H18A H 0.5672 1.1052 0.2256 0.015 Uiso 1 1 calc R . .
H18B H 0.7071 0.9887 0.2372 0.015 Uiso 1 1 calc R . .
C19 C 0.6733 1.1569 0.1036 0.009 Uani 1 1 d . . .
H19 H 0.6294 1.2493 0.0868 0.011 Uiso 1 1 calc R . .
C20 C 0.8142(2) 1.1199(2) 0.08107(19) 0.0103(4) Uani 1 1 d . . .
H20A H 0.8150 1.1807 0.0087 0.012 Uiso 1 1 calc R . .
H20B H 0.8703 1.1199 0.1356 0.012 Uiso 1 1 calc R . .
C21 C 0.3829(3) 1.1419(3) 0.8132(3) 0.0115(6) Uani 1 1 d . . .
C22 C 0.3638(3) 1.2126(3) 0.6923(2) 0.0102(6) Uani 1 1 d . . .
C23 C 0.4722(3) 1.1976(3) 0.6375(3) 0.0159(7) Uani 1 1 d . . .
H23 H 0.5598 1.1434 0.6777 0.019 Uiso 1 1 calc R . .
C24 C 0.4549(3) 1.2594(3) 0.5270(3) 0.0134(6) Uani 1 1 d . . .
H24 H 0.5292 1.2460 0.4908 0.016 Uiso 1 1 calc R . .
C25 C 0.3262(3) 1.3422(3) 0.4691(3) 0.0144(6) Uani 1 1 d . . .
C26 C 0.2175(3) 1.3587(3) 0.5222(3) 0.0140(6) Uani 1 1 d . . .
H26 H 0.1301 1.4153 0.4821 0.017 Uiso 1 1 calc R . .
C27 C 0.2362(3) 1.2938(3) 0.6321(3) 0.0136(6) Uani 1 1 d . . .
H27 H 0.1613 1.3042 0.6676 0.016 Uiso 1 1 calc R . .
C28 C 0.4013(3) 1.3856(3) 0.2969(2) 0.0170(6) Uani 1 1 d . . .
H28A H 0.4393 1.2962 0.3075 0.020 Uiso 1 1 calc R . .
H28B H 0.4734 1.4015 0.3185 0.020 Uiso 1 1 calc R . .
C29 C 0.3365(3) 1.4756(2) 0.18031(19) 0.0165(5) Uani 1 1 d . . .
H29 H 0.3068 1.5645 0.1713 0.020 Uiso 1 1 calc R . .
C30 C 0.4299(3) 1.4536(2) 0.1002(2) 0.0234(5) Uani 1 1 d . . .
H30A H 0.4452 1.3724 0.0989 0.028 Uiso 1 1 calc R . .
H30B H 0.3842 1.5221 0.0273 0.028 Uiso 1 1 calc R . .
C31 C 0.2052(3) 0.8405(3) 1.2162(3) 0.0129(6) Uani 1 1 d . . .
C32 C 0.1755(3) 0.7745(3) 1.3232(3) 0.0137(6) Uani 1 1 d . . .
C33 C 0.2771(3) 0.6731(3) 1.4058(3) 0.0174(7) Uani 1 1 d . . .
H33 H 0.3653 0.6417 1.3917 0.021 Uiso 1 1 calc R . .
C34 C 0.2527(3) 0.6160(3) 1.5097(2) 0.0186(6) Uani 1 1 d . . .
H34 H 0.3239 0.5476 1.5658 0.022 Uiso 1 1 calc R . .
C35 C 0.1235(3) 0.6602(3) 1.5301(2) 0.0177(6) Uani 1 1 d . . .
C36 C 0.0206(3) 0.7592(3) 1.4483(3) 0.0175(6) Uani 1 1 d . . .
H36 H -0.0681 0.7880 1.4619 0.021 Uiso 1 1 calc R . .
C37 C 0.0461(3) 0.8167(3) 1.3466(3) 0.0139(6) Uani 1 1 d . . .
H37 H -0.0254 0.8862 1.2914 0.017 Uiso 1 1 calc R . .
C38 C 0.1773(3) 0.5092(2) 1.7198(2) 0.0227(5) Uani 1 1 d . . .
H38A H 0.2632 0.4688 1.6983 0.027 Uiso 1 1 calc R . .
H38B H 0.1437 0.4450 1.7527 0.027 Uiso 1 1 calc R . .
C39 C 0.1988(2) 0.5537(2) 1.80258(19) 0.0196(5) Uani 1 1 d . . .
H39 H 0.2300 0.6207 1.7689 0.024 Uiso 1 1 calc R . .
C40 C 0.0763(3) 0.6035(3) 1.8482(2) 0.0301(7) Uani 1 1 d . . .
H40A H 0.0053 0.6789 1.7897 0.036 Uiso 1 1 calc R . .
H40B H 0.0444 0.5378 1.8800 0.036 Uiso 1 1 calc R . .
C41 C 0.2518(3) 1.1262(3) 1.2565(3) 0.0136(6) Uani 1 1 d . . .
C42 C 0.2432(3) 1.0725(3) 1.3733(3) 0.0139(6) Uani 1 1 d . . .
C43 C 0.1713(3) 1.0015(3) 1.4129(3) 0.0149(6) Uani 1 1 d . . .
H43 H 0.1253 0.9897 1.3640 0.018 Uiso 1 1 calc R . .
C44 C 0.1666(3) 0.9486(3) 1.5214(3) 0.0203(7) Uani 1 1 d . . .
H44 H 0.1163 0.9021 1.5469 0.024 Uiso 1 1 calc R . .
C45 C 0.2356(3) 0.9636(3) 1.5933(2) 0.0172(6) Uani 1 1 d . . .
C46 C 0.3089(3) 1.0320(3) 1.5565(3) 0.0168(7) Uani 1 1 d . . .
H46 H 0.3572 1.0413 1.6059 0.020 Uiso 1 1 calc R . .
C47 C 0.3105(3) 1.0867(3) 1.4464(3) 0.0173(7) Uani 1 1 d . . .
H47 H 0.3590 1.1350 1.4209 0.021 Uiso 1 1 calc R . .
C48 C 0.2818(3) 0.9321(3) 1.7750(2) 0.0232(6) Uani 1 1 d . . .
H48A H 0.2502 1.0246 1.7503 0.028 Uiso 1 1 calc R . .
H48B H 0.3800 0.8915 1.7824 0.028 Uiso 1 1 calc R . .
C49 C 0.2385(3) 0.8744(2) 1.8851(2) 0.0196(5) Uani 1 1 d . . .
H49 H 0.1865 0.8298 1.8785 0.024 Uiso 1 1 calc R . .
C50 C 0.3585(3) 0.7829(2) 1.9709(2) 0.0248(5) Uani 1 1 d . . .
H50A H 0.3333 0.7364 2.0384 0.030 Uiso 1 1 calc R . .
H50B H 0.4231 0.7206 1.9475 0.030 Uiso 1 1 calc R . .
C51 C 0.6184(3) 0.8517(3) 1.1871(3) 0.0120(6) Uani 1 1 d . . .
C52 C 0.6275(3) 0.7845(3) 1.3054(3) 0.0128(6) Uani 1 1 d . . .
C53 C 0.5154(3) 0.8135(3) 1.3532(2) 0.0099(6) Uani 1 1 d . . .
H53 H 0.4313 0.8746 1.3089 0.012 Uiso 1 1 calc R . .
C54 C 0.5232(3) 0.7552(3) 1.4645(3) 0.0158(6) Uani 1 1 d . . .
H54 H 0.4454 0.7764 1.4960 0.019 Uiso 1 1 calc R . .
C55 C 0.6456(3) 0.6663(3) 1.5286(2) 0.0126(6) Uani 1 1 d . . .
C56 C 0.7600(3) 0.6346(3) 1.4833(3) 0.0163(7) Uani 1 1 d . . .
H56 H 0.8437 0.5728 1.5279 0.020 Uiso 1 1 calc R . .
C57 C 0.7508(3) 0.6943(3) 1.3719(3) 0.0141(6) Uani 1 1 d . . .
H57 H 0.8289 0.6737 1.3407 0.017 Uiso 1 1 calc R . .
C58 C 0.5508(3) 0.6471(3) 1.6887(2) 0.0153(5) Uani 1 1 d . . .
H58A H 0.4779 0.6350 1.6632 0.018 Uiso 1 1 calc R . .
H58B H 0.5185 0.7387 1.6692 0.018 Uiso 1 1 calc R . .
C59 C 0.5922(3) 0.5714(2) 1.80985(19) 0.0189(5) Uani 1 1 d . . .
H59 H 0.5157 0.6071 1.8445 0.023 Uiso 1 1 calc R . .
C60 C 0.6318(2) 0.4317(2) 1.8484(2) 0.0193(5) Uani 1 1 d . . .
H60A H 0.7127 0.3928 1.8205 0.023 Uiso 1 1 calc R . .
H60B H 0.6526 0.3890 1.9283 0.023 Uiso 1 1 calc R . .
H4O H 0.853(4) 1.612(3) 0.173(3) 0.060(12) Uiso 1 1 d D . .
H5O H 0.818(4) 1.455(4) 0.001(4) 0.055(13) Uiso 1 1 d . . .
H9O H 0.530(2) 1.147(3) 0.045(3) 0.026(9) Uiso 1 1 d D . .
H10O H 0.938(4) 0.965(4) 0.098(3) 0.032(11) Uiso 1 1 d . . .
H14O H 0.247(3) 1.394(3) 0.173(2) 0.012(7) Uiso 1 1 d . . .
H19O H 0.377(2) 0.433(3) 1.864(3) 0.040(9) Uiso 1 1 d D . .
H20O H 0.139(4) 0.565(4) 1.991(4) 0.041(12) Uiso 1 1 d . . .
H24O H 0.088(4) 1.000(4) 1.906(3) 0.025(10) Uiso 1 1 d . . .
H25O H 0.501(3) 0.823(3) 1.989(2) 0.019(8) Uiso 1 1 d . . .
H29O H 0.696(3) 0.651(4) 1.824(3) 0.035(9) Uiso 1 1 d . . .
H31A H 0.718(3) 0.722(3) 1.012(3) 0.019(9) Uiso 1 1 d . . .
H31B H 0.687(6) 0.782(6) 0.907(3) 0.10(2) Uiso 1 1 d D . .
H32A H 0.980(3) 0.739(3) 1.085(3) 0.016(8) Uiso 1 1 d . . .
H32B H 0.978(5) 0.744(5) 0.981(4) 0.09(2) Uiso 1 1 d D . .
H33A H 0.323(3) 1.214(3) 1.093(3) 0.017(8) Uiso 1 1 d . . .
H33B H 0.309(4) 1.288(4) 0.983(3) 0.036(11) Uiso 1 1 d . . .
H34A H 0.034(5) 1.276(5) 0.886(4) 0.080(17) Uiso 1 1 d . . .
H34B H 0.009(3) 1.267(3) 0.994(3) 0.023(9) Uiso 1 1 d . . .
H37A H 0.493(4) 1.670(2) 0.206(4) 0.085(15) Uiso 1 1 d D . .
H37B H 0.626(4) 1.594(4) 0.227(3) 0.049(10) Uiso 1 1 d . . .
H36A H 1.058(3) 0.661(3) 1.282(3) 0.037(10) Uiso 1 1 d . . .
H35A H -0.120(5) 1.469(4) 0.755(5) 0.10(2) Uiso 1 1 d D . .
H35B H -0.101(6) 1.382(7) 0.705(5) 0.14(3) Uiso 1 1 d D . .
H36B H 1.095(4) 0.565(4) 1.224(5) 0.082(18) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
La1 0.01012(7) 0.01128(7) 0.00520(8) -0.00292(6) 0.00140(5) -0.00528(6)
La2 0.00926(6) 0.01148(7) 0.00591(8) -0.00317(6) 0.00147(5) -0.00488(6)
O1 0.0198(11) 0.0182(11) 0.0127(12) -0.0021(10) 0.0018(9) -0.0107(9)
O2 0.0198(11) 0.0181(11) 0.0141(11) -0.0069(9) 0.0072(8) -0.0107(9)
O3 0.0163(8) 0.0233(9) 0.0084(8) -0.0020(7) 0.0024(6) -0.0077(7)
O4 0.0363(10) 0.0163(8) 0.0147(9) -0.0025(7) 0.0004(7) -0.0118(8)
O5 0.0385(13) 0.0379(15) 0.0165(13) -0.0167(12) 0.0008(11) 0.0012(12)
O6 0.0196(10) 0.0225(11) 0.0080(10) -0.0088(9) 0.0059(8) -0.0126(9)
O7 0.0402(12) 0.0216(11) 0.0105(11) -0.0060(9) 0.0066(9) -0.0218(10)
O8 0.0265(10) 0.0233(9) 0.0073(9) -0.0076(8) 0.0058(7) -0.0193(9)
O9 0.0087(8) 0.0216(10) 0.0109(10) -0.0084(8) 0.0034(7) -0.0059(8)
O10 0.0101(9) 0.0157(9) 0.0135(10) -0.0089(8) 0.0026(7) -0.0053(7)
O11 0.0149(10) 0.0189(11) 0.0092(11) -0.0019(9) -0.0018(8) -0.0082(9)
O12 0.0141(10) 0.0206(11) 0.0103(11) -0.0045(9) 0.0024(8) -0.0075(8)
O13 0.0173(10) 0.0213(10) 0.0056(9) -0.0018(7) 0.0026(7) -0.0053(8)
O14 0.0225(9) 0.0188(10) 0.0178(9) -0.0067(8) 0.0018(7) -0.0092(8)
O15 0.0303(10) 0.0452(12) 0.0406(12) -0.0265(11) 0.0112(9) -0.0205(9)
O16 0.0141(10) 0.0159(11) 0.0125(11) -0.0036(9) 0.0056(8) -0.0067(9)
O17 0.0116(9) 0.0224(12) 0.0097(11) -0.0022(10) -0.0004(8) -0.0094(9)
O18 0.0273(10) 0.0309(10) 0.0104(9) -0.0043(8) 0.0066(7) -0.0107(8)
O19 0.0208(8) 0.0188(8) 0.0143(9) -0.0035(7) 0.0026(7) -0.0058(7)
O20 0.0375(12) 0.0295(13) 0.0173(13) -0.0133(11) 0.0007(9) 0.0039(10)
O21 0.0201(11) 0.0206(11) 0.0149(12) -0.0101(9) 0.0035(8) -0.0105(9)
O22 0.0310(11) 0.0203(10) 0.0145(11) -0.0089(9) 0.0077(8) -0.0161(9)
O23 0.0456(13) 0.0318(11) 0.0100(10) -0.0104(9) 0.0092(9) -0.0280(11)
O24 0.0152(10) 0.0337(13) 0.0163(11) -0.0154(10) 0.0041(8) -0.0121(9)
O25 0.0142(10) 0.0187(10) 0.0237(12) -0.0126(9) 0.0062(8) -0.0084(8)
O26 0.0146(10) 0.0175(11) 0.0120(12) -0.0015(9) -0.0007(8) -0.0074(9)
O27 0.0186(10) 0.0153(10) 0.0076(11) -0.0034(9) 0.0054(8) -0.0071(8)
O28 0.0166(10) 0.0206(9) 0.0082(9) -0.0040(8) 0.0034(7) -0.0041(8)
O29 0.0521(14) 0.0222(11) 0.0177(10) -0.0028(9) -0.0084(9) -0.0206(10)
O30 0.0229(9) 0.0163(8) 0.0373(11) -0.0113(8) 0.0088(8) -0.0106(7)
O31 0.0177(11) 0.0136(12) 0.0125(13) -0.0048(10) 0.0035(9) -0.0056(10)
O32 0.0202(11) 0.0220(11) 0.0118(11) -0.0064(10) 0.0012(8) -0.0019(9)
O33 0.0165(10) 0.0151(11) 0.0094(12) -0.0052(10) 0.0052(8) -0.0079(9)
O34 0.0154(10) 0.0192(11) 0.0148(12) -0.0080(10) 0.0040(9) -0.0010(9)
O35 0.0280(12) 0.0318(14) 0.0272(14) -0.0032(11) 0.0014(10) -0.0108(11)
O36 0.0189(10) 0.0202(10) 0.0255(12) -0.0098(9) 0.0025(8) -0.0051(9)
O37 0.0212(9) 0.0218(10) 0.0411(12) -0.0131(9) -0.0019(8) -0.0052(8)
C1 0.0164(14) 0.0185(16) 0.0119(17) -0.0091(14) 0.0038(12) -0.0121(13)
C2 0.0200(14) 0.0167(15) 0.0132(17) -0.0082(13) 0.0071(12) -0.0129(12)
C3 0.0198(14) 0.0179(14) 0.0191(17) -0.0033(12) 0.0004(11) -0.0080(12)
C4 0.0120(12) 0.0196(13) 0.0127(14) -0.0044(12) 0.0046(10) -0.0073(11)
C5 0.0206(13) 0.0140(11) 0.0074(12) -0.0040(10) 0.0045(10) -0.0099(11)
C6 0.0140(12) 0.0174(12) 0.0148(13) -0.0051(10) 0.0011(10) -0.0057(11)
C7 0.0140(12) 0.0155(13) 0.0124(14) -0.0041(11) 0.0035(10) -0.0067(11)
C8 0.0154(10) 0.0253(12) 0.0136(12) -0.0069(10) 0.0054(9) -0.0101(10)
C9 0.0197(11) 0.0231(12) 0.0113(12) -0.0030(10) 0.0040(9) -0.0115(10)
C10 0.0236(13) 0.0254(13) 0.0190(14) -0.0119(11) 0.0022(11) -0.0065(11)
C11 0.0156(13) 0.0106(12) 0.0148(15) -0.0056(11) 0.0038(10) -0.0057(11)
C12 0.0157(13) 0.0108(12) 0.0061(13) -0.0043(11) 0.0048(10) -0.0044(10)
C13 0.0176(13) 0.0183(14) 0.0112(15) -0.0087(12) 0.0050(10) -0.0124(11)
C14 0.0193(13) 0.0196(14) 0.0106(14) -0.0073(11) 0.0034(10) -0.0137(11)
C15 0.0163(13) 0.0160(12) 0.0084(13) -0.0090(11) 0.0031(10) -0.0064(10)
C16 0.0207(14) 0.0202(13) 0.0126(14) -0.0082(11) 0.0079(10) -0.0138(12)
C17 0.0176(13) 0.0214(14) 0.0162(15) -0.0114(12) 0.0021(10) -0.0099(11)
C18 0.0148(11) 0.0189(11) 0.0081(11) -0.0076(9) 0.0046(9) -0.0095(10)
C19 0.014 0.009 0.001 -0.001 0.000 -0.004
C20 0.0114(10) 0.0140(11) 0.0079(11) -0.0043(9) 0.0033(8) -0.0083(9)
C21 0.0156(14) 0.0136(15) 0.0059(16) -0.0031(13) 0.0004(11) -0.0081(12)
C22 0.0178(13) 0.0126(14) 0.0036(14) -0.0027(12) 0.0046(11) -0.0107(12)
C23 0.0126(13) 0.0173(14) 0.0156(16) -0.0067(13) -0.0026(11) -0.0048(11)
C24 0.0155(13) 0.0177(13) 0.0082(14) -0.0050(11) 0.0063(10) -0.0091(11)
C25 0.0192(13) 0.0127(12) 0.0079(13) -0.0011(11) -0.0019(10) -0.0071(10)
C26 0.0133(12) 0.0166(13) 0.0113(13) -0.0054(11) 0.0015(10) -0.0064(10)
C27 0.0123(12) 0.0147(13) 0.0119(15) -0.0039(11) 0.0012(10) -0.0060(11)
C28 0.0158(13) 0.0171(13) 0.0137(13) -0.0035(11) 0.0027(10) -0.0065(11)
C29 0.0197(12) 0.0171(11) 0.0088(11) -0.0041(10) 0.0050(9) -0.0062(10)
C30 0.0288(13) 0.0211(12) 0.0227(14) -0.0115(11) 0.0122(10) -0.0115(11)
C31 0.0171(15) 0.0118(15) 0.0105(16) -0.0032(13) 0.0015(12) -0.0085(13)
C32 0.0165(14) 0.0122(14) 0.0111(16) -0.0021(13) -0.0009(11) -0.0077(11)
C33 0.0159(13) 0.0189(14) 0.0179(15) -0.0068(12) 0.0043(10) -0.0092(11)
C34 0.0201(14) 0.0176(12) 0.0116(13) 0.0001(10) -0.0019(11) -0.0086(12)
C35 0.0261(14) 0.0192(13) 0.0118(13) -0.0068(11) 0.0062(11) -0.0137(12)
C36 0.0153(13) 0.0224(14) 0.0152(14) -0.0073(12) 0.0027(10) -0.0095(11)
C37 0.0138(12) 0.0187(13) 0.0079(14) -0.0037(11) 0.0025(10) -0.0081(11)
C38 0.0287(13) 0.0236(12) 0.0148(12) -0.0076(11) 0.0062(10) -0.0115(11)
C39 0.0235(12) 0.0164(11) 0.0143(12) -0.0047(10) 0.0021(9) -0.0065(10)
C40 0.0240(14) 0.0393(17) 0.0217(15) -0.0177(14) 0.0028(11) -0.0049(13)
C41 0.0157(13) 0.0146(13) 0.0069(14) -0.0052(11) 0.0020(10) -0.0030(10)
C42 0.0126(12) 0.0125(13) 0.0147(15) -0.0067(11) -0.0004(10) -0.0029(10)
C43 0.0191(13) 0.0174(13) 0.0115(14) -0.0078(11) 0.0042(10) -0.0098(11)
C44 0.0280(16) 0.0237(15) 0.0216(16) -0.0150(13) 0.0105(12) -0.0179(13)
C45 0.0272(15) 0.0171(13) 0.0078(13) -0.0037(11) 0.0074(11) -0.0119(12)
C46 0.0185(13) 0.0223(14) 0.0134(14) -0.0110(12) 0.0018(10) -0.0092(11)
C47 0.0194(14) 0.0163(14) 0.0162(16) -0.0075(13) 0.0064(11) -0.0076(11)
C48 0.0346(16) 0.0273(14) 0.0132(13) -0.0098(11) 0.0059(12) -0.0178(14)
C49 0.0232(13) 0.0194(12) 0.0205(14) -0.0099(11) 0.0029(11) -0.0121(11)
C50 0.0302(13) 0.0260(13) 0.0279(15) -0.0163(12) 0.0092(11) -0.0166(11)
C51 0.0152(14) 0.0106(14) 0.0129(17) -0.0058(13) 0.0020(12) -0.0073(12)
C52 0.0112(13) 0.0123(14) 0.0141(16) -0.0055(13) -0.0025(11) -0.0045(11)
C53 0.0137(12) 0.0113(12) 0.0042(13) -0.0012(10) 0.0021(10) -0.0071(10)
C54 0.0151(13) 0.0194(14) 0.0151(15) -0.0082(12) 0.0030(10) -0.0088(11)
C55 0.0187(13) 0.0146(13) 0.0076(13) -0.0052(11) 0.0065(10) -0.0098(11)
C56 0.0152(13) 0.0145(13) 0.0105(14) -0.0008(11) -0.0023(10) -0.0032(11)
C57 0.0132(12) 0.0173(14) 0.0123(15) -0.0078(12) 0.0057(10) -0.0060(11)
C58 0.0185(13) 0.0168(13) 0.0094(12) -0.0044(10) 0.0061(10) -0.0082(11)
C59 0.0300(13) 0.0149(12) 0.0120(12) -0.0052(10) 0.0074(10) -0.0110(11)
C60 0.0220(11) 0.0158(11) 0.0185(12) -0.0053(10) 0.0068(9) -0.0094(9)

_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 O11 2.420(2) . ?
La1 O32 2.498(2) . ?
La1 O6 2.501(2) . ?
La1 O27 2.532(2) . ?
La1 O2 2.550(2) . ?
La1 O10 2.572(2) 1_556 ?
La1 O9 2.589(2) 1_556 ?
La1 O31 2.645(2) . ?
La1 O1 2.732(2) . ?
La1 C1 2.984(3) . ?
La2 O26 2.446(2) . ?
La2 O12 2.474(2) . ?
La2 O21 2.483(2) . ?
La2 O25 2.530(2) 1_554 ?
La2 O34 2.536(2) . ?
La2 O16 2.619(2) . ?
La2 O17 2.638(2) . ?
La2 O33 2.660(2) . ?
La2 O24 2.667(2) 1_554 ?
La2 C31 2.989(3) . ?
O1 C1 1.248(4) . ?
O2 C1 1.286(4) . ?
O3 C5 1.362(3) . ?
O3 C8 1.421(3) . ?
O4 C9 1.421(3) . ?
O4 H4O 0.849(19) . ?
O5 C10 1.430(4) . ?
O5 H5O 0.85(4) . ?
O6 C11 1.263(4) . ?
O7 C11 1.274(4) . ?
O8 C15 1.367(4) . ?
O8 C18 1.430(3) . ?
O9 C19 1.431(2) . ?
O9 La1 2.589(2) 1_554 ?
O9 H9O 0.843(18) . ?
O10 C20 1.429(3) . ?
O10 La1 2.572(2) 1_554 ?
O10 H10O 0.76(4) . ?
O11 C21 1.263(3) . ?
O12 C21 1.251(4) . ?
O13 C25 1.372(4) . ?
O13 C28 1.437(3) . ?
O14 C29 1.431(3) . ?
O14 H14O 0.75(3) . ?
O15 C30 1.387(3) . ?
O15 H15O 0.8400 . ?
O16 C31 1.250(4) . ?
O17 C31 1.281(4) . ?
O18 C35 1.365(3) . ?
O18 C38 1.428(3) . ?
O19 C39 1.425(3) . ?
O19 H19O 0.911(18) . ?
O20 C40 1.431(4) . ?
O20 H20O 0.90(4) . ?
O21 C41 1.263(4) . ?
O22 C41 1.259(4) . ?
O23 C45 1.375(4) . ?
O23 C48 1.424(3) . ?
O24 C49 1.431(4) . ?
O24 La2 2.667(2) 1_556 ?
O24 H24O 0.72(4) . ?
O25 C50 1.415(3) . ?
O25 La2 2.530(2) 1_556 ?
O25 H25O 0.87(3) . ?
O26 C51 1.267(4) . ?
O27 C51 1.266(4) . ?
O28 C55 1.375(4) . ?
O28 C58 1.430(3) . ?
O29 C59 1.415(3) . ?
O29 H29O 0.84(4) . ?
O30 C60 1.426(3) . ?
O30 H30O 0.8400 . ?
O31 H31A 0.76(4) . ?
O31 H31B 0.88(2) . ?
O32 H32A 0.79(4) . ?
O32 H32B 0.86(2) . ?
O33 H33A 0.89(3) . ?
O33 H33B 0.89(4) . ?
O34 H34A 1.00(5) . ?
O34 H34B 0.79(4) . ?
O35 H35A 0.89(2) . ?
O35 H35B 0.90(2) . ?
O36 H36A 0.94(4) . ?
O36 H36B 0.91(2) . ?
O37 H37A 0.890(19) . ?
O37 H37B 0.92(4) . ?
C1 C2 1.500(5) . ?
C2 C3 1.381(5) . ?
C2 C7 1.402(4) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(4) . ?
C6 C7 1.374(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.512(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.514(3) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.491(5) . ?
C12 C13 1.384(4) . ?
C12 C17 1.396(4) . ?
C13 C14 1.384(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(4) . ?
C16 C17 1.375(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.518(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.514(2) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.506(4) . ?
C22 C27 1.394(4) . ?
C22 C23 1.400(5) . ?
C23 C24 1.374(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(4) . ?
C26 C27 1.369(5) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.515(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.528(3) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.484(5) . ?
C32 C33 1.385(4) . ?
C32 C37 1.403(5) . ?
C33 C34 1.399(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(4) . ?
C36 C37 1.380(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.524(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.496(4) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.489(5) . ?
C42 C47 1.382(5) . ?
C42 C43 1.405(4) . ?
C43 C44 1.378(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.386(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.390(4) . ?
C46 C47 1.391(5) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.562(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.491(4) . ?
C49 H49 1.0000 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.483(5) . ?
C52 C53 1.384(5) . ?
C52 C57 1.402(4) . ?
C53 C54 1.392(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.381(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.390(4) . ?
C56 C57 1.391(5) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C59 1.512(3) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.508(3) . ?
C59 H59 1.0000 . ?
C60 H60A 0.9900 . ?
C60 H60B 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
O11 La1 O32 149.75(8) . . ?
O11 La1 O6 82.05(8) . . ?
O32 La1 O6 78.19(8) . . ?
O11 La1 O27 104.01(7) . . ?
O32 La1 O27 74.05(8) . . ?
O6 La1 O27 132.31(8) . . ?
O11 La1 O2 73.27(8) . . ?
O32 La1 O2 123.61(8) . . ?
O6 La1 O2 77.94(7) . . ?
O27 La1 O2 149.57(7) . . ?
O11 La1 O10 137.58(7) . 1_556 ?
O32 La1 O10 71.60(8) . 1_556 ?
O6 La1 O10 132.51(7) . 1_556 ?
O27 La1 O10 72.40(7) . 1_556 ?
O2 La1 O10 89.17(7) . 1_556 ?
O11 La1 O9 77.05(7) . 1_556 ?
O32 La1 O9 130.29(8) . 1_556 ?
O6 La1 O9 146.12(7) . 1_556 ?
O27 La1 O9 79.12(7) . 1_556 ?
O2 La1 O9 70.69(7) . 1_556 ?
O10 La1 O9 60.63(6) 1_556 1_556 ?
O11 La1 O31 72.96(8) . . ?
O32 La1 O31 78.94(8) . . ?
O6 La1 O31 70.51(8) . . ?
O27 La1 O31 66.66(8) . . ?
O2 La1 O31 136.21(8) . . ?
O10 La1 O31 134.60(7) 1_556 . ?
O9 La1 O31 126.28(7) 1_556 . ?
O11 La1 O1 118.37(7) . . ?
O32 La1 O1 74.67(8) . . ?
O6 La1 O1 68.11(7) . . ?
O27 La1 O1 136.18(7) . . ?
O2 La1 O1 49.05(7) . . ?
O10 La1 O1 69.07(7) 1_556 . ?
O9 La1 O1 99.03(7) 1_556 . ?
O31 La1 O1 134.38(8) . . ?
O11 La1 C1 94.19(8) . . ?
O32 La1 C1 98.45(9) . . ?
O6 La1 C1 66.21(8) . . ?
O27 La1 C1 155.20(8) . . ?
O2 La1 C1 25.35(8) . . ?
O10 La1 C1 82.80(8) 1_556 . ?
O9 La1 C1 88.90(8) 1_556 . ?
O31 La1 C1 136.17(8) . . ?
O1 La1 C1 24.73(7) . . ?
O26 La2 O12 101.87(7) . . ?
O26 La2 O21 84.64(8) . . ?
O12 La2 O21 132.04(8) . . ?
O26 La2 O25 71.38(7) . 1_554 ?
O12 La2 O25 79.28(8) . 1_554 ?
O21 La2 O25 144.81(8) . 1_554 ?
O26 La2 O34 147.17(8) . . ?
O12 La2 O34 71.89(8) . . ?
O21 La2 O34 77.53(8) . . ?
O25 La2 O34 135.19(8) 1_554 . ?
O26 La2 O16 73.98(7) . . ?
O12 La2 O16 149.60(8) . . ?
O21 La2 O16 78.15(8) . . ?
O25 La2 O16 70.82(7) 1_554 . ?
O34 La2 O16 127.41(8) . . ?
O26 La2 O17 120.59(7) . . ?
O12 La2 O17 135.30(7) . . ?
O21 La2 O17 69.74(8) . . ?
O25 La2 O17 100.37(8) 1_554 . ?
O34 La2 O17 78.63(8) . . ?
O16 La2 O17 49.25(6) . . ?
O26 La2 O33 69.01(7) . . ?
O12 La2 O33 69.43(8) . . ?
O21 La2 O33 69.06(8) . . ?
O25 La2 O33 121.84(7) 1_554 . ?
O34 La2 O33 78.88(8) . . ?
O16 La2 O33 131.96(7) . . ?
O17 La2 O33 136.28(7) . . ?
O26 La2 O24 131.40(7) . 1_554 ?
O12 La2 O24 72.34(7) . 1_554 ?
O21 La2 O24 135.79(7) . 1_554 ?
O25 La2 O24 60.07(7) 1_554 1_554 ?
O34 La2 O24 78.61(8) . 1_554 ?
O16 La2 O24 87.78(7) . 1_554 ?
O17 La2 O24 69.41(7) . 1_554 ?
O33 La2 O24 140.01(8) . 1_554 ?
O26 La2 C31 95.62(8) . . ?
O12 La2 C31 154.12(8) . . ?
O21 La2 C31 68.08(9) . . ?
O25 La2 C31 88.57(8) 1_554 . ?
O34 La2 C31 102.78(9) . . ?
O16 La2 C31 24.63(8) . . ?
O17 La2 C31 25.35(7) . . ?
O33 La2 C31 135.52(8) . . ?
O24 La2 C31 81.80(8) 1_554 . ?
C1 O1 La1 89.03(19) . . ?
C1 O2 La1 96.5(2) . . ?
C5 O3 C8 118.23(19) . . ?
C9 O4 H4O 108(3) . . ?
C10 O5 H5O 105(3) . . ?
C11 O6 La1 138.9(2) . . ?
C15 O8 C18 116.5(2) . . ?
C19 O9 La1 123.57(11) . 1_554 ?
C19 O9 H9O 109(2) . . ?
La1 O9 H9O 118(2) 1_554 . ?
C20 O10 La1 116.15(14) . 1_554 ?
C20 O10 H10O 108(3) . . ?
La1 O10 H10O 125(3) 1_554 . ?
C21 O11 La1 169.2(2) . . ?
C21 O12 La2 124.9(2) . . ?
C25 O13 C28 118.8(2) . . ?
C29 O14 H14O 103(2) . . ?
C30 O15 H15O 109.5 . . ?
C31 O16 La2 94.48(19) . . ?
C31 O17 La2 92.83(18) . . ?
C35 O18 C38 121.7(2) . . ?
C39 O19 H19O 105(2) . . ?
C40 O20 H20O 107(3) . . ?
C41 O21 La2 142.9(2) . . ?
C45 O23 C48 117.5(2) . . ?
C49 O24 La2 120.20(16) . 1_556 ?
C49 O24 H24O 120(3) . . ?
La2 O24 H24O 119(3) 1_556 . ?
C50 O25 La2 118.77(16) . 1_556 ?
C50 O25 H25O 112(2) . . ?
La2 O25 H25O 128(2) 1_556 . ?
C51 O26 La2 159.3(2) . . ?
C51 O27 La1 120.9(2) . . ?
C55 O28 C58 116.7(2) . . ?
C59 O29 H29O 112(2) . . ?
C60 O30 H30O 109.5 . . ?
La1 O31 H31A 110(3) . . ?
La1 O31 H31B 101(5) . . ?
H31A O31 H31B 104(5) . . ?
La1 O32 H32A 121(2) . . ?
La1 O32 H32B 116(4) . . ?
H32A O32 H32B 116(4) . . ?
La2 O33 H33A 102(2) . . ?
La2 O33 H33B 128(2) . . ?
H33A O33 H33B 103(3) . . ?
La2 O34 H34A 116(3) . . ?
La2 O34 H34B 128(2) . . ?
H34A O34 H34B 111(4) . . ?
H35A O35 H35B 110(6) . . ?
H36A O36 H36B 124(4) . . ?
H37A O37 H37B 97(4) . . ?
O1 C1 O2 120.4(3) . . ?
O1 C1 C2 121.4(3) . . ?
O2 C1 C2 118.1(3) . . ?
O1 C1 La1 66.24(18) . . ?
O2 C1 La1 58.12(17) . . ?
C2 C1 La1 156.1(2) . . ?
C3 C2 C7 119.1(3) . . ?
C3 C2 C1 121.0(3) . . ?
C7 C2 C1 119.4(3) . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
O3 C5 C4 124.1(2) . . ?
O3 C5 C6 115.4(2) . . ?
C4 C5 C6 120.5(3) . . ?
C7 C6 C5 120.3(3) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C2 120.0(3) . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
O3 C8 C9 108.19(18) . . ?
O3 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
O3 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O4 C9 C8 110.7(2) . . ?
O4 C9 C10 109.23(19) . . ?
C8 C9 C10 112.2(2) . . ?
O4 C9 H9 108.2 . . ?
C8 C9 H9 108.2 . . ?
C10 C9 H9 108.2 . . ?
O5 C10 C9 111.5(2) . . ?
O5 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
O5 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
O6 C11 O7 123.1(3) . . ?
O6 C11 C12 118.5(3) . . ?
O7 C11 C12 118.3(3) . . ?
C13 C12 C17 118.3(3) . . ?
C13 C12 C11 119.9(3) . . ?
C17 C12 C11 121.8(3) . . ?
C12 C13 C14 122.0(3) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
O8 C15 C14 123.8(2) . . ?
O8 C15 C16 116.1(3) . . ?
C14 C15 C16 120.1(3) . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C12 121.0(3) . . ?
C16 C17 H17 119.5 . . ?
C12 C17 H17 119.5 . . ?
O8 C18 C19 106.09(17) . . ?
O8 C18 H18A 110.5 . . ?
C19 C18 H18A 110.5 . . ?
O8 C18 H18B 110.5 . . ?
C19 C18 H18B 110.5 . . ?
H18A C18 H18B 108.7 . . ?
O9 C19 C20 105.62(12) . . ?
O9 C19 C18 108.56(13) . . ?
C20 C19 C18 114.85(13) . . ?
O9 C19 H19 109.2 . . ?
C20 C19 H19 109.2 . . ?
C18 C19 H19 109.2 . . ?
O10 C20 C19 106.87(16) . . ?
O10 C20 H20A 110.3 . . ?
C19 C20 H20A 110.3 . . ?
O10 C20 H20B 110.3 . . ?
C19 C20 H20B 110.3 . . ?
H20A C20 H20B 108.6 . . ?
O12 C21 O11 123.9(3) . . ?
O12 C21 C22 116.9(3) . . ?
O11 C21 C22 119.1(3) . . ?
C27 C22 C23 118.3(3) . . ?
C27 C22 C21 120.2(3) . . ?
C23 C22 C21 121.5(3) . . ?
C24 C23 C22 121.6(3) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 118.7(3) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
O13 C25 C26 115.6(3) . . ?
O13 C25 C24 124.0(3) . . ?
C26 C25 C24 120.4(3) . . ?
C27 C26 C25 120.1(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C22 120.7(3) . . ?
C26 C27 H27 119.6 . . ?
C22 C27 H27 119.6 . . ?
O13 C28 C29 105.5(2) . . ?
O13 C28 H28A 110.6 . . ?
C29 C28 H28A 110.6 . . ?
O13 C28 H28B 110.6 . . ?
C29 C28 H28B 110.6 . . ?
H28A C28 H28B 108.8 . . ?
O14 C29 C28 111.5(2) . . ?
O14 C29 C30 107.15(19) . . ?
C28 C29 C30 113.2(2) . . ?
O14 C29 H29 108.3 . . ?
C28 C29 H29 108.3 . . ?
C30 C29 H29 108.3 . . ?
O15 C30 C29 116.1(2) . . ?
O15 C30 H30A 108.3 . . ?
C29 C30 H30A 108.3 . . ?
O15 C30 H30B 108.3 . . ?
C29 C30 H30B 108.3 . . ?
H30A C30 H30B 107.4 . . ?
O16 C31 O17 119.9(3) . . ?
O16 C31 C32 120.4(3) . . ?
O17 C31 C32 119.5(3) . . ?
O16 C31 La2 60.89(17) . . ?
O17 C31 La2 61.82(17) . . ?
C32 C31 La2 158.3(2) . . ?
C33 C32 C37 117.6(3) . . ?
C33 C32 C31 120.5(3) . . ?
C37 C32 C31 121.7(3) . . ?
C32 C33 C34 121.5(3) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C35 C34 C33 119.3(3) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
O18 C35 C36 114.0(3) . . ?
O18 C35 C34 126.0(3) . . ?
C36 C35 C34 120.1(3) . . ?
C35 C36 C37 120.1(3) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C36 C37 C32 121.3(3) . . ?
C36 C37 H37 119.3 . . ?
C32 C37 H37 119.3 . . ?
O18 C38 C39 111.1(2) . . ?
O18 C38 H38A 109.4 . . ?
C39 C38 H38A 109.4 . . ?
O18 C38 H38B 109.4 . . ?
C39 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
O19 C39 C40 107.9(2) . . ?
O19 C39 C38 107.09(19) . . ?
C40 C39 C38 112.8(2) . . ?
O19 C39 H39 109.7 . . ?
C40 C39 H39 109.7 . . ?
C38 C39 H39 109.7 . . ?
O20 C40 C39 110.5(2) . . ?
O20 C40 H40A 109.5 . . ?
C39 C40 H40A 109.5 . . ?
O20 C40 H40B 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
O22 C41 O21 123.8(3) . . ?
O22 C41 C42 118.8(3) . . ?
O21 C41 C42 117.3(3) . . ?
C47 C42 C43 118.2(3) . . ?
C47 C42 C41 120.7(3) . . ?
C43 C42 C41 121.1(3) . . ?
C44 C43 C42 121.1(3) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C43 C44 C45 119.7(3) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
O23 C45 C44 115.5(3) . . ?
O23 C45 C46 124.1(3) . . ?
C44 C45 C46 120.5(3) . . ?
C45 C46 C47 119.0(3) . . ?
C45 C46 H46 120.5 . . ?
C47 C46 H46 120.5 . . ?
C42 C47 C46 121.5(3) . . ?
C42 C47 H47 119.2 . . ?
C46 C47 H47 119.2 . . ?
O23 C48 C49 106.9(2) . . ?
O23 C48 H48A 110.3 . . ?
C49 C48 H48A 110.3 . . ?
O23 C48 H48B 110.3 . . ?
C49 C48 H48B 110.3 . . ?
H48A C48 H48B 108.6 . . ?
O24 C49 C50 107.3(2) . . ?
O24 C49 C48 110.4(2) . . ?
C50 C49 C48 109.8(2) . . ?
O24 C49 H49 109.8 . . ?
C50 C49 H49 109.8 . . ?
C48 C49 H49 109.8 . . ?
O25 C50 C49 106.5(2) . . ?
O25 C50 H50A 110.4 . . ?
C49 C50 H50A 110.4 . . ?
O25 C50 H50B 110.4 . . ?
C49 C50 H50B 110.4 . . ?
H50A C50 H50B 108.6 . . ?
O27 C51 O26 122.3(3) . . ?
O27 C51 C52 118.7(3) . . ?
O26 C51 C52 119.0(3) . . ?
C53 C52 C57 118.5(3) . . ?
C53 C52 C51 120.8(3) . . ?
C57 C52 C51 120.6(3) . . ?
C52 C53 C54 121.5(3) . . ?
C52 C53 H53 119.2 . . ?
C54 C53 H53 119.2 . . ?
C55 C54 C53 119.1(3) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
O28 C55 C54 123.4(3) . . ?
O28 C55 C56 115.7(3) . . ?
C54 C55 C56 120.9(3) . . ?
C55 C56 C57 119.3(3) . . ?
C55 C56 H56 120.3 . . ?
C57 C56 H56 120.3 . . ?
C56 C57 C52 120.7(3) . . ?
C56 C57 H57 119.7 . . ?
C52 C57 H57 119.7 . . ?
O28 C58 C59 108.5(2) . . ?
O28 C58 H58A 110.0 . . ?
C59 C58 H58A 110.0 . . ?
O28 C58 H58B 110.0 . . ?
C59 C58 H58B 110.0 . . ?
H58A C58 H58B 108.4 . . ?
O29 C59 C60 105.0(2) . . ?
O29 C59 C58 112.9(2) . . ?
C60 C59 C58 113.9(2) . . ?
O29 C59 H59 108.3 . . ?
C60 C59 H59 108.3 . . ?
C58 C59 H59 108.3 . . ?
O30 C60 C59 110.3(2) . . ?
O30 C60 H60A 109.6 . . ?
C59 C60 H60A 109.6 . . ?
O30 C60 H60B 109.6 . . ?
C59 C60 H60B 109.6 . . ?
H60A C60 H60B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.058