# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H13 F N O7 U'
_chemical_formula_weight         504.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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                   12.1361(8)
_cell_length_b                   8.5565(6)
_cell_length_c                   23.3240(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2422.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    13.447
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10278
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2120
_reflns_number_gt                1789
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0282P)²+28.3834P] where P=(Fo²+2Fc²)/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_number_reflns         2120
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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
U1 U 0.81698(2) 0.85394(3) 0.362952(14) 0.01304(13) Uani 1 1 d . . .
O1W O 0.5779(8) 0.7048(13) 0.2544(4) 0.075(3) Uani 1 1 d . . .
H1W H 0.5530 0.6208 0.2397 0.091 Uiso 1 1 d R . .
H2W H 0.5879 0.7763 0.2296 0.091 Uiso 1 1 d R . .
O1 O 0.6245(4) 0.9063(6) 0.3692(3) 0.0188(14) Uani 1 1 d . . .
O2 O 0.5562(5) 1.1414(6) 0.3488(3) 0.0321(18) Uani 1 1 d . . .
O3 O 0.3385(6) 0.3760(7) 0.3504(4) 0.037(2) Uani 1 1 d . . .
O4 O 0.5079(5) 0.4699(7) 0.3647(3) 0.0266(16) Uani 1 1 d . . .
F1 F 0.7134(4) 0.6223(5) 0.3634(2) 0.0214(11) Uani 1 1 d . . .
O5 O 0.8086(5) 0.8603(7) 0.2865(3) 0.0222(14) Uani 1 1 d . . .
O6 O 0.8243(5) 0.8451(7) 0.4387(3) 0.0233(14) Uani 1 1 d . . .
N1 N 0.4333(6) 0.7644(7) 0.3682(3) 0.0134(15) Uani 1 1 d . . .
H0A H 0.5037 0.7288 0.3711 0.016 Uiso 1 1 calc R . .
C1 C 0.5491(7) 0.9966(9) 0.3541(4) 0.0167(19) Uani 1 1 d . . .
C2 C 0.4390(7) 0.9226(9) 0.3406(4) 0.0173(19) Uani 1 1 d . . .
H2A H 0.3799 0.9882 0.3550 0.021 Uiso 1 1 calc R . .
H2B H 0.4303 0.9126 0.2994 0.021 Uiso 1 1 calc R . .
C3 C 0.3705(7) 0.6460(10) 0.3337(4) 0.0187(19) Uani 1 1 d . . .
H3A H 0.3847 0.6616 0.2931 0.022 Uiso 1 1 calc R . .
H3B H 0.2921 0.6584 0.3402 0.022 Uiso 1 1 calc R . .
C4 C 0.4065(7) 0.4817(10) 0.3513(4) 0.020(2) Uani 1 1 d . . .
C5 C 0.5937(7) 0.9619(10) 0.5279(4) 0.020(2) Uani 1 1 d . . .
H5A H 0.6587 0.9375 0.5470 0.024 Uiso 1 1 calc R . .
C6 C 0.5443(7) 0.8466(10) 0.4959(4) 0.0180(18) Uani 1 1 d . . .
C7 C 0.4476(8) 0.8873(9) 0.4666(4) 0.0189(19) Uani 1 1 d . . .
C8 C 0.5923(9) 0.6857(10) 0.4936(5) 0.027(2) Uani 1 1 d . . .
H8A H 0.5433 0.6180 0.4728 0.040 Uiso 1 1 calc R . .
H8B H 0.6019 0.6467 0.5318 0.040 Uiso 1 1 calc R . .
H8C H 0.6623 0.6891 0.4745 0.040 Uiso 1 1 calc R . .
C9 C 0.3878(7) 0.7727(10) 0.4280(4) 0.018(2) Uani 1 1 d . . .
H9A H 0.3916 0.6695 0.4451 0.022 Uiso 1 1 calc R . .
H9B H 0.3107 0.8022 0.4260 0.022 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 O6 1.770(6) . ?
U1 O5 1.787(6) . ?
U1 F1 2.326(4) 8_765 ?
U1 O4 2.346(6) 8_765 ?
U1 F1 2.347(4) . ?
U1 O1 2.383(6) . ?
U1 O2 2.405(6) 8_755 ?
O1 C1 1.248(10) . ?
O2 C1 1.248(9) . ?
O2 U1 2.405(6) 8_765 ?
O3 C4 1.225(11) . ?
O4 C4 1.273(11) . ?
O4 U1 2.346(6) 8_755 ?
F1 U1 2.326(4) 8_755 ?
N1 C2 1.501(10) . ?
N1 C3 1.502(10) . ?
N1 C9 1.503(11) . ?
C1 C2 1.512(12) . ?
C3 C4 1.529(11) . ?
C5 C6 1.374(12) . ?
C5 C7 1.391(11) 5_676 ?
C6 C7 1.403(13) . ?
C6 C8 1.496(12) . ?
C7 C5 1.391(11) 5_676 ?
C7 C9 1.516(12) . ?

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
O6 U1 O5 179.2(3) . . ?
O6 U1 F1 92.6(2) . 8_765 ?
O5 U1 F1 88.1(2) . 8_765 ?
O6 U1 O4 87.4(3) . 8_765 ?
O5 U1 O4 93.2(3) . 8_765 ?
F1 U1 O4 74.09(19) 8_765 8_765 ?
O6 U1 F1 89.2(2) . . ?
O5 U1 F1 90.0(2) . . ?
F1 U1 F1 138.49(5) 8_765 . ?
O4 U1 F1 147.39(19) 8_765 . ?
O6 U1 O1 89.8(3) . . ?
O5 U1 O1 90.0(3) . . ?
F1 U1 O1 70.04(18) 8_765 . ?
O4 U1 O1 143.9(2) 8_765 . ?
F1 U1 O1 68.49(18) . . ?
O6 U1 O2 94.2(3) . 8_755 ?
O5 U1 O2 85.5(3) . 8_755 ?
F1 U1 O2 148.1(2) 8_765 8_755 ?
O4 U1 O2 75.1(2) 8_765 8_755 ?
F1 U1 O2 72.8(2) . 8_755 ?
O1 U1 O2 141.1(2) . 8_755 ?
C1 O1 U1 144.9(6) . . ?
C1 O2 U1 141.4(6) . 8_765 ?
C4 O4 U1 154.8(6) . 8_755 ?
U1 F1 U1 156.7(2) 8_755 . ?
C2 N1 C3 113.7(7) . . ?
C2 N1 C9 111.9(6) . . ?
C3 N1 C9 110.1(6) . . ?
O1 C1 O2 126.3(8) . . ?
O1 C1 C2 116.6(7) . . ?
O2 C1 C2 117.1(8) . . ?
N1 C2 C1 109.2(7) . . ?
N1 C3 C4 109.3(7) . . ?
O3 C4 O4 126.7(8) . . ?
O3 C4 C3 118.8(8) . . ?
O4 C4 C3 114.5(7) . . ?
C6 C5 C7 124.0(9) . 5_676 ?
C5 C6 C7 116.8(8) . . ?
C5 C6 C8 120.7(9) . . ?
C7 C6 C8 122.4(8) . . ?
C5 C7 C6 119.1(8) 5_676 . ?
C5 C7 C9 118.9(8) 5_676 . ?
C6 C7 C9 122.0(7) . . ?
N1 C9 C7 113.9(7) . . ?

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
O1W H2W O3 0.85 2.24 3.024(13) 154.0 3_655
O1W H1W O2 0.85 2.46 2.956(12) 118.0 3_645
N1 H0A O1W 0.91 2.87 3.222(12) 104.3 .
N1 H0A O1 0.91 2.11 2.619(8) 114.2 .
N1 H0A O4 0.91 2.22 2.679(9) 110.5 .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.109
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.207
_database_code_depnum_ccdc_archive 'CCDC 997026'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H25 N2 O10.50 U'
_chemical_formula_weight         687.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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                   23.664(3)
_cell_length_b                   14.0766(17)
_cell_length_c                   14.3858(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.281(5)
_cell_angle_gamma                90.00
_cell_volume                     4599.9(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2632
_exptl_absorpt_coefficient_mu    7.116
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17376
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4025
_reflns_number_gt                3709
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0264P)²+11.7351P] where P=(Fo²+2Fc²)/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_number_reflns         4025
_refine_ls_number_parameters     294
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0512
_refine_ls_wR_factor_gt          0.0501
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.364019(6) 0.324398(9) 0.362254(9) 0.02112(6) Uani 1 1 d . . .
O1 O 0.33374(12) 0.38676(19) 0.49310(19) 0.0311(6) Uani 1 1 d . . .
O1W O 0.5000 0.3839(6) 0.7500 0.093(2) Uani 1 2 d S . .
H1W H 0.5235 0.4249 0.7833 0.112 Uiso 0.50 1 d PR . .
H2W H 0.5000 0.3235 0.7500 0.112 Uiso 1 2 d SR . .
O2 O 0.41598(13) 0.4477(3) 0.5913(2) 0.0504(9) Uani 1 1 d . . .
O3 O 0.20696(13) 0.29170(19) 0.6006(2) 0.0352(7) Uani 1 1 d . . .
O4 O 0.16751(14) 0.33166(19) 0.7169(2) 0.0401(8) Uani 1 1 d . . .
O5 O 0.08141(11) 1.03338(18) 0.6191(2) 0.0308(6) Uani 1 1 d . . .
O6 O 0.14777(13) 0.9234(2) 0.6097(2) 0.0447(8) Uani 1 1 d . . .
O7 O 0.08457(12) 0.8082(2) 0.2528(2) 0.0340(7) Uani 1 1 d . . .
O8 O 0.15016(13) 0.8113(2) 0.3988(2) 0.0388(7) Uani 1 1 d . . .
O9 O 0.42342(12) 0.26658(19) 0.4456(2) 0.0332(6) Uani 1 1 d . . .
O10 O 0.30365(11) 0.38063(19) 0.28029(19) 0.0304(6) Uani 1 1 d . . .
N1 N 0.26532(13) 0.4511(2) 0.6011(2) 0.0227(6) Uani 1 1 d . . .
H1N H 0.2554 0.3993 0.5621 0.027 Uiso 1 1 calc R . .
N2 N 0.06964(13) 0.8078(2) 0.4962(2) 0.0218(6) Uani 1 1 d . . .
H2N H 0.1093 0.8163 0.5120 0.026 Uiso 1 1 calc R . .
C1 C 0.18220(17) 0.5495(3) 0.4973(3) 0.0292(9) Uani 1 1 d . . .
C2 C 0.15022(19) 0.4888(3) 0.4240(3) 0.0383(10) Uani 1 1 d . . .
C3 C 0.0899(2) 0.4992(3) 0.3915(3) 0.0454(11) Uani 1 1 d . . .
H3A H 0.0687 0.4579 0.3439 0.055 Uiso 1 1 calc R . .
C4 C 0.05928(19) 0.5686(3) 0.4265(3) 0.0382(10) Uani 1 1 d . . .
C5 C 0.09161(17) 0.6322(3) 0.4955(3) 0.0288(8) Uani 1 1 d . . .
C6 C 0.15313(17) 0.6222(3) 0.5323(3) 0.0276(8) Uani 1 1 d . . .
C8 C 0.1793(2) 0.4124(4) 0.3788(4) 0.0566(14) Uani 1 1 d . . .
H8A H 0.1498 0.3792 0.3301 0.085 Uiso 1 1 calc R . .
H8B H 0.1995 0.3684 0.4279 0.085 Uiso 1 1 calc R . .
H8C H 0.2069 0.4412 0.3497 0.085 Uiso 1 1 calc R . .
C9 C -0.0076(2) 0.5707(4) 0.3854(4) 0.0564(14) Uani 1 1 d . . .
H9A H -0.0234 0.6212 0.4152 0.085 Uiso 1 1 calc R . .
H9B H -0.0237 0.5112 0.3984 0.085 Uiso 1 1 calc R . .
H9C H -0.0177 0.5809 0.3167 0.085 Uiso 1 1 calc R . .
C10 C 0.18799(19) 0.6912(3) 0.6089(3) 0.0407(11) Uani 1 1 d . . .
H10A H 0.2290 0.6750 0.6257 0.061 Uiso 1 1 calc R . .
H10B H 0.1742 0.6873 0.6656 0.061 Uiso 1 1 calc R . .
H10C H 0.1827 0.7548 0.5838 0.061 Uiso 1 1 calc R . .
C11 C 0.24819(17) 0.5373(3) 0.5361(3) 0.0316(9) Uani 1 1 d . . .
H11A H 0.2648 0.5937 0.5722 0.038 Uiso 1 1 calc R . .
H11B H 0.2649 0.5312 0.4821 0.038 Uiso 1 1 calc R . .
C12 C 0.33060(16) 0.4469(3) 0.6445(3) 0.0291(9) Uani 1 1 d . . .
H12A H 0.3397 0.3979 0.6938 0.035 Uiso 1 1 calc R . .
H12B H 0.3440 0.5071 0.6758 0.035 Uiso 1 1 calc R . .
C13 C 0.36386(17) 0.4264(3) 0.5705(3) 0.0290(9) Uani 1 1 d . . .
C14 C 0.23310(18) 0.4420(3) 0.6768(3) 0.0282(8) Uani 1 1 d . . .
H14A H 0.2055 0.4942 0.6709 0.034 Uiso 1 1 calc R . .
H14B H 0.2609 0.4449 0.7408 0.034 Uiso 1 1 calc R . .
C15 C 0.20050(17) 0.3490(3) 0.6642(3) 0.0279(8) Uani 1 1 d . . .
C16 C 0.04681(17) 0.8862(3) 0.5471(3) 0.0308(9) Uani 1 1 d . . .
H16A H 0.0295 0.8593 0.5949 0.037 Uiso 1 1 calc R . .
H16B H 0.0165 0.9217 0.5006 0.037 Uiso 1 1 calc R . .
C17 C 0.09716(17) 0.9520(3) 0.5965(3) 0.0260(8) Uani 1 1 d . . .
C18 C 0.04888(18) 0.8149(3) 0.3889(3) 0.0303(9) Uani 1 1 d . . .
H18A H 0.0281 0.8745 0.3707 0.036 Uiso 1 1 calc R . .
H18B H 0.0217 0.7635 0.3633 0.036 Uiso 1 1 calc R . .
C19 C 0.10049(17) 0.8100(3) 0.3454(3) 0.0267(8) Uani 1 1 d . . .
C29 C 0.06072(17) 0.7106(3) 0.5350(3) 0.0280(8) Uani 1 1 d . . .
H29A H 0.0189 0.6969 0.5182 0.034 Uiso 1 1 calc R . .
H29B H 0.0755 0.7114 0.6051 0.034 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 O10 1.765(3) . ?
U1 O9 1.769(3) . ?
U1 O7 2.324(3) 4_545 ?
U1 O5 2.357(2) 7_566 ?
U1 O1 2.363(2) . ?
U1 O4 2.490(3) 7_556 ?
U1 O3 2.506(3) 7_556 ?
U1 C15 2.848(4) 7_556 ?
O1 C13 1.270(5) . ?
O2 C13 1.222(5) . ?
O3 C15 1.262(5) . ?
O3 U1 2.506(3) 7_556 ?
O4 C15 1.255(5) . ?
O4 U1 2.490(3) 7_556 ?
O5 C17 1.274(4) . ?
O5 U1 2.357(2) 7_566 ?
O6 C17 1.227(5) . ?
O7 C19 1.280(5) . ?
O7 U1 2.324(3) 4 ?
O8 C19 1.211(5) . ?
N1 C12 1.496(5) . ?
N1 C14 1.500(4) . ?
N1 C11 1.515(5) . ?
N2 C18 1.487(5) . ?
N2 C16 1.506(4) . ?
N2 C29 1.514(5) . ?
C1 C6 1.403(5) . ?
C1 C2 1.403(6) . ?
C1 C11 1.514(5) . ?
C2 C3 1.380(6) . ?
C2 C8 1.518(6) . ?
C3 C4 1.392(6) . ?
C4 C5 1.395(6) . ?
C4 C9 1.526(6) . ?
C5 C6 1.410(5) . ?
C5 C29 1.519(5) . ?
C6 C10 1.526(6) . ?
C12 C13 1.519(5) . ?
C14 C15 1.505(5) . ?
C15 U1 2.848(4) 7_556 ?
C16 C17 1.519(5) . ?
C18 C19 1.521(5) . ?

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
O10 U1 O9 178.69(12) . . ?
O10 U1 O7 93.18(11) . 4_545 ?
O9 U1 O7 87.83(11) . 4_545 ?
O10 U1 O5 90.59(11) . 7_566 ?
O9 U1 O5 90.44(11) . 7_566 ?
O7 U1 O5 77.56(9) 4_545 7_566 ?
O10 U1 O1 89.78(11) . . ?
O9 U1 O1 89.55(11) . . ?
O7 U1 O1 160.04(10) 4_545 . ?
O5 U1 O1 82.68(9) 7_566 . ?
O10 U1 O4 90.43(12) . 7_556 ?
O9 U1 O4 89.03(12) . 7_556 ?
O7 U1 O4 74.80(9) 4_545 7_556 ?
O5 U1 O4 152.36(9) 7_566 7_556 ?
O1 U1 O4 124.95(9) . 7_556 ?
O10 U1 O3 88.26(11) . 7_556 ?
O9 U1 O3 90.47(12) . 7_556 ?
O7 U1 O3 127.17(9) 4_545 7_556 ?
O5 U1 O3 155.26(9) 7_566 7_556 ?
O1 U1 O3 72.61(9) . 7_556 ?
O4 U1 O3 52.38(9) 7_556 7_556 ?
O10 U1 C15 89.54(12) . 7_556 ?
O9 U1 C15 89.46(12) . 7_556 ?
O7 U1 C15 100.90(10) 4_545 7_556 ?
O5 U1 C15 178.46(10) 7_566 7_556 ?
O1 U1 C15 98.86(10) . 7_556 ?
O4 U1 C15 26.11(10) 7_556 7_556 ?
O3 U1 C15 26.27(10) 7_556 7_556 ?
C13 O1 U1 129.8(2) . . ?
C15 O3 U1 92.2(2) . 7_556 ?
C15 O4 U1 93.1(2) . 7_556 ?
C17 O5 U1 127.0(2) . 7_566 ?
C19 O7 U1 132.8(3) . 4 ?
C12 N1 C14 111.7(3) . . ?
C12 N1 C11 110.8(3) . . ?
C14 N1 C11 114.5(3) . . ?
C18 N2 C16 113.3(3) . . ?
C18 N2 C29 113.9(3) . . ?
C16 N2 C29 112.1(3) . . ?
C6 C1 C2 119.9(4) . . ?
C6 C1 C11 120.7(4) . . ?
C2 C1 C11 119.4(3) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 C8 118.6(4) . . ?
C1 C2 C8 122.7(4) . . ?
C2 C3 C4 123.0(4) . . ?
C3 C4 C5 118.1(4) . . ?
C3 C4 C9 117.4(4) . . ?
C5 C4 C9 124.4(4) . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 C29 120.5(3) . . ?
C6 C5 C29 119.1(3) . . ?
C1 C6 C5 119.8(4) . . ?
C1 C6 C10 120.2(3) . . ?
C5 C6 C10 120.0(3) . . ?
C1 C11 N1 112.9(3) . . ?
N1 C12 C13 113.1(3) . . ?
O2 C13 O1 127.1(3) . . ?
O2 C13 C12 117.8(4) . . ?
O1 C13 C12 115.1(3) . . ?
N1 C14 C15 109.5(3) . . ?
O4 C15 O3 122.4(3) . . ?
O4 C15 C14 118.8(3) . . ?
O3 C15 C14 118.8(3) . . ?
O4 C15 U1 60.83(19) . 7_556 ?
O3 C15 U1 61.58(19) . 7_556 ?
C14 C15 U1 178.5(3) . 7_556 ?
N2 C16 C17 109.4(3) . . ?
O6 C17 O5 126.7(4) . . ?
O6 C17 C16 118.4(3) . . ?
O5 C17 C16 114.8(3) . . ?
N2 C18 C19 110.7(3) . . ?
O8 C19 O7 127.7(4) . . ?
O8 C19 C18 119.2(4) . . ?
O7 C19 C18 113.1(3) . . ?
N2 C29 C5 112.7(3) . . ?

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
O1W H1W O2 0.85 1.99 2.725(4) 144.2 2_656

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.091
_database_code_depnum_ccdc_archive 'CCDC 997027'
