# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

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

data_1
_audit_block_doi                 10.5517/cc147ksq
_database_code_depnum_ccdc_archive 'CCDC 1049963'
_audit_update_record             
;
2015-03-26 deposited with the CCDC.
2015-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        UO2(dbsf)(phen)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 N2 O8 S U'
_chemical_formula_weight         754.50

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'
S S 0.1246 0.1234 '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   P212121

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

_cell_length_a                   8.4350(17)
_cell_length_b                   12.595(3)
_cell_length_c                   22.468(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2387.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate-like
_exptl_crystal_colour            yellow-green
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_absorpt_coefficient_mu    6.944
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            7932
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         25.12
_reflns_number_total             4248
_reflns_number_gt                4227
_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)+(0.0480P)²+26.6671P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.494(10)
_refine_ls_number_reflns         4248
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0919
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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 1.04023(3) 0.42410(2) 0.563525(12) 0.00712(10) Uani 1 1 d . . .
S1 S 0.2543(2) 0.62514(16) 0.32757(9) 0.0103(4) Uani 1 1 d . . .
N2 N 1.1626(8) 0.2558(6) 0.6137(3) 0.0096(14) Uani 1 1 d . . .
O4 O 0.7672(7) 0.4147(5) 0.5266(2) 0.0127(12) Uani 1 1 d . . .
N1 N 0.8577(9) 0.3084(6) 0.6335(3) 0.0126(15) Uani 1 1 d . . .
O3 O 0.9083(7) 0.5513(5) 0.4964(3) 0.0133(13) Uani 1 1 d . . .
O8 O 0.1424(7) 0.5380(5) 0.3234(3) 0.0145(13) Uani 1 1 d . . .
O7 O 0.3250(8) 0.6659(5) 0.2739(3) 0.0143(13) Uani 1 1 d . . .
C25 C 0.9248(10) 0.2347(7) 0.6700(3) 0.0107(16) Uani 1 1 d . . .
C13 C 0.1545(10) 0.7319(7) 0.3635(4) 0.0127(17) Uani 1 1 d . . .
C2 C 0.6479(11) 0.5299(7) 0.4543(4) 0.0128(17) Uani 1 1 d . . .
C4 C 0.5425(11) 0.6500(7) 0.3800(4) 0.0140(16) Uani 1 1 d . . .
H4 H 0.5519 0.7102 0.3562 0.017 Uiso 1 1 calc R . .
C1 C 0.7803(11) 0.4977(7) 0.4942(4) 0.0128(17) Uani 1 1 d . . .
C3 C 0.6634(10) 0.6208(7) 0.4188(4) 0.0141(18) Uani 1 1 d . . .
H3 H 0.7548 0.6618 0.4212 0.017 Uiso 1 1 calc R . .
O2 O 1.2248(7) 0.5668(5) 0.5338(2) 0.0124(12) Uani 1 1 d . . .
O6 O 0.9921(7) 0.5068(5) 0.6244(3) 0.0138(13) Uani 1 1 d . . .
O1 O 1.3169(7) 0.4490(5) 0.5972(3) 0.0154(13) Uani 1 1 d . . .
O5 O 1.0904(7) 0.3463(5) 0.5005(3) 0.0144(13) Uani 1 1 d . . .
C27 C 1.0627(11) 0.0689(7) 0.7368(3) 0.0145(17) Uani 1 1 d . . .
H27 H 1.1061 0.0124 0.7579 0.017 Uiso 1 1 calc R . .
C15 C -0.0114(9) 0.7947(6) 0.4425(3) 0.0109(16) Uani 1 1 d . . .
H15 H -0.0558 0.7858 0.4800 0.013 Uiso 1 1 calc R . .
C18 C 1.3041(10) 0.0826(7) 0.6726(3) 0.0142(17) Uani 1 1 d . . .
H18 H 1.3529 0.0266 0.6924 0.017 Uiso 1 1 calc R . .
C10 C -0.0472(10) 0.8851(6) 0.4095(3) 0.0101(15) Uani 1 1 d . . .
C5 C 0.4061(10) 0.5865(7) 0.3774(3) 0.0108(16) Uani 1 1 d . . .
C6 C 0.3882(10) 0.4977(6) 0.4127(4) 0.0092(15) Uani 1 1 d . . .
H6 H 0.2957 0.4577 0.4108 0.011 Uiso 1 1 calc R . .
C9 C 1.3269(10) 0.5394(6) 0.5719(3) 0.0106(16) Uani 1 1 d . . .
C11 C 0.0301(10) 0.9023(6) 0.3544(3) 0.0101(15) Uani 1 1 d . . .
H11 H 0.0128 0.9651 0.3336 0.012 Uiso 1 1 calc R . .
C24 C 0.8423(11) 0.1881(7) 0.7187(4) 0.0142(18) Uani 1 1 d . . .
C14 C 0.0904(10) 0.7173(7) 0.4198(4) 0.0142(17) Uani 1 1 d . . .
H14 H 0.1148 0.6572 0.4420 0.017 Uiso 1 1 calc R . .
C7 C 0.5120(10) 0.4683(6) 0.4515(3) 0.0101(17) Uani 1 1 d . . .
H7 H 0.5025 0.4079 0.4751 0.012 Uiso 1 1 calc R . .
C19 C 1.1519(10) 0.1160(6) 0.6893(4) 0.0121(16) Uani 1 1 d . . .
C16 C 1.3074(10) 0.2203(7) 0.5983(4) 0.0129(17) Uani 1 1 d . . .
H16 H 1.3609 0.2545 0.5676 0.015 Uiso 1 1 calc R . .
C22 C 0.6219(11) 0.3022(7) 0.6950(4) 0.0169(18) Uani 1 1 d . . .
H22 H 0.5215 0.3290 0.7031 0.020 Uiso 1 1 calc R . .
C20 C 1.0839(10) 0.2017(6) 0.6574(3) 0.0112(17) Uani 1 1 d . . .
C17 C 1.3811(11) 0.1339(7) 0.6264(4) 0.0138(17) Uani 1 1 d . . .
H17 H 1.4809 0.1113 0.6142 0.017 Uiso 1 1 calc R . .
C12 C 0.1323(10) 0.8254(7) 0.3312(4) 0.0123(16) Uani 1 1 d . . .
H12 H 0.1841 0.8362 0.2951 0.015 Uiso 1 1 calc R . .
C21 C 0.7079(12) 0.3392(7) 0.6458(4) 0.0168(18) Uani 1 1 d . . .
H21 H 0.6593 0.3874 0.6203 0.020 Uiso 1 1 calc R . .
C23 C 0.6881(12) 0.2259(8) 0.7311(4) 0.0194(19) Uani 1 1 d . . .
H23 H 0.6317 0.1995 0.7634 0.023 Uiso 1 1 calc R . .
C26 C 0.9167(11) 0.1047(7) 0.7517(4) 0.0157(19) Uani 1 1 d . . .
H26 H 0.8640 0.0747 0.7840 0.019 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 1.767(6) . ?
U1 O5 1.774(6) . ?
U1 O4 2.451(6) . ?
U1 O3 2.466(6) . ?
U1 O2 2.470(6) . ?
U1 O1 2.473(6) . ?
U1 N2 2.613(7) . ?
U1 N1 2.640(7) . ?
U1 C9 2.827(8) . ?
U1 C1 2.844(9) . ?
S1 O7 1.440(6) . ?
S1 O8 1.451(6) . ?
S1 C5 1.769(8) . ?
S1 C13 1.780(9) . ?
N2 C16 1.346(12) . ?
N2 C20 1.368(11) . ?
O4 C1 1.278(11) . ?
N1 C21 1.350(12) . ?
N1 C25 1.362(11) . ?
O3 C1 1.274(11) . ?
C25 C24 1.423(12) . ?
C25 C20 1.433(12) . ?
C13 C14 1.388(12) . ?
C13 C12 1.397(12) . ?
C2 C7 1.385(12) . ?
C2 C3 1.401(13) . ?
C2 C1 1.489(12) . ?
C4 C3 1.392(12) . ?
C4 C5 1.402(12) . ?
O2 C9 1.263(10) . ?
O1 C9 1.275(10) . ?
C27 C26 1.353(13) . ?
C27 C19 1.434(12) . ?
C15 C10 1.392(11) . ?
C15 C14 1.395(12) . ?
C18 C17 1.384(13) . ?
C18 C19 1.402(13) . ?
C10 C11 1.415(11) . ?
C10 C9 1.486(12) 3_366 ?
C5 C6 1.379(12) . ?
C6 C7 1.410(12) . ?
C9 C10 1.486(12) 3_666 ?
C11 C12 1.398(12) . ?
C24 C23 1.413(14) . ?
C24 C26 1.431(13) . ?
C19 C20 1.417(12) . ?
C16 C17 1.404(12) . ?
C22 C23 1.376(13) . ?
C22 C21 1.401(13) . ?

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 177.4(3) . . ?
O6 U1 O4 94.3(2) . . ?
O5 U1 O4 85.8(2) . . ?
O6 U1 O3 89.3(2) . . ?
O5 U1 O3 88.7(2) . . ?
O4 U1 O3 53.1(2) . . ?
O6 U1 O2 85.7(2) . . ?
O5 U1 O2 92.0(2) . . ?
O4 U1 O2 122.39(19) . . ?
O3 U1 O2 69.28(19) . . ?
O6 U1 O1 84.6(2) . . ?
O5 U1 O1 95.1(2) . . ?
O4 U1 O1 175.1(2) . . ?
O3 U1 O1 122.04(19) . . ?
O2 U1 O1 52.82(19) . . ?
O6 U1 N2 103.6(2) . . ?
O5 U1 N2 78.6(2) . . ?
O4 U1 N2 118.6(2) . . ?
O3 U1 N2 165.7(2) . . ?
O2 U1 N2 117.3(2) . . ?
O1 U1 N2 66.3(2) . . ?
O6 U1 N1 74.4(2) . . ?
O5 U1 N1 108.0(3) . . ?
O4 U1 N1 68.1(2) . . ?
O3 U1 N1 117.4(2) . . ?
O2 U1 N1 158.5(2) . . ?
O1 U1 N1 116.0(2) . . ?
N2 U1 N1 61.7(2) . . ?
O6 U1 C9 80.9(2) . . ?
O5 U1 C9 97.6(3) . . ?
O4 U1 C9 148.3(2) . . ?
O3 U1 C9 95.3(2) . . ?
O2 U1 C9 26.5(2) . . ?
O1 U1 C9 26.8(2) . . ?
N2 U1 C9 92.9(2) . . ?
N1 U1 C9 138.0(2) . . ?
O6 U1 C1 93.1(3) . . ?
O5 U1 C1 85.8(3) . . ?
O4 U1 C1 26.6(2) . . ?
O3 U1 C1 26.5(2) . . ?
O2 U1 C1 95.8(2) . . ?
O1 U1 C1 148.6(2) . . ?
N2 U1 C1 143.6(2) . . ?
N1 U1 C1 93.2(2) . . ?
C9 U1 C1 121.9(2) . . ?
O7 S1 O8 119.0(4) . . ?
O7 S1 C5 109.2(4) . . ?
O8 S1 C5 107.7(4) . . ?
O7 S1 C13 107.9(4) . . ?
O8 S1 C13 107.0(4) . . ?
C5 S1 C13 105.2(4) . . ?
C16 N2 C20 117.3(7) . . ?
C16 N2 U1 121.1(6) . . ?
C20 N2 U1 121.5(5) . . ?
C1 O4 U1 94.1(5) . . ?
C21 N1 C25 117.5(7) . . ?
C21 N1 U1 120.6(6) . . ?
C25 N1 U1 119.5(5) . . ?
C1 O3 U1 93.5(5) . . ?
N1 C25 C24 122.7(8) . . ?
N1 C25 C20 117.9(7) . . ?
C24 C25 C20 119.3(8) . . ?
C14 C13 C12 122.2(8) . . ?
C14 C13 S1 119.9(7) . . ?
C12 C13 S1 117.7(6) . . ?
C7 C2 C3 120.6(8) . . ?
C7 C2 C1 119.7(8) . . ?
C3 C2 C1 119.7(8) . . ?
C3 C4 C5 118.4(7) . . ?
O3 C1 O4 119.0(8) . . ?
O3 C1 C2 121.0(8) . . ?
O4 C1 C2 120.0(8) . . ?
O3 C1 U1 59.9(4) . . ?
O4 C1 U1 59.3(4) . . ?
C2 C1 U1 175.4(6) . . ?
C4 C3 C2 120.3(8) . . ?
C9 O2 U1 92.8(5) . . ?
C9 O1 U1 92.3(5) . . ?
C26 C27 C19 121.6(8) . . ?
C10 C15 C14 120.7(7) . . ?
C17 C18 C19 119.4(8) . . ?
C15 C10 C11 119.5(7) . . ?
C15 C10 C9 121.9(7) . 3_366 ?
C11 C10 C9 118.5(7) . 3_366 ?
C6 C5 C4 121.9(7) . . ?
C6 C5 S1 120.5(6) . . ?
C4 C5 S1 117.6(6) . . ?
C5 C6 C7 119.2(8) . . ?
O2 C9 O1 120.0(8) . . ?
O2 C9 C10 120.3(7) . 3_666 ?
O1 C9 C10 119.6(7) . 3_666 ?
O2 C9 U1 60.7(4) . . ?
O1 C9 U1 60.9(4) . . ?
C10 C9 U1 163.5(6) 3_666 . ?
C12 C11 C10 120.3(7) . . ?
C23 C24 C25 117.5(8) . . ?
C23 C24 C26 123.3(8) . . ?
C25 C24 C26 119.2(8) . . ?
C13 C14 C15 118.7(8) . . ?
C2 C7 C6 119.5(7) . . ?
C18 C19 C20 117.6(8) . . ?
C18 C19 C27 123.8(8) . . ?
C20 C19 C27 118.6(8) . . ?
N2 C16 C17 123.0(8) . . ?
C23 C22 C21 119.1(9) . . ?
N2 C20 C19 123.1(8) . . ?
N2 C20 C25 116.8(7) . . ?
C19 C20 C25 120.0(8) . . ?
C18 C17 C16 119.4(8) . . ?
C13 C12 C11 118.2(8) . . ?
N1 C21 C22 123.3(8) . . ?
C22 C23 C24 119.6(8) . . ?
C27 C26 C24 121.0(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.12
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.985
_refine_diff_density_rms         0.154
_exptl_crystal_recrystallization_method hydrothermal
_chemical_properties_physical    'Heat-sensitive, Light-sensitive'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_audit_block_doi                 10.5517/cc147ktr
_database_code_depnum_ccdc_archive 'CCDC 1049964'
_audit_update_record             
;
2015-03-26 deposited with the CCDC.
2015-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        UO2(dbsf)(phen)(H2O)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H18 N2 O9 S U'
_chemical_formula_weight         772.51

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'
S S 0.1246 0.1234 '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   P21/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                   14.395(3)
_cell_length_b                   8.6750(17)
_cell_length_c                   20.368(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.16(3)
_cell_angle_gamma                90.00
_cell_volume                     2533.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    6.549
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            4469
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.12
_reflns_number_total             4469
_reflns_number_gt                3888
_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)+(0.0788P)²+4.6726P] 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     SHELXL
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4469
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1113
_refine_ls_wR_factor_gt          0.1074
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.724460(15) 1.73461(3) 0.911236(12) 0.02685(14) Uani 1 1 d . . .
S1 S 0.30850(11) 0.98546(18) 0.87607(8) 0.0309(4) Uani 1 1 d . . .
O3 O 0.3663(3) 0.4043(5) 0.6693(2) 0.0315(10) Uani 1 1 d . . .
O7 O 0.2214(3) 1.0701(6) 0.8687(2) 0.0385(11) Uani 1 1 d . . .
O8 O 0.3273(3) 0.8836(5) 0.9314(2) 0.0392(11) Uani 1 1 d . . .
N1 N 0.9022(4) 1.7993(7) 0.9454(3) 0.0309(12) Uani 1 1 d . . .
N2 N 0.8055(3) 1.6110(6) 1.0199(3) 0.0293(12) Uani 1 1 d . . .
C5 C 0.3997(4) 1.1229(7) 0.8775(3) 0.0280(13) Uani 1 1 d . . .
C3 C 0.5472(5) 1.2179(7) 0.9227(3) 0.0288(14) Uani 1 1 d . . .
H3 H 0.6022 1.2057 0.9498 0.035 Uiso 1 1 calc R . .
C11 C 0.3973(5) 0.7974(8) 0.7925(3) 0.0310(14) Uani 1 1 d . . .
H11 H 0.4530 0.8227 0.8168 0.037 Uiso 1 1 calc R . .
C24 C 0.9493(5) 1.7285(7) 0.9981(4) 0.0300(15) Uani 1 1 d . . .
C2 C 0.5302(4) 1.3533(7) 0.8884(3) 0.0285(14) Uani 1 1 d . . .
C12 C 0.3137(4) 0.8725(7) 0.8042(3) 0.0276(13) Uani 1 1 d . . .
C23 C 1.0467(5) 1.7485(7) 1.0139(4) 0.0355(17) Uani 1 1 d . . .
C4 C 0.4821(4) 1.0998(7) 0.9167(3) 0.0308(14) Uani 1 1 d . . .
H4 H 0.4936 1.0068 0.9386 0.037 Uiso 1 1 calc R . .
C1 C 0.5982(4) 1.4845(7) 0.8950(3) 0.0298(14) Uani 1 1 d . . .
C15 C 0.7558(5) 1.5298(8) 1.0601(3) 0.0332(15) Uani 1 1 d . . .
H15 H 0.6927 1.5136 1.0478 0.040 Uiso 1 1 calc R . .
C18 C 0.9425(5) 1.5695(8) 1.0975(3) 0.0340(15) Uani 1 1 d . . .
C8 C 0.3057(4) 0.5102(8) 0.6627(3) 0.0304(14) Uani 1 1 d . . .
C26 C 1.0419(5) 1.5903(8) 1.1116(4) 0.0401(17) Uani 1 1 d . . .
H26 H 1.0720 1.5454 1.1491 0.048 Uiso 1 1 calc R . .
C16 C 0.7942(5) 1.4679(8) 1.1202(3) 0.0373(16) Uani 1 1 d . . .
H16 H 0.7566 1.4153 1.1475 0.045 Uiso 1 1 calc R . .
C19 C 0.8979(4) 1.6338(7) 1.0399(3) 0.0297(14) Uani 1 1 d . . .
C6 C 0.3820(5) 1.2575(7) 0.8414(4) 0.0346(17) Uani 1 1 d . . .
H6 H 0.3272 1.2694 0.8140 0.042 Uiso 1 1 calc R . .
C14 C 0.2296(5) 0.7278(7) 0.7180(4) 0.0300(15) Uani 1 1 d . . .
H14 H 0.1745 0.7060 0.6923 0.036 Uiso 1 1 calc R . .
C13 C 0.2313(4) 0.8418(7) 0.7659(3) 0.0297(14) Uani 1 1 d . . .
H13 H 0.1775 0.8972 0.7723 0.036 Uiso 1 1 calc R . .
C7 C 0.4480(4) 1.3725(8) 0.8475(3) 0.0346(15) Uani 1 1 d . . .
H7 H 0.4377 1.4639 0.8241 0.042 Uiso 1 1 calc R . .
C9 C 0.3107(4) 0.6461(7) 0.7082(3) 0.0294(14) Uani 1 1 d . . .
C10 C 0.3948(4) 0.6852(8) 0.7441(3) 0.0298(14) Uani 1 1 d . . .
H10 H 0.4496 0.6353 0.7354 0.036 Uiso 1 1 calc R . .
C20 C 0.9504(5) 1.8855(8) 0.9067(4) 0.0378(16) Uani 1 1 d . . .
H20 H 0.9189 1.9326 0.8702 0.045 Uiso 1 1 calc R . .
C22 C 1.0949(5) 1.8425(8) 0.9715(4) 0.0394(17) Uani 1 1 d . . .
H22 H 1.1587 1.8587 0.9798 0.047 Uiso 1 1 calc R . .
C25 C 1.0917(5) 1.6740(9) 1.0712(4) 0.0387(17) Uani 1 1 d . . .
H25 H 1.1559 1.6834 1.0806 0.046 Uiso 1 1 calc R . .
C17 C 0.8876(5) 1.4857(8) 1.1384(3) 0.0374(16) Uani 1 1 d . . .
H17 H 0.9143 1.4426 1.1774 0.045 Uiso 1 1 calc R . .
C21 C 1.0469(5) 1.9086(8) 0.9185(4) 0.0402(17) Uani 1 1 d . . .
H21 H 1.0780 1.9695 0.8899 0.048 Uiso 1 1 calc R . .
O4 O 0.2360(3) 0.4981(5) 0.6195(2) 0.0326(10) Uani 1 1 d . . .
O2 O 0.5802(3) 1.6112(5) 0.8655(2) 0.0343(11) Uani 1 1 d . . .
O6 O 0.7815(3) 1.6564(5) 0.8457(2) 0.0342(11) Uani 1 1 d . . .
O1 O 0.6751(3) 1.4686(5) 0.9307(2) 0.0320(10) Uani 1 1 d . . .
O5 O 0.6631(3) 1.8151(6) 0.9735(2) 0.0354(10) Uani 1 1 d . . .
O1W O 0.9211(9) 1.6900(15) 0.7456(7) 0.145(4) Uani 1 1 d G . .
H1WA H 0.9458 1.7788 0.7493 0.218 Uiso 1 1 d G . .
H1WB H 0.8645 1.6954 0.7543 0.218 Uiso 1 1 d G . .


_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 O5 1.754(5) . ?
U1 O6 1.764(4) . ?
U1 O2 2.445(4) . ?
U1 O4 2.450(4) 2_666 ?
U1 O1 2.457(4) . ?
U1 O3 2.486(4) 2_666 ?
U1 N2 2.636(5) . ?
U1 N1 2.650(5) . ?
U1 C1 2.831(6) . ?
U1 C8 2.837(7) 2_666 ?
S1 O8 1.438(5) . ?
S1 O7 1.449(5) . ?
S1 C12 1.768(6) . ?
S1 C5 1.771(6) . ?
O3 C8 1.265(7) . ?
O3 U1 2.486(4) 2_636 ?
N1 C20 1.328(8) . ?
N1 C24 1.362(9) . ?
N2 C15 1.336(8) . ?
N2 C19 1.370(8) . ?
C5 C4 1.384(9) . ?
C5 C6 1.391(9) . ?
C3 C2 1.377(9) . ?
C3 C4 1.386(9) . ?
C11 C10 1.384(10) . ?
C11 C12 1.407(9) . ?
C24 C23 1.421(10) . ?
C24 C19 1.436(9) . ?
C2 C7 1.396(9) . ?
C2 C1 1.499(9) . ?
C12 C13 1.386(8) . ?
C23 C22 1.415(11) . ?
C23 C25 1.436(11) . ?
C1 O2 1.268(8) . ?
C1 O1 1.275(7) . ?
C15 C16 1.404(10) . ?
C18 C19 1.401(9) . ?
C18 C17 1.402(10) . ?
C18 C26 1.444(9) . ?
C8 O4 1.276(7) . ?
C8 C9 1.498(9) . ?
C8 U1 2.837(7) 2_636 ?
C26 C25 1.351(11) . ?
C16 C17 1.371(10) . ?
C6 C7 1.375(9) . ?
C14 C13 1.388(9) . ?
C14 C9 1.394(9) . ?
C9 C10 1.399(9) . ?
C20 C21 1.402(9) . ?
C22 C21 1.354(10) . ?
O4 U1 2.450(4) 2_636 ?

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
O5 U1 O6 177.12(19) . . ?
O5 U1 O2 89.10(19) . . ?
O6 U1 O2 88.89(18) . . ?
O5 U1 O4 87.53(19) . 2_666 ?
O6 U1 O4 91.76(19) . 2_666 ?
O2 U1 O4 121.32(14) . 2_666 ?
O5 U1 O1 94.92(19) . . ?
O6 U1 O1 85.52(18) . . ?
O2 U1 O1 53.27(14) . . ?
O4 U1 O1 173.90(14) 2_666 . ?
O5 U1 O3 88.43(18) . 2_666 ?
O6 U1 O3 88.91(18) . 2_666 ?
O2 U1 O3 68.29(15) . 2_666 ?
O4 U1 O3 53.06(14) 2_666 2_666 ?
O1 U1 O3 121.33(14) . 2_666 ?
O5 U1 N2 76.62(19) . . ?
O6 U1 N2 106.12(18) . . ?
O2 U1 N2 116.00(15) . . ?
O4 U1 N2 119.93(15) 2_666 . ?
O1 U1 N2 66.12(15) . . ?
O3 U1 N2 164.15(16) 2_666 . ?
O5 U1 N1 105.2(2) . . ?
O6 U1 N1 77.06(18) . . ?
O2 U1 N1 163.63(17) . . ?
O4 U1 N1 68.22(16) 2_666 . ?
O1 U1 N1 116.29(16) . . ?
O3 U1 N1 119.04(16) 2_666 . ?
N2 U1 N1 61.41(16) . . ?
O5 U1 C1 91.7(2) . . ?
O6 U1 C1 87.41(19) . . ?
O2 U1 C1 26.55(16) . . ?
O4 U1 C1 147.84(16) 2_666 . ?
O1 U1 C1 26.73(16) . . ?
O3 U1 C1 94.77(17) 2_666 . ?
N2 U1 C1 90.98(17) . . ?
N1 U1 C1 141.95(18) . . ?
O5 U1 C8 89.1(2) . 2_666 ?
O6 U1 C8 89.0(2) . 2_666 ?
O2 U1 C8 94.75(16) . 2_666 ?
O4 U1 C8 26.67(15) 2_666 2_666 ?
O1 U1 C8 147.57(16) . 2_666 ?
O3 U1 C8 26.46(15) 2_666 2_666 ?
N2 U1 C8 145.42(17) . 2_666 ?
N1 U1 C8 93.38(18) . 2_666 ?
C1 U1 C8 121.20(18) . 2_666 ?
O8 S1 O7 119.5(3) . . ?
O8 S1 C12 106.8(3) . . ?
O7 S1 C12 107.2(3) . . ?
O8 S1 C5 108.3(3) . . ?
O7 S1 C5 107.1(3) . . ?
C12 S1 C5 107.5(3) . . ?
C8 O3 U1 92.4(4) . 2_636 ?
C20 N1 C24 118.1(6) . . ?
C20 N1 U1 120.5(4) . . ?
C24 N1 U1 120.8(4) . . ?
C15 N2 C19 116.9(6) . . ?
C15 N2 U1 120.5(4) . . ?
C19 N2 U1 122.4(4) . . ?
C4 C5 C6 122.2(6) . . ?
C4 C5 S1 120.5(5) . . ?
C6 C5 S1 117.2(5) . . ?
C2 C3 C4 119.9(6) . . ?
C10 C11 C12 118.6(6) . . ?
N1 C24 C23 122.4(6) . . ?
N1 C24 C19 118.6(6) . . ?
C23 C24 C19 119.0(7) . . ?
C3 C2 C7 120.4(6) . . ?
C3 C2 C1 121.2(6) . . ?
C7 C2 C1 118.4(6) . . ?
C13 C12 C11 121.1(6) . . ?
C13 C12 S1 118.3(5) . . ?
C11 C12 S1 119.9(5) . . ?
C22 C23 C24 117.4(7) . . ?
C22 C23 C25 123.0(7) . . ?
C24 C23 C25 119.6(7) . . ?
C5 C4 C3 118.8(6) . . ?
O2 C1 O1 119.5(6) . . ?
O2 C1 C2 120.8(6) . . ?
O1 C1 C2 119.7(6) . . ?
O2 C1 U1 59.5(3) . . ?
O1 C1 U1 60.1(3) . . ?
C2 C1 U1 178.3(5) . . ?
N2 C15 C16 123.0(6) . . ?
C19 C18 C17 117.6(6) . . ?
C19 C18 C26 119.2(6) . . ?
C17 C18 C26 123.2(6) . . ?
O3 C8 O4 120.4(6) . . ?
O3 C8 C9 120.7(6) . . ?
O4 C8 C9 118.8(6) . . ?
O3 C8 U1 61.1(3) . 2_636 ?
O4 C8 U1 59.5(3) . 2_636 ?
C9 C8 U1 171.1(4) . 2_636 ?
C25 C26 C18 121.1(7) . . ?
C17 C16 C15 119.5(7) . . ?
N2 C19 C18 123.5(6) . . ?
N2 C19 C24 116.3(6) . . ?
C18 C19 C24 120.2(6) . . ?
C7 C6 C5 118.0(7) . . ?
C13 C14 C9 120.0(6) . . ?
C12 C13 C14 119.5(6) . . ?
C6 C7 C2 120.6(6) . . ?
C14 C9 C10 119.9(6) . . ?
C14 C9 C8 119.6(6) . . ?
C10 C9 C8 120.3(6) . . ?
C11 C10 C9 120.5(6) . . ?
N1 C20 C21 122.8(7) . . ?
C21 C22 C23 119.2(6) . . ?
C26 C25 C23 120.7(6) . . ?
C16 C17 C18 119.3(6) . . ?
C22 C21 C20 120.1(7) . . ?
C8 O4 U1 93.8(4) . 2_636 ?
C1 O2 U1 93.9(4) . . ?
C1 O1 U1 93.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.12
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.397
_refine_diff_density_min         -2.247
_refine_diff_density_rms         0.170
_exptl_crystal_recrystallization_method hydrothemal
_chemical_properties_physical    'Heat-sensitive, Light-sensitive'
_exptl_crystal_preparation       Luminescent
