# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Pierre Thuery'

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

_publ_section_title              
;
Uranyl-organic bilayer assemblages with flexible
aromatic di-, tri- and tetracarboxylic acids
;

# Attachment 'CIF.txt'

data_1
_database_code_depnum_ccdc_archive 'CCDC 712709'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 O7 U'
_chemical_formula_weight         480.21

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

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

_cell_length_a                   8.5125(8)
_cell_length_b                   11.5690(8)
_cell_length_c                   25.143(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2476.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    48064
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_absorpt_coefficient_mu    13.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_T_max  0.674
_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 three ω scans with 2° steps (285 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            48064
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         25.68
_reflns_number_total             2341
_reflns_number_gt                1751
_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. The aromatic ring was distorted, probably due
to unresolved disorder, and it was refined as an idealized hexagon. Some
restraints on bond lengths and/or displacement parameters were applied
for the aromatic ring and the atoms C2 and C3. 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)+(0.0632P)²+36.3431P] 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       0.00122(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2341
_refine_ls_number_parameters     152
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1417
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.966
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.222

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 0.65838(6) 0.27744(4) 0.419657(19) 0.0452(3) Uani 1 1 d . . .
O1 O 0.6253(12) 0.2848(9) 0.4888(4) 0.061(3) Uani 1 1 d . . .
O2 O 0.6938(14) 0.2684(11) 0.3519(4) 0.076(3) Uani 1 1 d . . .
O3 O 0.5087(13) 0.4596(9) 0.4096(5) 0.070(3) Uani 1 1 d . . .
O4 O 0.3778(13) 0.3043(10) 0.4063(5) 0.071(3) Uani 1 1 d . . .
O5 O -0.0712(15) 0.5926(10) 0.4208(5) 0.085(4) Uani 1 1 d . . .
O6 O -0.1535(13) 0.4208(10) 0.4308(5) 0.077(3) Uani 1 1 d . . .
O7 O 0.9001(12) 0.1717(9) 0.4353(5) 0.066(3) Uani 1 1 d . . .
H7A H 0.9316 0.1986 0.4702 0.079 Uiso 1 1 d R . .
H7B H 0.9770 0.1271 0.4250 0.079 Uiso 1 1 d R . .
C1 C 0.3804(18) 0.4115(12) 0.4091(7) 0.062(4) Uani 1 1 d . . .
C2 C 0.252(2) 0.4879(18) 0.4245(6) 0.059(8) Uani 1 1 d DU . .
H2A H 0.2781 0.5678 0.4168 0.071 Uiso 1 1 calc R . .
H2B H 0.2300 0.4807 0.4622 0.071 Uiso 1 1 calc R . .
C3 C 0.1172(17) 0.4506(18) 0.3930(4) 0.084(11) Uani 1 1 d DU . .
H3 H 0.1180 0.3661 0.3951 0.101 Uiso 1 1 calc R . .
C4 C -0.0451(15) 0.4876(12) 0.4159(6) 0.063(4) Uani 1 1 d . . .
C5 C 0.1331(15) 0.4770(10) 0.3360(3) 0.093(6) Uani 1 1 d GDU . .
C6 C 0.0702(15) 0.3993(9) 0.2996(5) 0.101(7) Uani 1 1 d GU . .
H6 H 0.0286 0.3295 0.3114 0.122 Uiso 1 1 calc R . .
C7 C 0.0696(15) 0.4259(11) 0.2457(4) 0.096(6) Uani 1 1 d GU . .
H7 H 0.0275 0.3739 0.2214 0.115 Uiso 1 1 calc R . .
C8 C 0.1318(14) 0.5303(11) 0.2282(3) 0.082(6) Uani 1 1 d G . .
H8 H 0.1313 0.5481 0.1921 0.098 Uiso 1 1 calc R . .
C9 C 0.1947(15) 0.6080(9) 0.2646(4) 0.083(6) Uani 1 1 d G . .
H9 H 0.2363 0.6778 0.2529 0.099 Uiso 1 1 calc R . .
C10 C 0.1954(15) 0.5814(10) 0.3185(4) 0.097(6) Uani 1 1 d GU . .
H10 H 0.2375 0.6334 0.3428 0.116 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
U O2 1.733(11) . ?
U O1 1.763(10) . ?
U O5 2.264(12) 8_655 ?
U O6 2.322(11) 1_655 ?
U O7 2.426(10) . ?
U O4 2.432(10) . ?
U O3 2.475(10) . ?
O3 C1 1.225(18) . ?
O4 C1 1.242(18) . ?
O5 C4 1.241(18) . ?
O5 U 2.264(12) 8_665 ?
O6 C4 1.260(9) . ?
O6 U 2.322(11) 1_455 ?
O7 H7A 0.9679 . ?
O7 H7B 0.8735 . ?
C1 C2 1.458(10) . ?
C2 C3 1.460(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.472(13) . ?
C3 C4 1.557(10) . ?
C3 H3 0.9800 . ?
C5 C6 1.3900 . ?
C5 C10 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U O1 178.9(5) . . ?
O2 U O5 90.7(6) . 8_655 ?
O1 U O5 88.9(5) . 8_655 ?
O2 U O6 92.4(6) . 1_655 ?
O1 U O6 87.5(5) . 1_655 ?
O5 U O6 154.1(4) 8_655 1_655 ?
O2 U O7 88.9(5) . . ?
O1 U O7 90.0(4) . . ?
O5 U O7 78.4(4) 8_655 . ?
O6 U O7 75.9(4) 1_655 . ?
O2 U O4 92.5(5) . . ?
O1 U O4 88.5(5) . . ?
O5 U O4 78.5(4) 8_655 . ?
O6 U O4 127.0(4) 1_655 . ?
O7 U O4 156.9(4) . . ?
O2 U O3 92.3(5) . . ?
O1 U O3 88.7(4) . . ?
O5 U O3 129.5(4) 8_655 . ?
O6 U O3 76.1(4) 1_655 . ?
O7 U O3 151.9(4) . . ?
O4 U O3 51.1(4) . . ?
C1 O3 U 94.2(9) . . ?
C1 O4 U 95.9(10) . . ?
C4 O5 U 169.2(13) . 8_665 ?
C4 O6 U 155.1(11) . 1_455 ?
U O7 H7A 102.7 . . ?
U O7 H7B 152.3 . . ?
H7A O7 H7B 104.6 . . ?
O3 C1 O4 118.0(13) . . ?
O3 C1 C2 113.0(14) . . ?
O4 C1 C2 127.3(16) . . ?
C1 C2 C3 105.4(13) . . ?
C1 C2 H2A 110.7 . . ?
C3 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
C3 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
C2 C3 C5 113.3(9) . . ?
C2 C3 C4 114.5(13) . . ?
C5 C3 C4 112.7(9) . . ?
C2 C3 H3 105.1 . . ?
C5 C3 H3 105.1 . . ?
C4 C3 H3 105.1 . . ?
O5 C4 O6 116.1(12) . . ?
O5 C4 C3 117.7(12) . . ?
O6 C4 C3 126.2(13) . . ?
C6 C5 C10 120.0 . . ?
C6 C5 C3 118.1(12) . . ?
C10 C5 C3 121.6(6) . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C5 120.0 . . ?
C9 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?

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 O1 0.97 1.95 2.751(14) 138.0 4_556
O7 H7B O3 0.87 1.98 2.653(15) 133.0 8_755

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 712710'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H38 O28 U3'
_chemical_formula_weight         1488.63

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   'C 2/c'

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

_cell_length_a                   17.1976(13)
_cell_length_b                   14.4008(10)
_cell_length_c                   17.4440(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.938(4)
_cell_angle_gamma                90.00
_cell_volume                     3885.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    58543
_cell_measurement_theta_min      2.63
_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          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2728
_exptl_absorpt_coefficient_mu    12.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_T_max  0.686
_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 four ω scans with 2° steps (409 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            58543
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         25.68
_reflns_number_total             3684
_reflns_number_gt                3092
_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. 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)+(0.0358P)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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3684
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0646
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_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         0.825
_refine_diff_density_min         -1.904
_refine_diff_density_rms         0.196

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 0.088340(15) 0.240265(15) 0.107740(14) 0.01959(8) Uani 1 1 d . . .
U2 U 0.0000 0.17350(2) 0.7500 0.02173(10) Uani 1 2 d S . .
O1 O 0.0068(3) 0.2954(3) 0.1273(3) 0.0244(9) Uani 1 1 d . . .
O2 O 0.1668(3) 0.1842(3) 0.0865(3) 0.0250(10) Uani 1 1 d . . .
O3 O 0.1551(3) 0.1721(3) 0.2514(3) 0.0252(10) Uani 1 1 d . . .
O4 O 0.1934(3) 0.3136(3) 0.2368(2) 0.0250(10) Uani 1 1 d . . .
O5 O 0.3634(3) -0.1068(3) 0.4186(2) 0.0242(10) Uani 1 1 d . . .
O6 O 0.4660(3) -0.1735(3) 0.5288(2) 0.0221(9) Uani 1 1 d . . .
O7 O 0.0280(3) 0.1489(3) 0.5102(2) 0.0227(9) Uani 1 1 d . . .
O8 O -0.0207(3) 0.0927(3) 0.3809(2) 0.0217(9) Uani 1 1 d . . .
O9 O 0.0896(3) 0.1737(3) 0.8500(3) 0.0264(10) Uani 1 1 d . . .
O10 O 0.0000 0.0030(4) 0.7500 0.0265(15) Uani 1 2 d S . .
H10 H -0.0115 -0.0416 0.7865 0.032 Uiso 1 1 d R . .
O11 O 0.0861(3) 0.1150(3) 0.6832(2) 0.0246(10) Uani 1 1 d . . .
H11A H 0.0722 0.1236 0.6320 0.030 Uiso 1 1 d R . .
H11B H 0.1344 0.0762 0.7053 0.030 Uiso 1 1 d R . .
O12 O 0.0484(3) 0.3045(3) 0.6992(3) 0.0293(11) Uani 1 1 d . . .
H12A H 0.0342 0.3184 0.6472 0.035 Uiso 1 1 d R . .
H12B H 0.0707 0.3649 0.7271 0.035 Uiso 1 1 d R . .
O13 O 0.0000 0.4196(4) 0.2500 0.0346(16) Uani 1 2 d S . .
H13 H 0.0019 0.3809 0.2092 0.041 Uiso 1 1 d R . .
O14 O 0.2244(3) 0.0095(3) 0.7729(3) 0.0277(10) Uani 1 1 d . . .
H14A H 0.2058 -0.0401 0.7904 0.033 Uiso 1 1 d R . .
H14B H 0.2528 0.0437 0.8111 0.033 Uiso 1 1 d R . .
O15 O 0.1360(3) 0.4563(3) 0.7682(3) 0.0322(11) Uani 1 1 d . . .
H15A H 0.1066 0.5091 0.7669 0.039 Uiso 1 1 d R . .
H15B H 0.1892 0.4706 0.7674 0.039 Uiso 1 1 d R . .
C1 C 0.2569(4) 0.1647(4) 0.4274(4) 0.0198(13) Uani 1 1 d . . .
C2 C 0.3326(4) 0.1143(4) 0.4678(4) 0.0216(13) Uani 1 1 d . . .
H2 H 0.3826 0.1346 0.4648 0.026 Uiso 1 1 calc R . .
C3 C 0.3353(4) 0.0339(4) 0.5128(4) 0.0212(13) Uani 1 1 d . . .
C4 C 0.2600(4) 0.0050(4) 0.5189(4) 0.0231(14) Uani 1 1 d . . .
H4 H 0.2611 -0.0480 0.5498 0.028 Uiso 1 1 calc R . .
C5 C 0.1845(4) 0.0557(4) 0.4789(4) 0.0207(13) Uani 1 1 d . . .
C6 C 0.1824(4) 0.1352(4) 0.4337(4) 0.0207(13) Uani 1 1 d . . .
H6 H 0.1315 0.1692 0.4075 0.025 Uiso 1 1 calc R . .
C7 C 0.2537(5) 0.2527(4) 0.3783(4) 0.0245(14) Uani 1 1 d . . .
H7A H 0.2326 0.3030 0.4010 0.029 Uiso 1 1 calc R . .
H7B H 0.3120 0.2684 0.3875 0.029 Uiso 1 1 calc R . .
C8 C 0.1971(4) 0.2454(4) 0.2834(4) 0.0226(14) Uani 1 1 d . . .
C9 C 0.4160(4) -0.0253(4) 0.5534(4) 0.0226(14) Uani 1 1 d . . .
H9A H 0.4663 0.0130 0.5649 0.027 Uiso 1 1 calc R . .
H9B H 0.4212 -0.0491 0.6074 0.027 Uiso 1 1 calc R . .
C10 C 0.4150(4) -0.1058(4) 0.4974(4) 0.0217(13) Uani 1 1 d . . .
C11 C 0.1054(4) 0.0200(4) 0.4879(4) 0.0221(14) Uani 1 1 d . . .
H11C H 0.0849 -0.0363 0.4546 0.026 Uiso 1 1 calc R . .
H11D H 0.1220 0.0045 0.5472 0.026 Uiso 1 1 calc R . .
C12 C 0.0334(4) 0.0896(4) 0.4590(4) 0.0196(13) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.746(4) . ?
U1 O1 1.769(4) . ?
U1 O4 2.427(4) . ?
U1 O3 2.458(4) . ?
U1 O5 2.467(4) 4 ?
U1 O8 2.471(4) 2 ?
U1 O6 2.478(4) 4 ?
U1 O7 2.523(4) 2 ?
U2 O9 1.751(4) 2_556 ?
U2 O9 1.751(4) . ?
U2 O12 2.383(4) 2_556 ?
U2 O12 2.383(4) . ?
U2 O11 2.403(4) 2_556 ?
U2 O11 2.403(4) . ?
U2 O10 2.455(6) . ?
O3 C8 1.263(7) . ?
O4 C8 1.258(7) . ?
O5 C10 1.268(7) . ?
O5 U1 2.467(4) 4_545 ?
O6 C10 1.265(7) . ?
O6 U1 2.478(4) 4_545 ?
O7 C12 1.268(7) . ?
O7 U1 2.523(4) 2 ?
O8 C12 1.271(7) . ?
O8 U1 2.471(4) 2 ?
O10 H10 0.9835 . ?
O11 H11A 0.8255 . ?
O11 H11B 0.9322 . ?
O12 H12A 0.8539 . ?
O12 H12B 0.9891 . ?
O13 H13 0.9157 . ?
O14 H14A 0.8893 . ?
O14 H14B 0.8004 . ?
O15 H15A 0.9080 . ?
O15 H15B 0.9437 . ?
C1 C2 1.384(8) . ?
C1 C6 1.399(8) . ?
C1 C7 1.517(8) . ?
C2 C3 1.389(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.407(9) . ?
C3 C9 1.516(8) . ?
C4 C5 1.382(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(8) . ?
C5 C11 1.526(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.514(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 C10 1.511(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.499(8) . ?
C11 H11C 0.9700 . ?
C11 H11D 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
O2 U1 O1 178.59(19) . . ?
O2 U1 O4 93.88(17) . . ?
O1 U1 O4 87.51(17) . . ?
O2 U1 O3 88.42(17) . . ?
O1 U1 O3 92.20(17) . . ?
O4 U1 O3 53.28(14) . . ?
O2 U1 O5 91.08(17) . 4 ?
O1 U1 O5 89.71(17) . 4 ?
O4 U1 O5 67.02(13) . 4 ?
O3 U1 O5 120.09(13) . 4 ?
O2 U1 O8 93.12(17) . 2 ?
O1 U1 O8 85.96(17) . 2 ?
O4 U1 O8 119.01(13) . 2 ?
O3 U1 O8 66.48(13) . 2 ?
O5 U1 O8 172.34(13) 4 2 ?
O2 U1 O6 91.67(17) . 4 ?
O1 U1 O6 87.89(16) . 4 ?
O4 U1 O6 119.23(13) . 4 ?
O3 U1 O6 172.49(13) . 4 ?
O5 U1 O6 52.40(13) 4 4 ?
O8 U1 O6 121.00(13) 2 4 ?
O2 U1 O7 89.79(16) . 2 ?
O1 U1 O7 88.80(17) . 2 ?
O4 U1 O7 170.55(13) . 2 ?
O3 U1 O7 118.23(13) . 2 ?
O5 U1 O7 121.67(13) 4 2 ?
O8 U1 O7 52.00(13) 2 2 ?
O6 U1 O7 69.28(13) 4 2 ?
O9 U2 O9 179.8(3) 2_556 . ?
O9 U2 O12 94.07(17) 2_556 2_556 ?
O9 U2 O12 85.77(17) . 2_556 ?
O9 U2 O12 85.77(17) 2_556 . ?
O9 U2 O12 94.07(17) . . ?
O12 U2 O12 75.4(2) 2_556 . ?
O9 U2 O11 91.34(17) 2_556 2_556 ?
O9 U2 O11 88.73(17) . 2_556 ?
O12 U2 O11 72.99(15) 2_556 2_556 ?
O12 U2 O11 147.95(15) . 2_556 ?
O9 U2 O11 88.73(17) 2_556 . ?
O9 U2 O11 91.34(17) . . ?
O12 U2 O11 147.95(15) 2_556 . ?
O12 U2 O11 72.99(15) . . ?
O11 U2 O11 138.9(2) 2_556 . ?
O9 U2 O10 90.10(13) 2_556 . ?
O9 U2 O10 90.10(13) . . ?
O12 U2 O10 142.31(11) 2_556 . ?
O12 U2 O10 142.31(11) . . ?
O11 U2 O10 69.47(10) 2_556 . ?
O11 U2 O10 69.47(10) . . ?
C8 O3 U1 92.2(4) . . ?
C8 O4 U1 93.8(4) . . ?
C10 O5 U1 94.5(4) . 4_545 ?
C10 O6 U1 94.1(3) . 4_545 ?
C12 O7 U1 93.0(3) . 2 ?
C12 O8 U1 95.4(3) . 2 ?
U2 O10 H10 130.8 . . ?
U2 O11 H11A 121.5 . . ?
U2 O11 H11B 129.4 . . ?
H11A O11 H11B 108.8 . . ?
U2 O12 H12A 126.7 . . ?
U2 O12 H12B 129.5 . . ?
H12A O12 H12B 100.7 . . ?
H14A O14 H14B 112.9 . . ?
H15A O15 H15B 110.4 . . ?
C2 C1 C6 119.4(5) . . ?
C2 C1 C7 121.3(6) . . ?
C6 C1 C7 119.3(6) . . ?
C1 C2 C3 121.0(6) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C2 C3 C4 119.0(6) . . ?
C2 C3 C9 122.0(6) . . ?
C4 C3 C9 118.9(6) . . ?
C5 C4 C3 119.9(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.6(6) . . ?
C4 C5 C11 117.0(5) . . ?
C6 C5 C11 122.4(5) . . ?
C5 C6 C1 120.0(6) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C8 C7 C1 114.0(5) . . ?
C8 C7 H7A 108.7 . . ?
C1 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
C1 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
O4 C8 O3 120.6(6) . . ?
O4 C8 C7 118.6(5) . . ?
O3 C8 C7 120.7(5) . . ?
C10 C9 C3 112.3(5) . . ?
C10 C9 H9A 109.1 . . ?
C3 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C3 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
O6 C10 O5 119.0(5) . . ?
O6 C10 C9 120.0(5) . . ?
O5 C10 C9 121.0(5) . . ?
C12 C11 C5 112.6(5) . . ?
C12 C11 H11C 109.1 . . ?
C5 C11 H11C 109.1 . . ?
C12 C11 H11D 109.1 . . ?
C5 C11 H11D 109.1 . . ?
H11C C11 H11D 107.8 . . ?
O7 C12 O8 119.1(5) . . ?
O7 C12 C11 121.2(5) . . ?
O8 C12 C11 119.6(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
O10 H10 O8 0.98 1.87 2.820(5) 160.8 6_556
O11 H11A O7 0.83 1.95 2.775(5) 174.2 .
O11 H11B O14 0.93 1.76 2.675(6) 164.7 .
O12 H12A O6 0.85 1.88 2.694(6) 158.9 3_455
O12 H12B O15 0.99 1.67 2.629(6) 161.0 .
O13 H13 O1 0.92 1.92 2.831(6) 177.4 .
O14 H14A O3 0.89 2.08 2.830(6) 141.7 6_556
O14 H14B O5 0.80 2.20 2.971(6) 161.6 6_556
O15 H15A O13 0.91 2.01 2.848(6) 153.5 5_566
O15 H15B O14 0.94 1.98 2.893(6) 161.6 4_556

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 712711'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H22 O28 U3'
_chemical_formula_weight         1592.61

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           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.7509(7)
_cell_length_b                   14.4507(13)
_cell_length_c                   16.4698(9)
_cell_angle_alpha                80.919(4)
_cell_angle_beta                 87.734(3)
_cell_angle_gamma                84.375(4)
_cell_volume                     2279.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    75249
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_absorpt_coefficient_mu    10.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.807
_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 (453 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            75249
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         25.68
_reflns_number_total             8604
_reflns_number_gt                6542
_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 restraints for some badly behaving atoms.
Four water solvent molecules were affected with 0.5 occupancy factors
so as to retain acceptable displacement parameters. The H atoms bound
to some O atoms (O12, O23, O26) were found on a Fourier-difference map,
but the other O-bound H atoms were not found, nor introduced. The C-bound
H atoms were introduced at calculated positions. All H atoms were treated
as riding atoms with an isotropic displacement parameter equal to 1.2
times that of the parent atom. Some voids in the lattice likely indicate
the presence of other, unresolved water solvent molecules.
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)+(0.0422P)²+93.0645P] 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         8604
_refine_ls_number_parameters     604
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1483
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.802
_refine_diff_density_min         -2.527
_refine_diff_density_rms         0.536

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 0.51715(5) 0.68415(4) 0.71355(3) 0.02404(16) Uani 1 1 d . . .
U2 U 0.01642(5) 0.66925(4) 0.57550(3) 0.01962(15) Uani 1 1 d . . .
U3 U 0.32653(12) 0.95475(7) -0.10124(4) 0.0758(4) Uani 1 1 d . . .
O1 O 0.4568(10) 0.8043(8) 0.6857(6) 0.027(2) Uani 1 1 d . . .
O2 O 0.5788(11) 0.5643(8) 0.7439(6) 0.028(2) Uani 1 1 d . . .
O3 O -0.0497(11) 0.7879(8) 0.5664(6) 0.026(2) Uani 1 1 d . . .
O4 O 0.0810(10) 0.5507(8) 0.5823(6) 0.026(2) Uani 1 1 d . . .
O5 O 0.2427(19) 0.9516(13) -0.0027(10) 0.081(5) Uani 1 1 d . . .
O6 O 0.4110(15) 0.9535(9) -0.1966(7) 0.053(4) Uani 1 1 d . . .
O7 O 0.6344(10) 0.7027(9) 0.5847(6) 0.030(3) Uani 1 1 d . . .
O8 O 0.8087(10) 0.6220(8) 0.5296(6) 0.027(2) Uani 1 1 d . . .
O9 O 0.3997(10) 0.6263(8) 0.6121(6) 0.030(3) Uani 1 1 d . . .
O10 O 0.2431(9) 0.7074(8) 0.5272(6) 0.024(2) Uani 1 1 d . . .
O11 O 0.7783(10) 0.5320(8) 0.2526(6) 0.030(3) Uani 1 1 d . . .
O12 O 0.5325(16) 0.8992(10) -0.0335(8) 0.053(3) Uani 1 1 d . . .
H12 H 0.6143 0.9090 -0.0641 0.064 Uiso 1 1 d R . .
O13 O 0.5586(18) 0.9072(11) 0.0990(9) 0.067(4) Uani 1 1 d . . .
O14 O 0.3591(12) 0.7912(9) -0.0834(7) 0.040(3) Uani 1 1 d . . .
O15 O 0.5192(10) 0.6968(8) -0.1382(6) 0.025(2) Uani 1 1 d . . .
O16 O 0.2994(10) 0.6561(9) 0.7736(6) 0.033(3) Uani 1 1 d . . .
O17 O 0.1240(10) 0.7083(7) 0.6912(6) 0.022(2) Uani 1 1 d . . .
O18 O -0.1105(9) 0.6234(7) 0.6987(5) 0.020(2) Uani 1 1 d . . .
O19 O -0.2640(9) 0.7241(7) 0.7510(6) 0.023(2) Uani 1 1 d . . .
O20 O 0.2502(10) 0.5706(8) 1.0633(6) 0.030(3) Uani 1 1 d . . .
O21 O -0.1564(15) 0.9037(10) 1.1295(8) 0.056(4) Uani 1 1 d . . .
O22 O -0.231(2) 0.8716(14) 1.2584(10) 0.087(5) Uani 1 1 d U . .
O23 O -0.1445(15) 0.7905(10) 1.3866(7) 0.054(4) Uani 1 1 d . . .
H23 H -0.1818 0.8275 1.3486 0.065 Uiso 1 1 d R . .
O24 O 0.0268(10) 0.6855(8) 1.4268(6) 0.024(2) Uani 1 1 d . . .
O25 O 0.1245(16) 0.9025(11) -0.1557(8) 0.062(4) Uani 1 1 d . . .
O26 O 0.184(2) 0.8905(16) 0.6845(11) 0.102(7) Uani 1 1 d . . .
H26A H 0.2702 0.8664 0.6718 0.122 Uiso 1 1 d R . .
H26B H 0.1683 0.8918 0.7384 0.122 Uiso 1 1 d R . .
O27 O -0.062(3) 0.877(2) -0.0470(17) 0.053(7) Uani 0.50 1 d PU . .
O28 O 0.725(3) 0.858(2) -0.1406(16) 0.052(7) Uani 0.50 1 d P . .
O29 O -0.124(3) 0.947(2) 0.6844(16) 0.053(7) Uani 0.50 1 d P . .
O30 O -0.247(3) 1.0433(19) 0.5219(16) 0.047(6) Uani 0.50 1 d PU . .
C1 C 0.5945(14) 0.6338(13) 0.4656(8) 0.028(4) Uani 1 1 d . . .
C2 C 0.4467(18) 0.6419(11) 0.4689(9) 0.030(4) Uani 1 1 d . . .
C3 C 0.3794(15) 0.6379(13) 0.3969(9) 0.031(4) Uani 1 1 d . . .
H3 H 0.2836 0.6457 0.3975 0.037 Uiso 1 1 calc R . .
C4 C 0.4483(16) 0.6229(14) 0.3243(9) 0.036(4) Uani 1 1 d . . .
H4 H 0.3997 0.6235 0.2767 0.043 Uiso 1 1 calc R . .
C5 C 0.5920(14) 0.6067(12) 0.3236(8) 0.027(3) Uani 1 1 d . . .
C6 C 0.6616(16) 0.6114(11) 0.3944(9) 0.027(3) Uani 1 1 d . . .
H6 H 0.7570 0.5992 0.3942 0.033 Uiso 1 1 calc R . .
C7 C 0.6835(15) 0.6543(12) 0.5328(9) 0.026(3) Uani 1 1 d . . .
C8 C 0.3583(15) 0.6609(12) 0.5416(8) 0.024(3) Uani 1 1 d . . .
C9 C 0.6691(15) 0.5823(12) 0.2486(9) 0.028(3) Uani 1 1 d . . .
C10 C 0.544(2) 0.7581(13) 0.0625(10) 0.041(5) Uani 1 1 d . . .
C11 C 0.5279(15) 0.6990(12) 0.0047(9) 0.026(3) Uani 1 1 d . . .
C12 C 0.5607(15) 0.6028(13) 0.0265(8) 0.030(4) Uani 1 1 d . . .
H12A H 0.5540 0.5636 -0.0125 0.036 Uiso 1 1 calc R . .
C13 C 0.6029(15) 0.5636(13) 0.1046(9) 0.031(4) Uani 1 1 d . . .
H13 H 0.6256 0.4991 0.1175 0.037 Uiso 1 1 calc R . .
C14 C 0.6114(16) 0.6225(13) 0.1647(9) 0.032(4) Uani 1 1 d . . .
C15 C 0.5833(19) 0.7175(14) 0.1427(10) 0.042(5) Uani 1 1 d . . .
H15 H 0.5899 0.7566 0.1818 0.051 Uiso 1 1 calc R . .
C16 C 0.544(2) 0.8608(15) 0.0414(12) 0.051(5) Uani 1 1 d . . .
C17 C 0.4650(17) 0.7332(12) -0.0790(9) 0.031(4) Uani 1 1 d . . .
C18 C 0.0813(13) 0.6593(10) 0.8316(8) 0.018(3) Uani 1 1 d . . .
C19 C -0.0697(15) 0.6604(12) 0.8314(9) 0.026(3) Uani 1 1 d . . .
C20 C -0.1460(17) 0.6526(15) 0.9036(9) 0.040(5) Uani 1 1 d . . .
H20 H -0.2416 0.6573 0.9013 0.048 Uiso 1 1 calc R . .
C21 C -0.0851(16) 0.6381(14) 0.9797(9) 0.034(4) Uani 1 1 d . . .
H21 H -0.1387 0.6318 1.0279 0.041 Uiso 1 1 calc R . .
C22 C 0.0598(15) 0.6328(11) 0.9826(9) 0.024(3) Uani 1 1 d . . .
C23 C 0.1355(14) 0.6397(11) 0.9101(8) 0.023(3) Uani 1 1 d . . .
H23A H 0.2309 0.6305 0.9137 0.027 Uiso 1 1 calc R . .
C24 C 0.1724(15) 0.6726(12) 0.7601(8) 0.025(3) Uani 1 1 d . . .
C25 C -0.1522(14) 0.6716(11) 0.7536(8) 0.022(3) Uani 1 1 d . . .
C26 C 0.1359(14) 0.6133(11) 1.0609(9) 0.021(3) Uani 1 1 d . . .
C27 C -0.0593(19) 0.7615(14) 1.2100(9) 0.041(5) Uani 1 1 d . . .
C28 C -0.0163(16) 0.7078(11) 1.2855(9) 0.028(3) Uani 1 1 d . . .
C29 C 0.0646(15) 0.6230(11) 1.2848(9) 0.025(3) Uani 1 1 d . . .
H29 H 0.0871 0.5855 1.3346 0.030 Uiso 1 1 calc R . .
C30 C 0.1126(14) 0.5928(11) 1.2121(9) 0.023(3) Uani 1 1 d . . .
H30 H 0.1694 0.5371 1.2132 0.028 Uiso 1 1 calc R . .
C31 C 0.0749(14) 0.6466(11) 1.1382(9) 0.024(3) Uani 1 1 d . . .
C32 C -0.0097(17) 0.7293(13) 1.1372(9) 0.034(4) Uani 1 1 d . . .
H32 H -0.0345 0.7648 1.0869 0.041 Uiso 1 1 calc R . .
C33 C -0.152(2) 0.8501(17) 1.1998(13) 0.058(5) Uani 1 1 d . . .
C34 C -0.0469(17) 0.7301(13) 1.3706(9) 0.033(4) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.773(11) . ?
U1 O2 1.777(11) . ?
U1 O16 2.351(10) . ?
U1 O7 2.361(10) . ?
U1 O9 2.363(10) . ?
U1 O19 2.393(9) 1_655 ?
U1 O15 2.478(9) 1_556 ?
U2 O4 1.755(10) . ?
U2 O3 1.757(11) . ?
U2 O18 2.371(9) . ?
U2 O17 2.381(9) . ?
U2 O8 2.386(10) 1_455 ?
U2 O10 2.405(9) . ?
U2 O24 2.422(9) 1_554 ?
U3 O6 1.746(13) . ?
U3 O5 1.783(17) . ?
U3 O14 2.327(13) . ?
U3 O12 2.346(13) . ?
U3 O13 2.388(17) 2_675 ?
U3 O25 2.428(17) . ?
U3 O21 2.500(13) 2_576 ?
O7 C7 1.242(19) . ?
O8 C7 1.265(18) . ?
O8 U2 2.386(10) 1_655 ?
O9 C8 1.255(17) . ?
O10 C8 1.262(18) . ?
O11 C9 1.227(18) . ?
O12 C16 1.28(2) . ?
O12 H12 0.9370 . ?
O13 C16 1.26(2) . ?
O13 U3 2.388(17) 2_675 ?
O14 C17 1.261(19) . ?
O15 C17 1.254(18) . ?
O15 U1 2.478(9) 1_554 ?
O16 C24 1.260(17) . ?
O17 C24 1.259(17) . ?
O18 C25 1.259(17) . ?
O19 C25 1.263(17) . ?
O19 U1 2.393(9) 1_455 ?
O20 C26 1.220(17) . ?
O21 C33 1.29(2) . ?
O21 U3 2.500(13) 2_576 ?
O22 C33 1.27(3) . ?
O23 C34 1.28(2) . ?
O23 H23 0.8267 . ?
O24 C34 1.250(18) . ?
O24 U2 2.422(9) 1_556 ?
O26 H26A 0.9075 . ?
O26 H26B 0.8973 . ?
C1 C6 1.39(2) . ?
C1 C2 1.43(2) . ?
C1 C7 1.515(19) . ?
C2 C3 1.39(2) . ?
C2 C8 1.49(2) . ?
C3 C4 1.39(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.40(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(19) . ?
C5 C9 1.49(2) . ?
C6 H6 0.9300 . ?
C9 C14 1.52(2) . ?
C10 C11 1.40(2) . ?
C10 C15 1.41(2) . ?
C10 C16 1.47(3) . ?
C11 C12 1.39(2) . ?
C11 C17 1.52(2) . ?
C12 C13 1.38(2) . ?
C12 H12A 0.9300 . ?
C13 C14 1.41(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.37(3) . ?
C15 H15 0.9300 . ?
C18 C23 1.393(18) . ?
C18 C24 1.447(19) . ?
C18 C19 1.471(19) . ?
C19 C20 1.37(2) . ?
C19 C25 1.518(18) . ?
C20 C21 1.39(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.41(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.37(2) . ?
C22 C26 1.487(19) . ?
C23 H23A 0.9300 . ?
C26 C31 1.510(19) . ?
C27 C32 1.40(2) . ?
C27 C28 1.41(2) . ?
C27 C33 1.48(3) . ?
C28 C29 1.39(2) . ?
C28 C34 1.50(2) . ?
C29 C30 1.39(2) . ?
C29 H29 0.9300 . ?
C30 C31 1.38(2) . ?
C30 H30 0.9300 . ?
C31 C32 1.38(2) . ?
C32 H32 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.5(5) . . ?
O1 U1 O16 89.0(5) . . ?
O2 U1 O16 90.9(5) . . ?
O1 U1 O7 84.9(4) . . ?
O2 U1 O7 96.1(4) . . ?
O16 U1 O7 141.4(3) . . ?
O1 U1 O9 96.8(4) . . ?
O2 U1 O9 84.6(4) . . ?
O16 U1 O9 75.3(3) . . ?
O7 U1 O9 67.7(3) . . ?
O1 U1 O19 91.8(4) . 1_655 ?
O2 U1 O19 87.4(4) . 1_655 ?
O16 U1 O19 139.5(3) . 1_655 ?
O7 U1 O19 78.9(3) . 1_655 ?
O9 U1 O19 144.5(3) . 1_655 ?
O1 U1 O15 92.9(4) . 1_556 ?
O2 U1 O15 85.7(4) . 1_556 ?
O16 U1 O15 70.7(3) . 1_556 ?
O7 U1 O15 147.6(3) . 1_556 ?
O9 U1 O15 144.4(3) . 1_556 ?
O19 U1 O15 68.8(3) 1_655 1_556 ?
O4 U2 O3 178.7(4) . . ?
O4 U2 O18 86.7(4) . . ?
O3 U2 O18 94.0(4) . . ?
O4 U2 O17 99.5(4) . . ?
O3 U2 O17 81.8(4) . . ?
O18 U2 O17 68.9(3) . . ?
O4 U2 O8 86.3(4) . 1_455 ?
O3 U2 O8 92.8(4) . 1_455 ?
O18 U2 O8 75.9(3) . 1_455 ?
O17 U2 O8 143.9(3) . 1_455 ?
O4 U2 O10 86.8(4) . . ?
O3 U2 O10 93.3(4) . . ?
O18 U2 O10 141.3(3) . . ?
O17 U2 O10 74.6(3) . . ?
O8 U2 O10 141.5(3) 1_455 . ?
O4 U2 O24 90.2(4) . 1_554 ?
O3 U2 O24 88.6(4) . 1_554 ?
O18 U2 O24 147.1(3) . 1_554 ?
O17 U2 O24 143.6(3) . 1_554 ?
O8 U2 O24 71.2(3) 1_455 1_554 ?
O10 U2 O24 71.0(3) . 1_554 ?
O6 U3 O5 177.9(7) . . ?
O6 U3 O14 86.8(5) . . ?
O5 U3 O14 91.1(7) . . ?
O6 U3 O12 90.6(5) . . ?
O5 U3 O12 88.1(7) . . ?
O14 U3 O12 69.0(4) . . ?
O6 U3 O13 84.2(6) . 2_675 ?
O5 U3 O13 97.2(8) . 2_675 ?
O14 U3 O13 143.3(5) . 2_675 ?
O12 U3 O13 75.6(5) . 2_675 ?
O6 U3 O25 89.7(6) . . ?
O5 U3 O25 90.3(7) . . ?
O14 U3 O25 73.6(5) . . ?
O12 U3 O25 142.6(5) . . ?
O13 U3 O25 141.6(5) 2_675 . ?
O6 U3 O21 102.2(5) . 2_576 ?
O5 U3 O21 79.8(6) . 2_576 ?
O14 U3 O21 145.8(5) . 2_576 ?
O12 U3 O21 142.5(5) . 2_576 ?
O13 U3 O21 70.9(5) 2_675 2_576 ?
O25 U3 O21 73.5(5) . 2_576 ?
C7 O7 U1 139.5(11) . . ?
C7 O8 U2 133.4(10) . 1_655 ?
C8 O9 U1 134.1(10) . . ?
C8 O10 U2 129.5(10) . . ?
C16 O12 U3 126.7(14) . . ?
C16 O12 H12 117.0 . . ?
U3 O12 H12 116.3 . . ?
C16 O13 U3 130.8(15) . 2_675 ?
C17 O14 U3 133.3(12) . . ?
C17 O15 U1 148.1(10) . 1_554 ?
C24 O16 U1 142.0(10) . . ?
C24 O17 U2 142.1(10) . . ?
C25 O18 U2 128.8(9) . . ?
C25 O19 U1 126.0(9) . 1_455 ?
C33 O21 U3 122.0(13) . 2_576 ?
C34 O23 H23 119.7 . . ?
C34 O24 U2 134.5(10) . 1_556 ?
H26A O26 H26B 114.1 . . ?
C6 C1 C2 118.5(13) . . ?
C6 C1 C7 117.1(12) . . ?
C2 C1 C7 124.4(13) . . ?
C3 C2 C1 117.5(14) . . ?
C3 C2 C8 116.8(14) . . ?
C1 C2 C8 125.6(13) . . ?
C4 C3 C2 123.1(14) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 119.0(13) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 118.9(14) . . ?
C6 C5 C9 120.5(13) . . ?
C4 C5 C9 120.6(13) . . ?
C5 C6 C1 122.6(14) . . ?
C5 C6 H6 118.7 . . ?
C1 C6 H6 118.7 . . ?
O7 C7 O8 123.9(13) . . ?
O7 C7 C1 120.5(14) . . ?
O8 C7 C1 115.6(13) . . ?
O9 C8 O10 124.5(13) . . ?
O9 C8 C2 118.5(14) . . ?
O10 C8 C2 116.9(12) . . ?
O11 C9 C5 122.0(13) . . ?
O11 C9 C14 119.1(13) . . ?
C5 C9 C14 118.8(13) . . ?
C11 C10 C15 118.9(17) . . ?
C11 C10 C16 123.5(15) . . ?
C15 C10 C16 116.9(16) . . ?
C12 C11 C10 118.8(14) . . ?
C12 C11 C17 117.5(14) . . ?
C10 C11 C17 123.6(15) . . ?
C13 C12 C11 121.9(15) . . ?
C13 C12 H12A 119.0 . . ?
C11 C12 H12A 119.0 . . ?
C12 C13 C14 119.4(16) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C15 C14 C13 118.7(14) . . ?
C15 C14 C9 120.5(15) . . ?
C13 C14 C9 120.3(15) . . ?
C14 C15 C10 122.1(16) . . ?
C14 C15 H15 119.0 . . ?
C10 C15 H15 119.0 . . ?
O13 C16 O12 123(2) . . ?
O13 C16 C10 117.9(18) . . ?
O12 C16 C10 119.3(16) . . ?
O15 C17 O14 124.8(14) . . ?
O15 C17 C11 116.5(13) . . ?
O14 C17 C11 118.5(13) . . ?
C23 C18 C24 120.1(12) . . ?
C23 C18 C19 113.5(12) . . ?
C24 C18 C19 126.3(12) . . ?
C20 C19 C18 120.9(13) . . ?
C20 C19 C25 115.4(13) . . ?
C18 C19 C25 123.7(12) . . ?
C19 C20 C21 122.1(15) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C22 118.7(14) . . ?
C20 C21 H21 120.7 . . ?
C22 C21 H21 120.7 . . ?
C23 C22 C21 118.9(13) . . ?
C23 C22 C26 117.9(13) . . ?
C21 C22 C26 123.0(13) . . ?
C22 C23 C18 125.5(13) . . ?
C22 C23 H23A 117.3 . . ?
C18 C23 H23A 117.3 . . ?
O17 C24 O16 123.9(13) . . ?
O17 C24 C18 119.7(13) . . ?
O16 C24 C18 115.9(12) . . ?
O18 C25 O19 124.2(12) . . ?
O18 C25 C19 118.3(13) . . ?
O19 C25 C19 117.3(12) . . ?
O20 C26 C22 120.0(13) . . ?
O20 C26 C31 118.8(12) . . ?
C22 C26 C31 121.2(12) . . ?
C32 C27 C28 117.8(15) . . ?
C32 C27 C33 116.1(15) . . ?
C28 C27 C33 126.1(15) . . ?
C29 C28 C27 119.1(13) . . ?
C29 C28 C34 113.0(13) . . ?
C27 C28 C34 128.0(14) . . ?
C30 C29 C28 122.0(14) . . ?
C30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C31 C30 C29 119.1(14) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C30 C31 C32 120.0(13) . . ?
C30 C31 C26 117.0(13) . . ?
C32 C31 C26 122.9(13) . . ?
C31 C32 C27 121.9(14) . . ?
C31 C32 H32 119.0 . . ?
C27 C32 H32 119.0 . . ?
O22 C33 O21 120(2) . . ?
O22 C33 C27 120.9(19) . . ?
O21 C33 C27 119.4(17) . . ?
O24 C34 O23 120.4(14) . . ?
O24 C34 C28 117.0(14) . . ?
O23 C34 C28 122.6(14) . . ?

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
O12 H12 O28 0.94 1.82 2.61(3) 140.4 .
O23 H23 O22 0.83 1.60 2.39(2) 160.5 .
O26 H26A O1 0.91 1.95 2.82(2) 160.2 .
O26 H26B O25 0.90 1.81 2.70(2) 174.9 1_556


