# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 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_apx1494
_database_code_depnum_ccdc_archive 'CCDC 913827'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31.50 H28 Cl N2 O5 S6 U'
_chemical_formula_weight         980.40
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'
Cl Cl 0.1484 0.1585 '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                   9.7141(6)
_cell_length_b                   12.0383(7)
_cell_length_c                   16.5610(1)
_cell_angle_alpha                82.0100(1)
_cell_angle_beta                 75.0980(1)
_cell_angle_gamma                68.0900(1)
_cell_volume                     1734.35(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    5.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      120(1)
_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  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19573
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         28.36
_reflns_number_total             7907
_reflns_number_gt                7304
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+2.2549P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7907
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Cl1 Cl 0.9442(2) 0.6602(2) 0.01263(12) 0.0351(4) Uani 0.50 1 d P . .
U1 U 0.570972(13) -0.128410(10) 0.655925(7) 0.01260(4) Uani 1 1 d . . .
S1 S 0.52414(9) 0.26713(7) 0.96074(5) 0.01799(16) Uani 1 1 d . . .
S2 S 0.78390(9) 0.04984(7) 0.99177(5) 0.01609(16) Uani 1 1 d . . .
S3 S 0.59898(10) 0.41059(7) 1.08729(5) 0.01978(17) Uani 1 1 d . . .
S4 S 0.85146(9) 0.19173(7) 1.11897(5) 0.01873(17) Uani 1 1 d . . .
S5 S 0.64606(9) 0.55222(8) 1.20768(5) 0.02183(18) Uani 1 1 d . . .
S6 S 0.93949(9) 0.30771(8) 1.23588(5) 0.02087(17) Uani 1 1 d . . .
N1 N 0.4067(3) 0.0121(2) 0.77295(15) 0.0141(5) Uani 1 1 d . . .
N2 N 0.6467(3) -0.1781(2) 0.79552(16) 0.0139(5) Uani 1 1 d . . .
O1 O 0.6873(2) -0.0389(2) 0.62136(14) 0.0182(5) Uani 1 1 d . . .
O2 O 0.4527(2) -0.2154(2) 0.69407(13) 0.0178(5) Uani 1 1 d . . .
O3 O 0.3726(2) 0.0248(2) 0.61051(13) 0.0168(5) Uani 1 1 d . . .
O4 O 0.7775(2) -0.29562(19) 0.64882(13) 0.0179(5) Uani 1 1 d . . .
O5 O 0.6111(3) -0.1840(2) 0.51272(14) 0.0189(5) Uani 1 1 d . . .
C1 C 0.2248(4) 0.0489(3) 0.64473(19) 0.0159(6) Uani 1 1 d . . .
C2 C 0.1225(4) 0.0638(3) 0.5941(2) 0.0183(7) Uani 1 1 d . . .
H2 H 0.1576 0.0597 0.5364 0.022 Uiso 1 1 calc R . .
C3 C -0.0304(4) 0.0848(3) 0.6296(2) 0.0204(7) Uani 1 1 d . . .
H3 H -0.0965 0.0932 0.5954 0.024 Uiso 1 1 calc R . .
C4 C -0.0864(4) 0.0934(3) 0.7158(2) 0.0218(7) Uani 1 1 d . . .
H4 H -0.1883 0.1049 0.7393 0.026 Uiso 1 1 calc R . .
C5 C 0.0110(4) 0.0846(3) 0.7654(2) 0.0175(7) Uani 1 1 d . . .
H5 H -0.0269 0.0932 0.8226 0.021 Uiso 1 1 calc R . .
C6 C 0.1676(3) 0.0628(3) 0.73170(19) 0.0142(6) Uani 1 1 d . . .
C7 C 0.2606(4) 0.0609(3) 0.78808(19) 0.0153(6) Uani 1 1 d . . .
C8 C 0.8114(3) -0.3954(3) 0.6957(2) 0.0155(6) Uani 1 1 d . . .
C9 C 0.8954(4) -0.5066(3) 0.6588(2) 0.0193(7) Uani 1 1 d . . .
H9 H 0.9230 -0.5097 0.6008 0.023 Uiso 1 1 calc R . .
C10 C 0.9371(4) -0.6108(3) 0.7077(2) 0.0229(7) Uani 1 1 d . . .
H10 H 0.9935 -0.6831 0.6821 0.028 Uiso 1 1 calc R . .
C11 C 0.8964(4) -0.6098(3) 0.7948(2) 0.0242(8) Uani 1 1 d . . .
H11 H 0.9232 -0.6809 0.8271 0.029 Uiso 1 1 calc R . .
C12 C 0.8160(4) -0.5023(3) 0.8323(2) 0.0199(7) Uani 1 1 d . . .
H12 H 0.7907 -0.5010 0.8903 0.024 Uiso 1 1 calc R . .
C13 C 0.7711(4) -0.3935(3) 0.7843(2) 0.0160(6) Uani 1 1 d . . .
C14 C 0.7065(3) -0.2838(3) 0.82832(19) 0.0157(6) Uani 1 1 d . . .
C15 C 0.7058(5) -0.2992(3) 0.4806(3) 0.0409(11) Uani 1 1 d . . .
H15A H 0.8075 -0.3177 0.4872 0.061 Uiso 1 1 calc R . .
H15B H 0.7071 -0.2980 0.4223 0.061 Uiso 1 1 calc R . .
H15C H 0.6664 -0.3590 0.5107 0.061 Uiso 1 1 calc R . .
C16 C 0.4872(3) 0.0239(3) 0.82973(18) 0.0142(6) Uani 1 1 d . . .
C17 C 0.6132(3) -0.0775(3) 0.84241(18) 0.0140(6) Uani 1 1 d . . .
C18 C 0.4526(4) 0.1302(3) 0.86793(19) 0.0152(6) Uani 1 1 d . . .
H18 H 0.3691 0.1972 0.8599 0.018 Uiso 1 1 calc R . .
C19 C 0.7026(3) -0.0731(3) 0.89415(18) 0.0145(6) Uani 1 1 d . . .
H19 H 0.7847 -0.1405 0.9036 0.017 Uiso 1 1 calc R . .
C20 C 0.5451(4) 0.1342(3) 0.91825(18) 0.0140(6) Uani 1 1 d . . .
C21 C 0.6685(3) 0.0329(3) 0.93169(18) 0.0142(6) Uani 1 1 d . . .
C22 C 0.6691(4) 0.1986(3) 1.01648(19) 0.0165(6) Uani 1 1 d . . .
C23 C 0.6989(4) 0.2578(3) 1.06876(19) 0.0170(6) Uani 1 1 d . . .
C24 C 0.6929(4) 0.4152(3) 1.1636(2) 0.0173(7) Uani 1 1 d . . .
C25 C 0.8098(4) 0.3163(3) 1.17728(19) 0.0169(6) Uani 1 1 d . . .
C26 C 0.4457(4) 0.5863(4) 1.2585(2) 0.0322(9) Uani 1 1 d . . .
H26A H 0.3834 0.6478 1.2253 0.039 Uiso 1 1 calc R . .
H26B H 0.4199 0.5151 1.2619 0.039 Uiso 1 1 calc R . .
C27 C 0.4122(5) 0.6289(4) 1.3450(2) 0.0354(9) Uani 1 1 d . . .
H27A H 0.4676 0.5639 1.3792 0.042 Uiso 1 1 calc R . .
H27B H 0.3044 0.6481 1.3695 0.042 Uiso 1 1 calc R . .
C28 C 0.4531(5) 0.7367(4) 1.3481(3) 0.0376(10) Uani 1 1 d . . .
H28A H 0.5610 0.7169 1.3282 0.056 Uiso 1 1 calc R . .
H28B H 0.4237 0.7609 1.4048 0.056 Uiso 1 1 calc R . .
H28C H 0.4008 0.8012 1.3135 0.056 Uiso 1 1 calc R . .
C29 C 0.8904(4) 0.2167(3) 1.3279(2) 0.0256(8) Uani 1 1 d . . .
H29A H 0.8622 0.1554 1.3112 0.031 Uiso 1 1 calc R . .
H29B H 0.9793 0.1766 1.3515 0.031 Uiso 1 1 calc R . .
C30 C 0.7605(5) 0.2889(4) 1.3947(2) 0.0364(10) Uani 1 1 d . . .
H30A H 0.7345 0.2346 1.4398 0.044 Uiso 1 1 calc R . .
H30B H 0.6720 0.3296 1.3709 0.044 Uiso 1 1 calc R . .
C31 C 0.7977(6) 0.3816(4) 1.4305(3) 0.0497(13) Uani 1 1 d . . .
H31A H 0.8864 0.3423 1.4532 0.075 Uiso 1 1 calc R . .
H31B H 0.7132 0.4218 1.4739 0.075 Uiso 1 1 calc R . .
H31C H 0.8168 0.4390 1.3869 0.075 Uiso 1 1 calc R . .
C32 C 0.9375(8) 0.5147(7) 0.0457(5) 0.0274(16) Uani 0.50 1 d P . .
Cl2 Cl 0.9093(2) 0.5947(2) 0.01594(13) 0.0367(5) Uani 0.50 1 d P . .
H5A H 0.608(6) -0.131(5) 0.473(4) 0.080 Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0334(11) 0.0344(11) 0.0315(10) 0.0120(8) -0.0074(8) -0.0099(9)
U1 0.01251(6) 0.01250(6) 0.01118(6) -0.00153(4) -0.00116(4) -0.00325(4)
S1 0.0215(4) 0.0126(4) 0.0188(4) -0.0038(3) -0.0078(3) -0.0017(3)
S2 0.0178(4) 0.0139(4) 0.0162(4) -0.0032(3) -0.0053(3) -0.0032(3)
S3 0.0223(4) 0.0150(4) 0.0219(4) -0.0057(3) -0.0084(3) -0.0025(3)
S4 0.0206(4) 0.0147(4) 0.0211(4) -0.0044(3) -0.0076(3) -0.0033(3)
S5 0.0184(4) 0.0194(4) 0.0276(5) -0.0121(3) -0.0013(3) -0.0051(3)
S6 0.0193(4) 0.0260(4) 0.0206(4) -0.0039(3) -0.0052(3) -0.0102(4)
N1 0.0160(13) 0.0129(13) 0.0114(12) -0.0004(10) -0.0021(10) -0.0035(11)
N2 0.0116(12) 0.0140(13) 0.0146(13) -0.0047(10) -0.0008(10) -0.0028(10)
O1 0.0168(11) 0.0188(12) 0.0188(12) -0.0026(9) -0.0021(9) -0.0066(9)
O2 0.0196(12) 0.0192(12) 0.0159(11) 0.0001(9) -0.0024(9) -0.0095(10)
O3 0.0146(11) 0.0203(12) 0.0134(11) -0.0004(9) -0.0020(9) -0.0044(9)
O4 0.0190(12) 0.0144(11) 0.0153(11) -0.0017(9) -0.0010(9) -0.0018(9)
O5 0.0235(12) 0.0174(12) 0.0133(11) -0.0027(9) -0.0022(9) -0.0050(10)
C1 0.0177(16) 0.0131(15) 0.0152(15) 0.0017(12) -0.0026(12) -0.0052(13)
C2 0.0190(16) 0.0164(16) 0.0175(16) 0.0024(12) -0.0056(13) -0.0041(13)
C3 0.0186(16) 0.0207(17) 0.0233(17) 0.0025(13) -0.0098(14) -0.0064(14)
C4 0.0131(16) 0.0202(17) 0.0284(18) 0.0035(14) -0.0039(13) -0.0040(13)
C5 0.0167(16) 0.0143(15) 0.0173(16) 0.0041(12) -0.0013(12) -0.0042(13)
C6 0.0156(15) 0.0075(14) 0.0167(15) 0.0015(11) -0.0037(12) -0.0018(12)
C7 0.0161(15) 0.0112(14) 0.0167(15) 0.0033(12) -0.0043(12) -0.0035(12)
C8 0.0121(15) 0.0151(15) 0.0209(16) -0.0023(12) -0.0043(12) -0.0056(12)
C9 0.0182(16) 0.0193(16) 0.0189(16) -0.0064(13) -0.0017(13) -0.0044(14)
C10 0.0200(17) 0.0164(16) 0.0283(19) -0.0072(14) -0.0033(14) -0.0012(14)
C11 0.0289(19) 0.0113(16) 0.0286(19) 0.0022(13) -0.0095(15) -0.0021(14)
C12 0.0240(18) 0.0161(16) 0.0188(16) 0.0003(13) -0.0083(14) -0.0044(14)
C13 0.0138(15) 0.0147(15) 0.0209(16) -0.0013(12) -0.0052(12) -0.0054(13)
C14 0.0128(15) 0.0158(15) 0.0172(16) -0.0007(12) -0.0041(12) -0.0033(12)
C15 0.061(3) 0.025(2) 0.029(2) -0.0108(16) -0.017(2) 0.002(2)
C16 0.0160(15) 0.0149(15) 0.0103(14) -0.0013(11) -0.0016(12) -0.0046(12)
C17 0.0157(15) 0.0150(15) 0.0092(14) -0.0011(11) 0.0003(11) -0.0048(12)
C18 0.0163(15) 0.0138(15) 0.0128(15) -0.0001(12) -0.0018(12) -0.0036(13)
C19 0.0149(15) 0.0130(15) 0.0142(15) -0.0001(12) -0.0036(12) -0.0033(12)
C20 0.0197(16) 0.0133(15) 0.0093(14) -0.0026(11) -0.0007(12) -0.0072(13)
C21 0.0147(15) 0.0153(15) 0.0109(14) -0.0013(11) -0.0025(12) -0.0032(12)
C22 0.0168(16) 0.0153(15) 0.0142(15) -0.0025(12) -0.0023(12) -0.0021(13)
C23 0.0161(16) 0.0151(15) 0.0163(16) -0.0003(12) -0.0025(12) -0.0025(13)
C24 0.0177(16) 0.0178(16) 0.0182(16) -0.0042(13) -0.0023(13) -0.0080(13)
C25 0.0181(16) 0.0206(16) 0.0134(15) -0.0038(12) 0.0007(12) -0.0103(14)
C26 0.0221(19) 0.036(2) 0.038(2) -0.0192(18) 0.0059(16) -0.0128(17)
C27 0.031(2) 0.036(2) 0.031(2) -0.0059(17) 0.0022(17) -0.0072(18)
C28 0.031(2) 0.043(2) 0.036(2) -0.0222(19) -0.0047(18) -0.0050(19)
C29 0.036(2) 0.0190(17) 0.0277(19) 0.0064(14) -0.0171(16) -0.0123(16)
C30 0.050(3) 0.046(3) 0.0219(19) -0.0037(17) -0.0003(18) -0.031(2)
C31 0.066(3) 0.061(3) 0.031(2) -0.022(2) 0.010(2) -0.040(3)
C32 0.024(4) 0.032(4) 0.025(4) 0.011(3) -0.004(3) -0.014(3)
Cl2 0.0342(11) 0.0396(13) 0.0309(11) -0.0034(10) -0.0050(9) -0.0078(10)
_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
Cl1 Cl2 0.958(3) . ?
Cl1 C32 1.782(8) . ?
Cl1 C32 2.208(9) 2_765 ?
U1 O2 1.776(2) . ?
U1 O1 1.780(2) . ?
U1 O4 2.241(2) . ?
U1 O3 2.322(2) . ?
U1 O5 2.449(2) . ?
U1 N2 2.531(3) . ?
U1 N1 2.544(2) . ?
S1 C20 1.759(3) . ?
S1 C22 1.762(3) . ?
S2 C21 1.758(3) . ?
S2 C22 1.760(3) . ?
S3 C24 1.756(3) . ?
S3 C23 1.758(3) . ?
S4 C23 1.758(3) . ?
S4 C25 1.759(3) . ?
S5 C24 1.750(3) . ?
S5 C26 1.823(4) . ?
S6 C25 1.744(3) . ?
S6 C29 1.818(4) . ?
N1 C7 1.287(4) . ?
N1 C16 1.419(4) . ?
N2 C14 1.293(4) . ?
N2 C17 1.418(4) . ?
O3 C1 1.335(4) . ?
O4 C8 1.316(4) . ?
O5 C15 1.433(4) . ?
O5 O3 2.615(3) 2_656 ?
C1 C2 1.406(4) . ?
C1 C6 1.413(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.394(5) . ?
C4 C5 1.371(5) . ?
C5 C6 1.414(4) . ?
C6 C7 1.450(4) . ?
C8 C9 1.410(4) . ?
C8 C13 1.419(4) . ?
C9 C10 1.378(5) . ?
C10 C11 1.395(5) . ?
C11 C12 1.375(4) . ?
C12 C13 1.413(4) . ?
C13 C14 1.443(4) . ?
C16 C18 1.395(4) . ?
C16 C17 1.407(4) . ?
C17 C19 1.386(4) . ?
C18 C20 1.390(4) . ?
C19 C21 1.387(4) . ?
C20 C21 1.395(4) . ?
C20 C19 3.581(4) 2_657 ?
C22 C23 1.340(4) . ?
C24 C25 1.344(5) . ?
C26 C27 1.504(5) . ?
C27 C28 1.503(6) . ?
C29 C30 1.517(5) . ?
C30 C31 1.523(5) . ?
C32 Cl2 0.993(8) . ?
C32 C32 1.665(14) 2_765 ?
C32 Cl2 1.766(8) 2_765 ?
C32 Cl1 2.208(9) 2_765 ?
Cl2 C32 1.767(8) 2_765 ?
Cl2 Cl2 2.333(4) 2_765 ?
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
Cl2 Cl1 C32 24.5(3) . . ?
Cl2 Cl1 C32 50.8(2) . 2_765 ?
C32 Cl1 C32 47.9(4) . 2_765 ?
O2 U1 O1 177.90(10) . . ?
O2 U1 O4 89.88(9) . . ?
O1 U1 O4 90.89(9) . . ?
O2 U1 O3 90.69(9) . . ?
O1 U1 O3 89.34(9) . . ?
O4 U1 O3 157.67(8) . . ?
O2 U1 O5 90.79(9) . . ?
O1 U1 O5 91.28(9) . . ?
O4 U1 O5 78.93(8) . . ?
O3 U1 O5 78.75(8) . . ?
O2 U1 N2 86.71(9) . . ?
O1 U1 N2 91.72(9) . . ?
O4 U1 N2 69.98(8) . . ?
O3 U1 N2 132.33(8) . . ?
O5 U1 N2 148.80(8) . . ?
O2 U1 N1 87.22(9) . . ?
O1 U1 N1 90.82(9) . . ?
O4 U1 N1 133.06(8) . . ?
O3 U1 N1 69.26(8) . . ?
O5 U1 N1 147.90(8) . . ?
N2 U1 N1 63.08(8) . . ?
C20 S1 C22 95.16(15) . . ?
C21 S2 C22 95.16(15) . . ?
C24 S3 C23 95.44(15) . . ?
C23 S4 C25 95.71(15) . . ?
C24 S5 C26 102.28(16) . . ?
C25 S6 C29 102.77(16) . . ?
C7 N1 C16 119.7(3) . . ?
C7 N1 U1 125.6(2) . . ?
C16 N1 U1 114.31(18) . . ?
C14 N2 C17 118.2(3) . . ?
C14 N2 U1 126.8(2) . . ?
C17 N2 U1 114.95(18) . . ?
C1 O3 U1 125.28(18) . . ?
C8 O4 U1 133.59(19) . . ?
C15 O5 U1 124.9(2) . . ?
C15 O5 O3 107.1(2) . 2_656 ?
U1 O5 O3 119.10(10) . 2_656 ?
O3 C1 C2 120.2(3) . . ?
O3 C1 C6 121.0(3) . . ?
C2 C1 C6 118.8(3) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 120.9(3) . . ?
C5 C4 C3 119.1(3) . . ?
C4 C5 C6 121.7(3) . . ?
C1 C6 C5 118.9(3) . . ?
C1 C6 C7 123.1(3) . . ?
C5 C6 C7 118.0(3) . . ?
N1 C7 C6 124.6(3) . . ?
O4 C8 C9 120.4(3) . . ?
O4 C8 C13 121.1(3) . . ?
C9 C8 C13 118.4(3) . . ?
C10 C9 C8 120.7(3) . . ?
C9 C10 C11 121.3(3) . . ?
C12 C11 C10 119.1(3) . . ?
C11 C12 C13 121.3(3) . . ?
C12 C13 C8 119.2(3) . . ?
C12 C13 C14 117.3(3) . . ?
C8 C13 C14 122.8(3) . . ?
N2 C14 C13 125.1(3) . . ?
C18 C16 C17 120.4(3) . . ?
C18 C16 N1 123.6(3) . . ?
C17 C16 N1 115.9(3) . . ?
C19 C17 C16 120.1(3) . . ?
C19 C17 N2 123.5(3) . . ?
C16 C17 N2 116.2(3) . . ?
C20 C18 C16 118.9(3) . . ?
C21 C19 C17 119.4(3) . . ?
C18 C20 C21 120.5(3) . . ?
C18 C20 S1 122.8(2) . . ?
C21 C20 S1 116.5(2) . . ?
C18 C20 C19 92.77(19) . 2_657 ?
C21 C20 C19 92.97(19) . 2_657 ?
S1 C20 C19 88.74(12) . 2_657 ?
C19 C21 C20 120.7(3) . . ?
C19 C21 S2 122.4(2) . . ?
C20 C21 S2 116.8(2) . . ?
C23 C22 S2 121.8(3) . . ?
C23 C22 S1 122.8(2) . . ?
S2 C22 S1 115.17(18) . . ?
C22 C23 S3 123.3(3) . . ?
C22 C23 S4 122.6(2) . . ?
S3 C23 S4 113.93(18) . . ?
C25 C24 S5 123.4(3) . . ?
C25 C24 S3 117.5(2) . . ?
S5 C24 S3 118.58(19) . . ?
C24 C25 S6 125.6(3) . . ?
C24 C25 S4 116.7(2) . . ?
S6 C25 S4 117.00(19) . . ?
C27 C26 S5 111.0(3) . . ?
C26 C27 C28 114.4(3) . . ?
C30 C29 S6 113.1(3) . . ?
C29 C30 C31 113.4(3) . . ?
Cl2 C32 C32 78.9(6) . 2_765 ?
Cl2 C32 Cl2 112.4(6) . 2_765 ?
C32 C32 Cl2 33.5(4) 2_765 2_765 ?
Cl2 C32 Cl1 23.6(3) . . ?
C32 C32 Cl1 79.6(5) 2_765 . ?
Cl2 C32 Cl1 110.2(4) 2_765 . ?
Cl2 C32 Cl1 126.4(6) . 2_765 ?
C32 C32 Cl1 52.5(5) 2_765 2_765 ?
Cl2 C32 Cl1 24.87(15) 2_765 2_765 ?
Cl1 C32 Cl1 132.1(4) . 2_765 ?
Cl1 Cl2 C32 131.9(5) . . ?
Cl1 Cl2 C32 104.3(3) . 2_765 ?
C32 Cl2 C32 67.6(6) . 2_765 ?
Cl1 Cl2 Cl2 118.1(2) . 2_765 ?
C32 Cl2 Cl2 44.4(4) . 2_765 ?
C32 Cl2 Cl2 23.2(2) 2_765 2_765 ?
_diffrn_measured_fraction_theta_max 0.911
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.106
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0