# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Pierre Thuery'

_publ_contact_author_name        'Pierre Thuery'
_publ_contact_author_email       PIERRE.THUERY@CEA.FR

_publ_section_title              
;
Templating effects in uranyl-organic frameworks with
cyclohexane-1,3-dicarboxylate ligands
;

# Attachment 'CIF.txt'

data_1
_database_code_depnum_ccdc_archive 'CCDC 701168'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 O7 U'
_chemical_formula_weight         458.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   10.6261(6)
_cell_length_b                   10.3755(4)
_cell_length_c                   10.9553(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.786(3)
_cell_angle_gamma                90.00
_cell_volume                     1105.24(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31301
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_absorpt_coefficient_mu    14.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.338
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and five ω scans with 2° steps (399 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31301
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.68
_reflns_number_total             2095
_reflns_number_gt                1628
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. The cyclohexane ring is disordered over two positions
sharing atom C2, which have been refined with occupancy parameters
constrained to sum to unity. All non-hydrogen atoms were refined with
anisotropic displacement parameters, with restraints (bond lengths and
displacement parameters) for some atoms of the disordered parts. The H
atoms bound to O7 were found on a Fourier-difference map and all the
others were introduced at calculated positions. All were treated as
riding atoms with an isotropic displacement parameter equal to 1.2
times that of the parent atom.
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0609P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2095
_refine_ls_number_parameters     192
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.350
_refine_diff_density_min         -1.966
_refine_diff_density_rms         0.204

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
U U 0.92472(4) 0.62709(3) 0.17528(3) 0.03655(19) Uani 1 1 d . . .
O1 O 0.9309(7) 0.5494(6) 0.3188(6) 0.0452(16) Uani 1 1 d . . .
O2 O 0.9232(7) 0.7004(6) 0.0303(6) 0.0442(16) Uani 1 1 d . . .
O3 O 0.7761(7) 0.7993(6) 0.1982(6) 0.0450(16) Uani 1 1 d . A .
O4 O 0.6750(7) 0.6276(6) 0.0859(7) 0.0475(16) Uani 1 1 d . A .
O5 O 0.1563(6) 0.5632(5) -0.0431(6) 0.0356(14) Uani 1 1 d . . .
O6 O 0.0784(7) 0.7184(7) -0.1918(6) 0.0453(17) Uani 1 1 d . . .
O7 O 1.1351(6) 0.5266(6) 0.1927(6) 0.0377(14) Uani 1 1 d . . .
H7A H 1.1718 0.4464 0.2289 0.045 Uiso 1 1 d R . .
H7B H 1.1913 0.5617 0.1682 0.045 Uiso 1 1 d R . .
C2 C 0.4133(12) 0.7042(10) 0.0305(12) 0.059(3) Uani 1 1 d D . .
H2A H 0.4221 0.6395 0.0965 0.070 Uiso 0.56(2) 1 d PR A .
H2B H 0.4201 0.6626 -0.0451 0.070 Uiso 0.56(2) 1 d PR . .
H2C H 0.4261 0.6123 0.0401 0.070 Uiso 0.44(2) 1 d PR . .
H2D H 0.4133 0.7308 -0.0536 0.070 Uiso 0.44(2) 1 d PR . .
C1A C 0.5288(18) 0.8037(16) 0.0872(18) 0.035(4) Uani 0.56(2) 1 d P A 1
H1A H 0.5209 0.8728 0.0235 0.042 Uiso 0.56(2) 1 calc PR A 1
C3A C 0.2739(18) 0.7748(18) -0.017(2) 0.038(5) Uani 0.56(2) 1 d P A 1
H3A H 0.2695 0.8461 -0.0775 0.045 Uiso 0.56(2) 1 calc PR A 1
C4A C 0.262(2) 0.823(2) 0.110(2) 0.051(6) Uani 0.56(2) 1 d P A 1
H4A1 H 0.1764 0.8693 0.0872 0.061 Uiso 0.56(2) 1 calc PR A 1
H4A2 H 0.2626 0.7503 0.1659 0.061 Uiso 0.56(2) 1 calc PR A 1
C5A C 0.383(3) 0.912(3) 0.186(3) 0.067(8) Uani 0.56(2) 1 d PU A 1
H5A1 H 0.3753 0.9897 0.1341 0.080 Uiso 0.56(2) 1 calc PR A 1
H5A2 H 0.3782 0.9378 0.2695 0.080 Uiso 0.56(2) 1 calc PR A 1
C6A C 0.5153(18) 0.8551(19) 0.2160(19) 0.041(5) Uani 0.56(2) 1 d P A 1
H6A1 H 0.5291 0.7844 0.2780 0.050 Uiso 0.56(2) 1 calc PR A 1
H6A2 H 0.5866 0.9186 0.2588 0.050 Uiso 0.56(2) 1 calc PR A 1
C1B C 0.5308(13) 0.771(3) 0.145(2) 0.058(8) Uani 0.44(2) 1 d PDU A 2
H1B H 0.5345 0.7319 0.2278 0.069 Uiso 0.44(2) 1 calc PR A 2
C3B C 0.2761(13) 0.749(3) 0.031(3) 0.060(10) Uani 0.44(2) 1 d PDU A 2
H3B H 0.2729 0.7184 0.1139 0.072 Uiso 0.44(2) 1 calc PR A 2
C4B C 0.261(2) 0.896(2) 0.029(2) 0.043(7) Uani 0.44(2) 1 d P A 2
H4B1 H 0.2625 0.9309 -0.0529 0.051 Uiso 0.44(2) 1 calc PR A 2
H4B2 H 0.1737 0.9192 0.0318 0.051 Uiso 0.44(2) 1 calc PR A 2
C5B C 0.378(3) 0.954(3) 0.148(3) 0.039(6) Uani 0.44(2) 1 d PU A 2
H5B1 H 0.3702 1.0467 0.1435 0.047 Uiso 0.44(2) 1 calc PR A 2
H5B2 H 0.3687 0.9261 0.2288 0.047 Uiso 0.44(2) 1 calc PR A 2
C6B C 0.515(3) 0.917(3) 0.158(3) 0.058(8) Uani 0.44(2) 1 d PU A 2
H6B1 H 0.5835 0.9461 0.2427 0.070 Uiso 0.44(2) 1 calc PR A 2
H6B2 H 0.5327 0.9608 0.0878 0.070 Uiso 0.44(2) 1 calc PR A 2
C7 C 0.6652(10) 0.7352(9) 0.1336(10) 0.049(3) Uani 1 1 d D . .
C8 C 0.1624(11) 0.6784(9) -0.0834(10) 0.042(2) Uani 1 1 d 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
U O1 1.744(6) . ?
U O2 1.755(6) . ?
U O6 2.332(6) 4_676 ?
U O5 2.394(6) 3_665 ?
U O7 2.404(6) . ?
U O4 2.429(7) . ?
U O3 2.464(6) . ?
O3 C7 1.288(11) . ?
O4 C7 1.254(10) . ?
O5 C8 1.284(11) . ?
O5 U 2.394(6) 3_665 ?
O6 C8 1.235(11) . ?
O6 U 2.332(6) 4_475 ?
O7 H7A 0.9358 . ?
O7 H7B 0.8304 . ?
C2 C1A 1.53(2) . ?
C2 C1B 1.531(10) . ?
C2 C3B 1.532(10) . ?
C2 C3A 1.54(2) . ?
C2 H2A 0.9624 . ?
C2 H2B 0.9621 . ?
C2 H2C 0.9624 . ?
C2 H2D 0.9621 . ?
C1A C7 1.51(2) . ?
C1A C6A 1.57(2) . ?
C1A H1A 0.9800 . ?
C3A C8 1.495(19) . ?
C3A C4A 1.54(3) . ?
C3A H3A 0.9800 . ?
C4A C5A 1.53(3) . ?
C4A H4A1 0.9700 . ?
C4A H4A2 0.9700 . ?
C5A C6A 1.43(4) . ?
C5A H5A1 0.9700 . ?
C5A H5A2 0.9700 . ?
C6A H6A1 0.9700 . ?
C6A H6A2 0.9700 . ?
C1B C7 1.527(10) . ?
C1B C6B 1.54(4) . ?
C1B H1B 0.9800 . ?
C3B C8 1.529(10) . ?
C3B C4B 1.54(4) . ?
C3B H3B 0.9800 . ?
C4B C5B 1.52(3) . ?
C4B H4B1 0.9700 . ?
C4B H4B2 0.9700 . ?
C5B C6B 1.47(4) . ?
C5B H5B1 0.9700 . ?
C5B H5B2 0.9700 . ?
C6B H6B1 0.9700 . ?
C6B H6B2 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
O1 U O2 177.6(3) . . ?
O1 U O6 89.6(3) . 4_676 ?
O2 U O6 90.9(3) . 4_676 ?
O1 U O5 92.2(2) . 3_665 ?
O2 U O5 86.6(3) . 3_665 ?
O6 U O5 159.2(2) 4_676 3_665 ?
O1 U O7 91.9(3) . . ?
O2 U O7 85.9(3) . . ?
O6 U O7 81.6(2) 4_676 . ?
O5 U O7 77.6(2) 3_665 . ?
O1 U O4 90.1(3) . . ?
O2 U O4 91.4(3) . . ?
O6 U O4 128.7(2) 4_676 . ?
O5 U O4 72.0(2) 3_665 . ?
O7 U O4 149.6(2) . . ?
O1 U O3 92.1(3) . . ?
O2 U O3 90.3(3) . . ?
O6 U O3 75.8(2) 4_676 . ?
O5 U O3 124.8(2) 3_665 . ?
O7 U O3 157.0(2) . . ?
O4 U O3 53.0(2) . . ?
C7 O3 U 93.0(5) . . ?
C7 O4 U 95.5(6) . . ?
C8 O5 U 128.0(5) . 3_665 ?
C8 O6 U 152.2(6) . 4_475 ?
U O7 H7A 129.3 . . ?
U O7 H7B 123.4 . . ?
H7A O7 H7B 107.3 . . ?
C1B C2 C3B 109.0(9) . . ?
C1A C2 C3A 108.7(11) . . ?
C1A C2 H2A 110.3 . . ?
C3A C2 H2A 112.0 . . ?
C1A C2 H2B 109.0 . . ?
C3A C2 H2B 108.3 . . ?
H2A C2 H2B 108.4 . . ?
C1B C2 H2C 109.0 . . ?
C3B C2 H2C 113.2 . . ?
C1B C2 H2D 109.9 . . ?
C3B C2 H2D 106.3 . . ?
H2C C2 H2D 109.5 . . ?
C7 C1A C2 108.8(12) . . ?
C7 C1A C6A 106.4(14) . . ?
C2 C1A C6A 104.2(14) . . ?
C7 C1A H1A 112.3 . . ?
C2 C1A H1A 112.3 . . ?
C6A C1A H1A 112.3 . . ?
C8 C3A C4A 108.6(15) . . ?
C8 C3A C2 108.2(12) . . ?
C4A C3A C2 105.3(15) . . ?
C8 C3A H3A 111.5 . . ?
C4A C3A H3A 111.5 . . ?
C2 C3A H3A 111.5 . . ?
C5A C4A C3A 109.6(17) . . ?
C5A C4A H4A1 109.8 . . ?
C3A C4A H4A1 109.8 . . ?
C5A C4A H4A2 109.8 . . ?
C3A C4A H4A2 109.8 . . ?
H4A1 C4A H4A2 108.2 . . ?
C6A C5A C4A 114(2) . . ?
C6A C5A H5A1 108.8 . . ?
C4A C5A H5A1 108.8 . . ?
C6A C5A H5A2 108.8 . . ?
C4A C5A H5A2 108.8 . . ?
H5A1 C5A H5A2 107.7 . . ?
C5A C6A C1A 111.9(17) . . ?
C5A C6A H6A1 109.2 . . ?
C1A C6A H6A1 109.2 . . ?
C5A C6A H6A2 109.2 . . ?
C1A C6A H6A2 109.2 . . ?
H6A1 C6A H6A2 107.9 . . ?
C7 C1B C2 107.7(11) . . ?
C7 C1B C6B 113(2) . . ?
C2 C1B C6B 116(2) . . ?
C7 C1B H1B 106.7 . . ?
C2 C1B H1B 106.7 . . ?
C6B C1B H1B 106.7 . . ?
C8 C3B C2 107.0(12) . . ?
C8 C3B C4B 115(2) . . ?
C2 C3B C4B 113.4(19) . . ?
C8 C3B H3B 107.0 . . ?
C2 C3B H3B 107.0 . . ?
C4B C3B H3B 107.0 . . ?
C5B C4B C3B 109(2) . . ?
C5B C4B H4B1 109.8 . . ?
C3B C4B H4B1 109.8 . . ?
C5B C4B H4B2 109.8 . . ?
C3B C4B H4B2 109.8 . . ?
H4B1 C4B H4B2 108.2 . . ?
C6B C5B C4B 114(2) . . ?
C6B C5B H5B1 108.8 . . ?
C4B C5B H5B1 108.8 . . ?
C6B C5B H5B2 108.8 . . ?
C4B C5B H5B2 108.8 . . ?
H5B1 C5B H5B2 107.7 . . ?
C5B C6B C1B 113(2) . . ?
C5B C6B H6B1 109.0 . . ?
C1B C6B H6B1 109.0 . . ?
C5B C6B H6B2 109.0 . . ?
C1B C6B H6B2 109.0 . . ?
H6B1 C6B H6B2 107.8 . . ?
O4 C7 O3 118.5(9) . . ?
O4 C7 C1A 120.7(10) . . ?
O3 C7 C1A 118.9(10) . . ?
O4 C7 C1B 119.1(12) . . ?
O3 C7 C1B 120.6(10) . . ?
O6 C8 O5 121.7(8) . . ?
O6 C8 C3A 111.4(11) . . ?
O5 C8 C3A 126.6(11) . . ?
O6 C8 C3B 130.6(15) . . ?
O5 C8 C3B 107.4(15) . . ?

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
O7 H7A O3 0.94 1.71 2.640(9) 173.3 2_745
O7 H7B O5 0.83 2.19 2.708(8) 120.4 1_655

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 701169'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H48 O21 U2'
_chemical_formula_weight         1172.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   9.9445(3)
_cell_length_b                   22.9894(9)
_cell_length_c                   15.6684(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.096(3)
_cell_angle_gamma                90.00
_cell_volume                     3576.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    118808
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_absorpt_coefficient_mu    9.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and seven ω scans with 2° steps (362 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            118808
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.68
_reflns_number_total             6764
_reflns_number_gt                5772
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters, with some restraints on bond lengths in one
dicarboxylic ligand and in the crown ether moiety. The H atoms bound
to O atoms were found on a Fourier-difference map and all the others
were introduced at calculated positions. All were treated as riding
atoms with an isotropic displacement parameter equal to 1.2 times that
of the parent atom.
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0464P)²+25.9292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6764
_refine_ls_number_parameters     442
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.944
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.192

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
U1 U 0.77130(3) 0.838950(13) 0.362933(19) 0.03083(10) Uani 1 1 d . . .
U2 U 0.37599(3) 0.587056(12) 0.386878(18) 0.02553(9) Uani 1 1 d . . .
O1 O 0.7766(6) 0.8693(3) 0.4661(4) 0.0403(14) Uani 1 1 d . . .
O2 O 0.7663(6) 0.8096(3) 0.2589(4) 0.0418(14) Uani 1 1 d . . .
O3 O 0.5259(5) 0.5844(2) 0.3330(4) 0.0319(12) Uani 1 1 d . . .
O4 O 0.2247(6) 0.5942(2) 0.4386(4) 0.0345(13) Uani 1 1 d . . .
O5 O 0.6319(6) 0.9198(2) 0.3063(4) 0.0400(14) Uani 1 1 d . . .
O6 O 0.5253(5) 0.8460(2) 0.3587(4) 0.0369(13) Uani 1 1 d . . .
O7 O 0.0201(6) 0.8461(3) 0.3620(4) 0.0427(15) Uani 1 1 d . . .
O8 O -0.0974(6) 0.9209(3) 0.3144(5) 0.058(2) Uani 1 1 d . . .
O9 O 0.6625(5) 0.7481(2) 0.4098(4) 0.0390(14) Uani 1 1 d . . .
O10 O 0.8840(6) 0.7505(3) 0.4177(4) 0.0410(14) Uani 1 1 d . . .
O11 O 0.5095(6) 0.5868(2) 0.5141(4) 0.0354(13) Uani 1 1 d . . .
O12 O 0.6066(6) 0.5108(2) 0.5766(4) 0.0370(13) Uani 1 1 d . . .
O13 O 0.4162(5) 0.6899(2) 0.4199(4) 0.0331(12) Uani 1 1 d . . .
H13A H 0.4873 0.7132 0.4161 0.040 Uiso 1 1 d R . .
H13B H 0.3451 0.7197 0.4165 0.040 Uiso 1 1 d R . .
O14 O 0.2856(5) 0.6430(2) 0.2685(3) 0.0332(12) Uani 1 1 d . . .
H14A H 0.3430 0.6586 0.2354 0.040 Uiso 1 1 d R . .
H14B H 0.2077 0.6430 0.2465 0.040 Uiso 1 1 d R . .
O15 O 0.2639(6) 0.5256(2) 0.2736(4) 0.0390(14) Uani 1 1 d . . .
H15A H 0.2191 0.5404 0.2346 0.047 Uiso 1 1 d R . .
H15B H 0.2900 0.4891 0.2635 0.047 Uiso 1 1 d R . .
O16 O 0.4727(8) 0.6912(4) 0.1719(5) 0.079(2) Uani 1 1 d . . .
O17 O 0.3513(11) 0.6026(4) 0.0665(6) 0.062(2) Uani 1 1 d . . .
O18 O 0.1146(10) 0.5654(4) 0.1341(6) 0.085(3) Uani 1 1 d . . .
O19 O 0.0331(9) 0.6717(5) 0.2077(6) 0.090(3) Uani 1 1 d . . .
O20 O 0.2201(17) 0.7570(6) 0.1900(9) 0.057(4) Uani 1 1 d . . .
O21 O 0.1862(7) 0.7521(3) 0.4233(5) 0.0584(19) Uani 1 1 d . . .
H21A H 0.1776 0.7891 0.4066 0.070 Uiso 1 1 d R . .
H21B H 0.0928 0.7419 0.4324 0.070 Uiso 1 1 d R . .
C1 C 0.3945(10) 0.9271(5) 0.3073(8) 0.063(3) Uani 1 1 d D . .
H1 H 0.3993 0.9594 0.3482 0.076 Uiso 1 1 calc R . .
C2 C 0.2704(8) 0.8939(4) 0.3290(7) 0.047(2) Uani 1 1 d . . .
H2A H 0.2788 0.8823 0.3886 0.057 Uiso 1 1 calc R . .
H2B H 0.2639 0.8588 0.2946 0.057 Uiso 1 1 calc R . .
C3 C 0.1421(11) 0.9293(6) 0.3137(8) 0.072(3) Uani 1 1 d D . .
H3 H 0.1478 0.9599 0.3573 0.087 Uiso 1 1 calc R . .
C4 C 0.1343(14) 0.9607(7) 0.2311(9) 0.088(4) Uani 1 1 d D . .
H4A H 0.0570 0.9865 0.2293 0.106 Uiso 1 1 calc R . .
H4B H 0.1207 0.9328 0.1850 0.106 Uiso 1 1 calc R . .
C5 C 0.2578(12) 0.9955(6) 0.2169(10) 0.083(4) Uani 1 1 d . . .
H5A H 0.2675 1.0259 0.2597 0.099 Uiso 1 1 calc R . .
H5B H 0.2495 1.0138 0.1611 0.099 Uiso 1 1 calc R . .
C6 C 0.3840(13) 0.9558(7) 0.2224(8) 0.089(4) Uani 1 1 d D . .
H6A H 0.3769 0.9266 0.1777 0.106 Uiso 1 1 calc R . .
H6B H 0.4641 0.9788 0.2145 0.106 Uiso 1 1 calc R . .
C7 C 0.5224(9) 0.8955(4) 0.3238(6) 0.041(2) Uani 1 1 d . . .
C8 C 0.0160(9) 0.8970(4) 0.3297(7) 0.052(3) Uani 1 1 d . . .
C9 C 0.7761(8) 0.6607(3) 0.4587(5) 0.0339(18) Uani 1 1 d . . .
H9 H 0.7125 0.6381 0.4220 0.041 Uiso 1 1 calc R . .
C10 C 0.7242(9) 0.6616(4) 0.5485(6) 0.0380(19) Uani 1 1 d . . .
H10A H 0.6336 0.6774 0.5460 0.046 Uiso 1 1 calc R . .
H10B H 0.7808 0.6870 0.5844 0.046 Uiso 1 1 calc R . .
C11 C 0.7226(9) 0.6007(4) 0.5888(6) 0.039(2) Uani 1 1 d . . .
H11 H 0.7099 0.6068 0.6497 0.047 Uiso 1 1 calc R . .
C12 C 0.8600(10) 0.5721(4) 0.5838(8) 0.062(3) Uani 1 1 d . . .
H12A H 0.9252 0.5932 0.6203 0.075 Uiso 1 1 calc R . .
H12B H 0.8554 0.5327 0.6053 0.075 Uiso 1 1 calc R . .
C13 C 0.9076(10) 0.5708(4) 0.4942(9) 0.063(3) Uani 1 1 d . . .
H13C H 0.8468 0.5470 0.4586 0.076 Uiso 1 1 calc R . .
H13D H 0.9963 0.5532 0.4948 0.076 Uiso 1 1 calc R . .
C14 C 0.9138(9) 0.6320(4) 0.4561(7) 0.050(3) Uani 1 1 d . . .
H14C H 0.9803 0.6551 0.4886 0.061 Uiso 1 1 calc R . .
H14D H 0.9403 0.6298 0.3976 0.061 Uiso 1 1 calc R . .
C15 C 0.7746(8) 0.7222(4) 0.4269(6) 0.038(2) Uani 1 1 d . . .
C16 C 0.6049(8) 0.5636(3) 0.5557(5) 0.0318(17) Uani 1 1 d . . .
C17 C 0.5248(16) 0.6725(9) 0.0954(10) 0.105(5) Uani 1 1 d . . .
H17A H 0.6217 0.6778 0.0976 0.126 Uiso 1 1 calc R . .
H17B H 0.4859 0.6950 0.0478 0.126 Uiso 1 1 calc R . .
C18 C 0.4899(17) 0.6082(9) 0.0835(12) 0.091(6) Uani 1 1 d . . .
H18A H 0.5377 0.5923 0.0364 0.109 Uiso 1 1 calc R . .
H18B H 0.5170 0.5867 0.1349 0.109 Uiso 1 1 calc R . .
C19 C 0.2939(17) 0.5439(6) 0.0612(8) 0.093(5) Uani 1 1 d D . .
H19A H 0.3249 0.5211 0.1105 0.112 Uiso 1 1 calc R . .
H19B H 0.3213 0.5244 0.0100 0.112 Uiso 1 1 calc R . .
C20 C 0.1427(17) 0.5501(9) 0.0586(12) 0.088(6) Uani 1 1 d D . .
H20A H 0.1128 0.5794 0.0172 0.105 Uiso 1 1 calc R . .
H20B H 0.0995 0.5135 0.0433 0.105 Uiso 1 1 calc R . .
C21 C -0.0247(16) 0.5924(7) 0.1422(13) 0.122(6) Uani 1 1 d D . .
H21C H -0.0894 0.5732 0.1031 0.146 Uiso 1 1 calc R . .
H21D H -0.0533 0.5868 0.1999 0.146 Uiso 1 1 calc R . .
C22 C -0.0212(18) 0.6566(7) 0.1222(12) 0.096(7) Uani 1 1 d D . .
H22A H 0.0393 0.6661 0.0777 0.115 Uiso 1 1 calc R . .
H22B H -0.1098 0.6729 0.1089 0.115 Uiso 1 1 calc R . .
C23 C -0.018(3) 0.7251(10) 0.2373(15) 0.102(12) Uani 1 1 d D . .
H23A H 0.0054 0.7331 0.2970 0.122 Uiso 1 1 calc R . .
H23B H -0.1142 0.7302 0.2247 0.122 Uiso 1 1 calc R . .
C24 C 0.0685(13) 0.7562(7) 0.1762(10) 0.083(5) Uani 1 1 d D . .
H24A H 0.0389 0.7964 0.1739 0.099 Uiso 1 1 calc R . .
H24B H 0.0480 0.7398 0.1200 0.099 Uiso 1 1 calc R . .
C25 C 0.3050(14) 0.7753(8) 0.1610(11) 0.095(8) Uani 1 1 d D . .
H25A H 0.3010 0.8166 0.1738 0.114 Uiso 1 1 calc R . .
H25B H 0.2841 0.7720 0.1000 0.114 Uiso 1 1 calc R . .
C26 C 0.4502(14) 0.7599(7) 0.1726(11) 0.093(5) Uani 1 1 d D . .
H26A H 0.4865 0.7757 0.2265 0.112 Uiso 1 1 calc R . .
H26B H 0.4989 0.7775 0.1272 0.112 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
U1 O1 1.759(6) . ?
U1 O2 1.762(6) . ?
U1 O8 2.436(6) 1_655 ?
U1 O6 2.449(5) . ?
U1 O10 2.455(5) . ?
U1 O5 2.455(5) . ?
U1 O7 2.480(6) 1_655 ?
U1 O9 2.481(5) . ?
U2 O3 1.754(5) . ?
U2 O4 1.755(5) . ?
U2 O12 2.325(5) 3_666 ?
U2 O11 2.335(5) . ?
U2 O14 2.392(5) . ?
U2 O13 2.449(5) . ?
U2 O15 2.484(5) . ?
O5 C7 1.266(10) . ?
O6 C7 1.262(10) . ?
O7 C8 1.274(10) . ?
O7 U1 2.480(6) 1_455 ?
O8 C8 1.266(11) . ?
O8 U1 2.436(6) 1_455 ?
O9 C15 1.280(10) . ?
O10 C15 1.282(10) . ?
O11 C16 1.242(10) . ?
O12 C16 1.258(9) . ?
O12 U2 2.325(5) 3_666 ?
O13 H13A 0.8917 . ?
O13 H13B 0.9841 . ?
O14 H14A 0.8684 . ?
O14 H14B 0.8311 . ?
O15 H15A 0.8107 . ?
O15 H15B 0.8963 . ?
O16 C17 1.399(16) . ?
O16 C26 1.595(18) . ?
O17 C18 1.40(2) . ?
O17 C19 1.466(17) . ?
O18 C20 1.28(2) . ?
O18 C21 1.530(19) . ?
O19 C23 1.42(2) . ?
O19 C22 1.459(19) . ?
O20 C25 1.067(19) . ?
O20 C24 1.511(19) . ?
O21 H21A 0.8925 . ?
O21 H21B 0.9758 . ?
C1 C7 1.475(13) . ?
C1 C6 1.483(9) . ?
C1 C2 1.506(13) . ?
C1 H1 0.9800 . ?
C2 C3 1.522(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.480(19) . ?
C3 C8 1.491(14) . ?
C3 H3 0.9800 . ?
C4 C5 1.492(17) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.551(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C15 1.500(11) . ?
C9 C14 1.522(11) . ?
C9 C10 1.524(12) . ?
C9 H9 0.9800 . ?
C10 C11 1.535(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C16 1.518(12) . ?
C11 C12 1.522(14) . ?
C11 H11 0.9800 . ?
C12 C13 1.506(17) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.531(13) . ?
C13 H13C 0.9700 . ?
C13 H13D 0.9700 . ?
C14 H14C 0.9700 . ?
C14 H14D 0.9700 . ?
C17 C18 1.53(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.508(10) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.51(2) . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.50(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.489(10) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 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
O1 U1 O2 179.2(3) . . ?
O1 U1 O8 89.5(3) . 1_655 ?
O2 U1 O8 89.8(3) . 1_655 ?
O1 U1 O6 88.8(2) . . ?
O2 U1 O6 91.3(2) . . ?
O8 U1 O6 119.44(19) 1_655 . ?
O1 U1 O10 91.0(2) . . ?
O2 U1 O10 89.7(2) . . ?
O8 U1 O10 120.50(19) 1_655 . ?
O6 U1 O10 120.05(18) . . ?
O1 U1 O5 91.2(2) . . ?
O2 U1 O5 88.2(2) . . ?
O8 U1 O5 66.67(19) 1_655 . ?
O6 U1 O5 52.86(18) . . ?
O10 U1 O5 172.54(19) . . ?
O1 U1 O7 89.9(2) . 1_655 ?
O2 U1 O7 89.9(3) . 1_655 ?
O8 U1 O7 52.8(2) 1_655 1_655 ?
O6 U1 O7 172.17(19) . 1_655 ?
O10 U1 O7 67.69(19) . 1_655 ?
O5 U1 O7 119.46(19) . 1_655 ?
O1 U1 O9 93.1(2) . . ?
O2 U1 O9 87.7(2) . . ?
O8 U1 O9 172.95(19) 1_655 . ?
O6 U1 O9 67.23(18) . . ?
O10 U1 O9 52.92(18) . . ?
O5 U1 O9 119.80(18) . . ?
O7 U1 O9 120.56(18) 1_655 . ?
O3 U2 O4 176.4(2) . . ?
O3 U2 O12 91.8(2) . 3_666 ?
O4 U2 O12 91.8(2) . 3_666 ?
O3 U2 O11 87.2(2) . . ?
O4 U2 O11 93.9(2) . . ?
O12 U2 O11 75.88(19) 3_666 . ?
O3 U2 O14 86.5(2) . . ?
O4 U2 O14 90.7(2) . . ?
O12 U2 O14 136.98(19) 3_666 . ?
O11 U2 O14 146.70(19) . . ?
O3 U2 O13 90.1(2) . . ?
O4 U2 O13 86.9(2) . . ?
O12 U2 O13 150.79(19) 3_666 . ?
O11 U2 O13 75.11(18) . . ?
O14 U2 O13 72.23(18) . . ?
O3 U2 O15 89.8(2) . . ?
O4 U2 O15 91.2(2) . . ?
O12 U2 O15 69.57(19) 3_666 . ?
O11 U2 O15 145.21(18) . . ?
O14 U2 O15 67.44(19) . . ?
O13 U2 O15 139.60(18) . . ?
C7 O5 U1 93.7(5) . . ?
C7 O6 U1 94.1(5) . . ?
C8 O7 U1 93.0(5) . 1_455 ?
C8 O8 U1 95.3(5) . 1_455 ?
C15 O9 U1 93.8(5) . . ?
C15 O10 U1 94.9(5) . . ?
C16 O11 U2 146.3(5) . . ?
C16 O12 U2 176.4(6) . 3_666 ?
U2 O13 H13A 133.3 . . ?
U2 O13 H13B 123.6 . . ?
H13A O13 H13B 98.5 . . ?
U2 O14 H14A 116.9 . . ?
U2 O14 H14B 128.6 . . ?
H14A O14 H14B 112.4 . . ?
U2 O15 H15A 120.5 . . ?
U2 O15 H15B 122.4 . . ?
H15A O15 H15B 114.3 . . ?
C17 O16 C26 111.7(11) . . ?
C18 O17 C19 118.3(13) . . ?
C20 O18 C21 115.7(13) . . ?
C23 O19 C22 112.6(14) . . ?
C25 O20 C24 138.6(18) . . ?
H21A O21 H21B 101.3 . . ?
C7 C1 C6 113.2(10) . . ?
C7 C1 C2 114.9(8) . . ?
C6 C1 C2 114.1(10) . . ?
C7 C1 H1 104.3 . . ?
C6 C1 H1 104.3 . . ?
C2 C1 H1 104.3 . . ?
C1 C2 C3 112.5(8) . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 C8 112.7(10) . . ?
C4 C3 C2 113.8(10) . . ?
C8 C3 C2 114.3(9) . . ?
C4 C3 H3 105.0 . . ?
C8 C3 H3 105.0 . . ?
C2 C3 H3 105.0 . . ?
C3 C4 C5 112.7(11) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 110.3(11) . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C1 C6 C5 109.2(11) . . ?
C1 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
C1 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
O6 C7 O5 119.4(8) . . ?
O6 C7 C1 121.2(8) . . ?
O5 C7 C1 119.3(8) . . ?
O8 C8 O7 118.9(8) . . ?
O8 C8 C3 120.0(8) . . ?
O7 C8 C3 121.0(8) . . ?
C15 C9 C14 113.1(7) . . ?
C15 C9 C10 107.2(7) . . ?
C14 C9 C10 112.4(8) . . ?
C15 C9 H9 108.0 . . ?
C14 C9 H9 108.0 . . ?
C10 C9 H9 108.0 . . ?
C9 C10 C11 112.2(7) . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C16 C11 C12 114.7(8) . . ?
C16 C11 C10 113.4(7) . . ?
C12 C11 C10 110.1(7) . . ?
C16 C11 H11 106.0 . . ?
C12 C11 H11 106.0 . . ?
C10 C11 H11 106.0 . . ?
C13 C12 C11 112.6(8) . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 C14 111.4(9) . . ?
C12 C13 H13C 109.3 . . ?
C14 C13 H13C 109.3 . . ?
C12 C13 H13D 109.3 . . ?
C14 C13 H13D 109.3 . . ?
H13C C13 H13D 108.0 . . ?
C9 C14 C13 109.4(7) . . ?
C9 C14 H14C 109.8 . . ?
C13 C14 H14C 109.8 . . ?
C9 C14 H14D 109.8 . . ?
C13 C14 H14D 109.8 . . ?
H14C C14 H14D 108.2 . . ?
O9 C15 O10 118.3(7) . . ?
O9 C15 C9 120.2(7) . . ?
O10 C15 C9 121.5(7) . . ?
O11 C16 O12 123.4(8) . . ?
O11 C16 C11 119.4(7) . . ?
O12 C16 C11 117.1(7) . . ?
O16 C17 C18 108.0(12) . . ?
O16 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
O16 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
O17 C18 C17 109.1(13) . . ?
O17 C18 H18A 109.9 . . ?
C17 C18 H18A 109.9 . . ?
O17 C18 H18B 109.9 . . ?
C17 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O17 C19 C20 107.4(12) . . ?
O17 C19 H19A 110.2 . . ?
C20 C19 H19A 110.2 . . ?
O17 C19 H19B 110.2 . . ?
C20 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
O18 C20 C19 105.6(13) . . ?
O18 C20 H20A 110.6 . . ?
C19 C20 H20A 110.6 . . ?
O18 C20 H20B 110.6 . . ?
C19 C20 H20B 110.6 . . ?
H20A C20 H20B 108.8 . . ?
C22 C21 O18 110.4(13) . . ?
C22 C21 H21C 109.6 . . ?
O18 C21 H21C 109.6 . . ?
C22 C21 H21D 109.6 . . ?
O18 C21 H21D 109.6 . . ?
H21C C21 H21D 108.1 . . ?
O19 C22 C21 93.1(14) . . ?
O19 C22 H22A 113.1 . . ?
C21 C22 H22A 113.1 . . ?
O19 C22 H22B 113.1 . . ?
C21 C22 H22B 113.1 . . ?
H22A C22 H22B 110.5 . . ?
O19 C23 C24 88.5(14) . . ?
O19 C23 H23A 113.9 . . ?
C24 C23 H23A 113.9 . . ?
O19 C23 H23B 113.9 . . ?
C24 C23 H23B 113.9 . . ?
H23A C23 H23B 111.1 . . ?
C23 C24 O20 121.2(18) . . ?
C23 C24 H24A 107.0 . . ?
O20 C24 H24A 107.0 . . ?
C23 C24 H24B 107.0 . . ?
O20 C24 H24B 107.0 . . ?
H24A C24 H24B 106.8 . . ?
O20 C25 C26 130(2) . . ?
O20 C25 H25A 104.9 . . ?
C26 C25 H25A 104.9 . . ?
O20 C25 H25B 104.9 . . ?
C26 C25 H25B 104.9 . . ?
H25A C25 H25B 105.8 . . ?
C25 C26 O16 111.7(11) . . ?
C25 C26 H26A 109.3 . . ?
O16 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
O16 C26 H26B 109.3 . . ?
H26A C26 H26B 107.9 . . ?

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
O13 H13A O9 0.89 1.93 2.804(8) 167.7 .
O13 H13B O21 0.98 1.76 2.700(8) 159.8 .
O14 H14A O16 0.87 1.83 2.700(9) 176.0 .
O14 H14B O19 0.83 1.92 2.718(10) 159.3 .
O15 H15A O18 0.81 1.93 2.733(10) 172.2 .
O15 H15B O5 0.90 2.11 2.951(8) 156.9 2_645
O21 H21A O7 0.89 2.13 2.854(9) 137.6 .
O21 H21B O10 0.98 2.09 3.003(9) 155.6 1_455


