# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'F Cloke'
'Alistair S Frey'
'Peter B Hitchcock'
'Owen T Summerscales'

_publ_contact_author_name        'F Cloke'
_publ_contact_author_email       F.G.CLOKE@SUSSEX.AC.UK

_publ_section_title              
;
Reductive Disproportionation of Carbon Dioxide to
Carbonate and Squarate Products Using A Mixed-Sandwich U(III) Complex
;
_publ_requested_category         FM

# Attachment 'apr1906.cif'

data_apr1906
_database_code_depnum_ccdc_archive 'CCDC 701455'

_audit_creation_date             2006-04-25T11:26:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C71 H122 O3 Si4 U2, C4 H10 O'
_chemical_formula_sum            'C75 H132 O4 Si4 U2'
_chemical_formula_weight         1686.23
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5128(6)
_cell_length_b                   13.7949(6)
_cell_length_c                   15.4698(7)
_cell_angle_alpha                66.040(3)
_cell_angle_beta                 76.536(3)
_cell_angle_gamma                73.608(3)
_cell_volume                     1948.86(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    56288
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      26.022
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             854
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_T_max  0.7685

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.606106E-1
_diffrn_orient_matrix_ub_12      -0.154785E-1
_diffrn_orient_matrix_ub_13      0.621159E-1
_diffrn_orient_matrix_ub_21      0.795321E-1
_diffrn_orient_matrix_ub_22      -0.298476E-1
_diffrn_orient_matrix_ub_23      0.351588E-1
_diffrn_orient_matrix_ub_31      -0.37783E-2
_diffrn_orient_matrix_ub_32      0.738634E-1
_diffrn_orient_matrix_ub_33      -0.1393E-2
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_number            29815
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_full        26.13
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_reflns_number_total             7612
_reflns_number_gt                6388
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
The carbonate anion bridging the two U atoms is disordered across the inversion
centre and its atoms had to be left isotropic.
The Et2O solvate disordered across an inversion centre was left isotropic and
with its H atoms omitted.

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^)+(0.0302P)^2^+13.4507P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7612
_refine_ls_number_parameters     375
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1081
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         5.338
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.141

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

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 0.64567(3) 0.36516(2) 0.683248(19) 0.03549(10) Uani 1 1 d . . .
Si1 Si 0.3056(2) 0.52596(17) 0.83795(14) 0.0381(5) Uani 1 1 d . A 1
Si2 Si 0.5521(2) 0.06114(17) 0.71841(15) 0.0407(5) Uani 1 1 d . A 1
O1 O 0.5738(10) 0.3953(9) 0.5349(7) 0.037(2) Uiso 0.5 1 d P . 1
O2 O 0.5220(10) 0.5342(8) 0.5807(7) 0.042(2) Uiso 0.5 1 d P . 1
O3 O 0.4508(12) 0.5531(11) 0.4495(8) 0.047(3) Uiso 0.5 1 d P . 1
C1 C 0.508(2) 0.5002(18) 0.5226(12) 0.048(4) Uiso 0.5 1 d P . 1
C2 C 0.4372(7) 0.4113(6) 0.8116(5) 0.0362(16) Uani 1 1 d . A 1
C3 C 0.3941(8) 0.3562(6) 0.7673(5) 0.0351(16) Uani 1 1 d . A 1
H3 H 0.3076 0.392 0.7491 0.042 Uiso 1 1 calc R A 1
C4 C 0.4438(8) 0.2631(6) 0.7425(5) 0.0367(17) Uani 1 1 d . A 1
H4 H 0.3825 0.2554 0.7105 0.044 Uiso 1 1 calc R A 1
C5 C 0.5595(8) 0.1777(6) 0.7519(5) 0.0357(16) Uani 1 1 d . A 1
C6 C 0.6731(8) 0.1575(6) 0.7959(5) 0.0387(17) Uani 1 1 d . A 1
H6 H 0.738 0.0963 0.7892 0.046 Uiso 1 1 calc R A 1
C7 C 0.7144(8) 0.2048(6) 0.8470(5) 0.0417(18) Uani 1 1 d . A 1
H7 H 0.7953 0.163 0.8721 0.05 Uiso 1 1 calc R A 1
C8 C 0.6662(8) 0.2979(6) 0.8699(5) 0.0413(18) Uani 1 1 d . A 1
H8 H 0.7232 0.3041 0.906 0.05 Uiso 1 1 calc R A 1
C9 C 0.5537(8) 0.3853(6) 0.8530(5) 0.0423(18) Uani 1 1 d . A 1
H9 H 0.5582 0.4393 0.8748 0.051 Uiso 1 1 calc R A 1
C10 C 0.3883(9) 0.6238(6) 0.8523(6) 0.048(2) Uani 1 1 d . A 1
H10 H 0.441 0.5802 0.9069 0.058 Uiso 1 1 calc R A 1
C11 C 0.4894(10) 0.6729(8) 0.7658(7) 0.066(3) Uani 1 1 d . A 1
H11A H 0.5548 0.6143 0.7494 0.1 Uiso 1 1 calc R A 1
H11B H 0.5358 0.7145 0.7819 0.1 Uiso 1 1 calc R A 1
H11C H 0.4416 0.7209 0.7111 0.1 Uiso 1 1 calc R A 1
C12 C 0.2862(10) 0.7137(8) 0.8810(7) 0.064(3) Uani 1 1 d . A 1
H12A H 0.2242 0.681 0.9368 0.095 Uiso 1 1 calc R A 1
H12B H 0.2359 0.7622 0.8278 0.095 Uiso 1 1 calc R A 1
H12C H 0.3332 0.7552 0.8968 0.095 Uiso 1 1 calc R A 1
C13 C 0.1801(9) 0.5956(7) 0.7487(6) 0.048(2) Uani 1 1 d . A 1
H13 H 0.1646 0.5379 0.7314 0 Uiso 1 1 calc R A 1
C14 C 0.2315(11) 0.6801(8) 0.6554(6) 0.067(3) Uani 1 1 d . A 1
H14A H 0.318 0.6466 0.6282 0.101 Uiso 1 1 calc R A 1
H14B H 0.2424 0.7409 0.6686 0.101 Uiso 1 1 calc R A 1
H14C H 0.167 0.7068 0.61 0.101 Uiso 1 1 calc R A 1
C15 C 0.0456(9) 0.6469(8) 0.7898(7) 0.062(2) Uani 1 1 d . A 1
H15A H 0.0122 0.5928 0.8489 0.093 Uiso 1 1 calc R A 1
H15B H -0.0177 0.6735 0.7436 0.093 Uiso 1 1 calc R A 1
H15C H 0.0552 0.7077 0.8036 0.093 Uiso 1 1 calc R A 1
C16 C 0.2122(8) 0.4572(6) 0.9598(5) 0.0419(18) Uani 1 1 d . A 1
H16 H 0.1354 0.5135 0.9733 0 Uiso 1 1 calc R A 1
C17 C 0.1536(9) 0.3680(7) 0.9588(6) 0.053(2) Uani 1 1 d . A 1
H17A H 0.0985 0.3983 0.9069 0.08 Uiso 1 1 calc R A 1
H17B H 0.0982 0.3393 1.0199 0.08 Uiso 1 1 calc R A 1
H17C H 0.2265 0.3095 0.9488 0.08 Uiso 1 1 calc R A 1
C18 C 0.2968(9) 0.4123(8) 1.0407(6) 0.060(2) Uani 1 1 d . A 1
H18A H 0.3325 0.4705 1.041 0.089 Uiso 1 1 calc R A 1
H18B H 0.371 0.3542 1.0314 0.089 Uiso 1 1 calc R A 1
H18C H 0.2413 0.3834 1.1017 0.089 Uiso 1 1 calc R A 1
C19 C 0.4931(10) -0.0445(7) 0.8346(6) 0.056(2) Uani 1 1 d . A 1
H19 H 0.4836 -0.1053 0.8188 0 Uiso 1 1 calc R A 1
C20 C 0.3555(11) 0.0008(8) 0.8785(7) 0.073(3) Uani 1 1 d . A 1
H20A H 0.2932 0.0313 0.8311 0.11 Uiso 1 1 calc R A 1
H20B H 0.3619 0.0579 0.8987 0.11 Uiso 1 1 calc R A 1
H20C H 0.3227 -0.0575 0.934 0.11 Uiso 1 1 calc R A 1
C21 C 0.5885(12) -0.0927(8) 0.9080(7) 0.080(3) Uani 1 1 d . A 1
H21A H 0.6767 -0.1227 0.8801 0.12 Uiso 1 1 calc R A 1
H21B H 0.5546 -0.1506 0.9634 0.12 Uiso 1 1 calc R A 1
H21C H 0.5961 -0.0361 0.9283 0.12 Uiso 1 1 calc R A 1
C22 C 0.4233(9) 0.1046(7) 0.6348(6) 0.053(2) Uani 1 1 d . A 1
H22 H 0.3433 0.1497 0.6605 0 Uiso 1 1 calc R A 1
C23 C 0.4642(12) 0.1775(8) 0.5324(7) 0.072(3) Uani 1 1 d . A 1
H23A H 0.4944 0.2381 0.5333 0.108 Uiso 1 1 calc R A 1
H23B H 0.3874 0.2058 0.497 0.108 Uiso 1 1 calc R A 1
H23C H 0.5371 0.1353 0.5014 0.108 Uiso 1 1 calc R A 1
C24 C 0.3741(11) 0.0098(8) 0.6346(8) 0.072(3) Uani 1 1 d . A 1
H24A H 0.347 -0.0358 0.7005 0.107 Uiso 1 1 calc R A 1
H24B H 0.4465 -0.0335 0.6044 0.107 Uiso 1 1 calc R A 1
H24C H 0.2975 0.0384 0.5989 0.107 Uiso 1 1 calc R A 1
C25 C 0.7247(9) -0.0007(7) 0.6697(6) 0.053(2) Uani 1 1 d . A 1
H25 H 0.7819 -0.0237 0.7209 0 Uiso 1 1 calc R A 1
C26 C 0.7928(11) 0.0780(9) 0.5813(8) 0.083(3) Uani 1 1 d . A 1
H26A H 0.7894 0.1434 0.593 0.124 Uiso 1 1 calc R A 1
H26B H 0.7462 0.0978 0.5266 0.124 Uiso 1 1 calc R A 1
H26C H 0.8863 0.0431 0.5677 0.124 Uiso 1 1 calc R A 1
C27 C 0.7309(11) -0.1041(8) 0.6529(9) 0.080(3) Uani 1 1 d . A 1
H27A H 0.6888 -0.1547 0.7104 0.12 Uiso 1 1 calc R A 1
H27B H 0.8246 -0.1381 0.6387 0.12 Uiso 1 1 calc R A 1
H27C H 0.6834 -0.0857 0.599 0.12 Uiso 1 1 calc R A 1
C28 C 0.8756(8) 0.3581(8) 0.5599(6) 0.055(2) Uani 1 1 d . . 1
H28 H 0.8751 0.3256 0.5164 0.066 Uiso 1 1 calc R . 1
C29 C 0.9234(8) 0.3036(8) 0.6483(7) 0.058(2) Uani 1 1 d . . 1
C30 C 0.9051(9) 0.3777(8) 0.6922(6) 0.055(2) Uani 1 1 d . . 1
C31 C 0.8456(8) 0.4819(8) 0.6285(6) 0.053(2) Uani 1 1 d . . 1
C32 C 0.8284(8) 0.4693(7) 0.5457(6) 0.0440(19) Uani 1 1 d . . 1
C33 C 1.0013(10) 0.1867(9) 0.6824(9) 0.091(4) Uani 1 1 d . . 1
H33A H 1.0965 0.1846 0.6585 0.136 Uiso 1 1 calc R . 1
H33B H 0.9683 0.1439 0.6584 0.136 Uiso 1 1 calc R . 1
H33C H 0.9891 0.1563 0.7524 0.136 Uiso 1 1 calc R . 1
C34 C 0.9615(11) 0.3580(11) 0.7791(7) 0.094(4) Uani 1 1 d . . 1
H34A H 0.9631 0.2829 0.823 0.141 Uiso 1 1 calc R . 1
H34B H 0.9057 0.4075 0.8107 0.141 Uiso 1 1 calc R . 1
H34C H 1.0528 0.3708 0.7608 0.141 Uiso 1 1 calc R . 1
C35 C 0.8235(10) 0.5883(8) 0.6405(8) 0.072(3) Uani 1 1 d . . 1
H35A H 0.8992 0.623 0.6053 0.108 Uiso 1 1 calc R . 1
H35B H 0.8161 0.5758 0.7084 0.108 Uiso 1 1 calc R . 1
H35C H 0.7409 0.6357 0.6157 0.108 Uiso 1 1 calc R . 1
C36 C 0.7871(10) 0.5561(8) 0.4552(6) 0.066(3) Uani 1 1 d . . 1
H36A H 0.8618 0.5917 0.4189 0.099 Uiso 1 1 calc R . 1
H36B H 0.7106 0.6098 0.4697 0.099 Uiso 1 1 calc R . 1
H36C H 0.7617 0.5242 0.4172 0.099 Uiso 1 1 calc R . 1
O1S O 0.0058(18) 0.0287(14) -0.0432(11) 0.096(5) Uiso 0.5 1 d P . 1
C1S C -0.017(3) -0.076(2) -0.021(2) 0.203(10) Uiso 1 1 d . . 1
C2S C -0.028(2) -0.099(2) -0.0899(18) 0.191(9) Uiso 1 1 d . B 1

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
U 0.03586(17) 0.04006(17) 0.03440(15) -0.01480(12) 0.00133(11) -0.01689(12)
Si1 0.0427(13) 0.0413(11) 0.0379(11) -0.0208(9) 0.0003(9) -0.0151(10)
Si2 0.0487(14) 0.0341(11) 0.0440(12) -0.0180(9) -0.0020(10) -0.0136(10)
C2 0.039(4) 0.043(4) 0.033(4) -0.017(3) 0.001(3) -0.019(3)
C3 0.038(4) 0.039(4) 0.032(4) -0.014(3) 0.004(3) -0.019(3)
C4 0.040(4) 0.041(4) 0.035(4) -0.016(3) -0.004(3) -0.017(3)
C5 0.043(5) 0.034(4) 0.029(4) -0.007(3) -0.001(3) -0.017(3)
C6 0.037(4) 0.035(4) 0.040(4) -0.011(3) -0.002(3) -0.008(3)
C7 0.043(5) 0.046(4) 0.039(4) -0.014(4) -0.009(3) -0.013(4)
C8 0.041(5) 0.058(5) 0.034(4) -0.017(4) -0.010(3) -0.018(4)
C9 0.046(5) 0.052(5) 0.039(4) -0.024(4) 0.002(3) -0.020(4)
C10 0.054(5) 0.044(5) 0.057(5) -0.024(4) -0.006(4) -0.020(4)
C11 0.069(7) 0.057(6) 0.084(7) -0.034(5) 0.015(5) -0.035(5)
C12 0.069(7) 0.062(6) 0.080(6) -0.047(5) -0.002(5) -0.018(5)
C13 0.057(6) 0.048(5) 0.046(5) -0.027(4) -0.008(4) -0.006(4)
C14 0.078(7) 0.067(6) 0.046(5) -0.014(5) -0.011(5) -0.007(5)
C15 0.060(6) 0.067(6) 0.062(6) -0.029(5) -0.018(5) -0.004(5)
C16 0.041(5) 0.051(5) 0.038(4) -0.023(4) 0.000(3) -0.009(4)
C17 0.057(6) 0.058(5) 0.048(5) -0.021(4) 0.004(4) -0.024(4)
C18 0.054(6) 0.085(7) 0.041(5) -0.026(5) 0.000(4) -0.019(5)
C19 0.077(7) 0.041(5) 0.055(5) -0.014(4) -0.005(5) -0.030(5)
C20 0.086(8) 0.071(7) 0.058(6) -0.015(5) 0.013(5) -0.042(6)
C21 0.112(10) 0.055(6) 0.059(6) 0.005(5) -0.016(6) -0.033(6)
C22 0.061(6) 0.047(5) 0.065(6) -0.034(4) -0.014(4) -0.008(4)
C23 0.110(9) 0.051(6) 0.064(6) -0.017(5) -0.035(6) -0.016(6)
C24 0.081(8) 0.067(6) 0.093(7) -0.051(6) -0.021(6) -0.016(5)
C25 0.056(6) 0.050(5) 0.060(5) -0.030(4) -0.006(4) -0.008(4)
C26 0.068(7) 0.079(7) 0.095(8) -0.042(7) 0.023(6) -0.018(6)
C27 0.079(8) 0.057(6) 0.112(9) -0.052(6) 0.007(6) -0.009(5)
C28 0.037(5) 0.076(6) 0.057(5) -0.035(5) 0.016(4) -0.025(4)
C29 0.030(5) 0.065(6) 0.070(6) -0.020(5) 0.001(4) -0.011(4)
C30 0.043(5) 0.083(7) 0.045(5) -0.017(5) 0.002(4) -0.038(5)
C31 0.041(5) 0.073(6) 0.061(5) -0.036(5) 0.010(4) -0.031(5)
C32 0.033(4) 0.056(5) 0.047(4) -0.018(4) -0.003(3) -0.018(4)
C33 0.045(6) 0.077(8) 0.126(10) -0.023(7) -0.003(6) -0.004(5)
C34 0.069(8) 0.156(12) 0.059(6) -0.011(7) -0.016(5) -0.064(8)
C35 0.069(7) 0.083(7) 0.082(7) -0.044(6) 0.016(5) -0.043(6)
C36 0.058(6) 0.083(7) 0.051(5) -0.004(5) -0.002(4) -0.040(5)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 O3 2.227(12) 2_666 ?
U O1 2.422(10) . ?
U O2 2.427(10) . ?
U C6 2.653(7) . ?
U C4 2.656(7) . ?
U C3 2.674(7) . ?
U C9 2.677(7) . ?
U C7 2.689(8) . ?
U C8 2.692(7) . ?
U C5 2.698(7) . ?
U C2 2.714(7) . ?
U C28 2.714(8) . ?
U C32 2.731(8) . ?
U C31 2.776(8) . ?
U C29 2.789(8) . ?
U C30 2.820(8) . ?
Si1 C2 1.899(8) . ?
Si1 C10 1.903(8) . ?
Si1 C13 1.904(8) . ?
Si1 C16 1.905(8) . ?
Si2 C22 1.896(9) . ?
Si2 C25 1.897(9) . ?
Si2 C19 1.898(8) . ?
Si2 C5 1.904(7) . ?
O1 C1 1.37(2) . ?
O2 C1 1.219(17) . ?
O3 C1 1.26(3) . ?
C2 C9 1.402(10) . ?
C2 C3 1.420(9) . ?
C3 C4 1.412(10) . ?
C3 H3 0.95 . ?
C4 C5 1.422(10) . ?
C4 H4 0.95 . ?
C5 C6 1.415(10) . ?
C6 C7 1.406(10) . ?
C6 H6 0.95 . ?
C7 C8 1.397(11) . ?
C7 H7 0.95 . ?
C8 C9 1.416(11) . ?
C8 H8 0.95 . ?
C9 H9 0.95 . ?
C10 C12 1.536(11) . ?
C10 C11 1.545(12) . ?
C10 H10 1 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C15 1.512(12) . ?
C13 C14 1.536(12) . ?
C13 H13 1 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C16 C18 1.523(11) . ?
C16 C17 1.530(11) . ?
C16 H16 1 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 C21 1.509(13) . ?
C19 C20 1.524(13) . ?
C19 H19 1 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 C23 1.529(13) . ?
C22 C24 1.536(11) . ?
C22 H22 1 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 C26 1.529(13) . ?
C25 C27 1.531(12) . ?
C25 H25 1 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 C29 1.400(13) . ?
C28 C32 1.412(12) . ?
C28 H28 0.95 . ?
C29 C30 1.391(13) . ?
C29 C33 1.521(13) . ?
C30 C31 1.435(13) . ?
C30 C34 1.489(12) . ?
C31 C32 1.419(11) . ?
C31 C35 1.501(12) . ?
C32 C36 1.487(12) . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?
C34 H34A 0.98 . ?
C34 H34B 0.98 . ?
C34 H34C 0.98 . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C36 H36A 0.98 . ?
C36 H36B 0.98 . ?
C36 H36C 0.98 . ?
O1S O1S 1.24(3) 2 ?
O1S C1S 1.42(3) . ?
O1S C1S 1.43(3) 2 ?
C1S C2S 1.26(3) . ?
C1S O1S 1.43(3) 2 ?

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
O3 U C6 126.9(4) 2_666 . ?
O1 U C6 110.6(3) . . ?
O2 U C6 152.6(3) . . ?
O3 U C4 82.2(3) 2_666 . ?
O1 U C4 77.4(3) . . ?
O2 U C4 95.1(3) . . ?
C6 U C4 57.8(2) . . ?
O3 U C3 83.0(3) 2_666 . ?
O1 U C3 88.3(3) . . ?
O2 U C3 78.6(3) . . ?
C6 U C3 78.6(2) . . ?
C4 U C3 30.7(2) . . ?
O3 U C9 128.0(4) 2_666 . ?
O1 U C9 142.1(3) . . ?
O2 U C9 100.0(3) . . ?
C6 U C9 80.0(2) . . ?
C4 U C9 78.8(2) . . ?
C3 U C9 57.3(2) . . ?
O3 U C7 156.8(4) 2_666 . ?
O1 U C7 141.0(3) . . ?
O2 U C7 157.7(3) . . ?
C6 U C7 30.5(2) . . ?
C4 U C7 77.3(2) . . ?
C3 U C7 84.8(2) . . ?
C9 U C7 58.2(2) . . ?
O3 U C8 157.8(4) 2_666 . ?
O1 U C8 162.7(3) . . ?
O2 U C8 129.6(3) . . ?
C6 U C8 58.2(2) . . ?
C4 U C8 85.3(2) . . ?
C3 U C8 76.9(2) . . ?
C9 U C8 30.6(2) . . ?
C7 U C8 30.1(2) . . ?
O3 U C5 98.6(4) 2_666 . ?
O1 U C5 85.6(3) . . ?
O2 U C5 122.3(3) . . ?
C6 U C5 30.7(2) . . ?
C4 U C5 30.8(2) . . ?
C3 U C5 59.0(2) . . ?
C9 U C5 88.8(2) . . ?
C7 U C5 58.2(2) . . ?
C8 U C5 79.2(2) . . ?
O3 U C2 100.1(4) 2_666 . ?
O1 U C2 112.1(3) . . ?
O2 U C2 79.6(3) . . ?
C6 U C2 88.3(2) . . ?
C4 U C2 59.0(2) . . ?
C3 U C2 30.6(2) . . ?
C9 U C2 30.1(2) . . ?
C7 U C2 78.5(2) . . ?
C8 U C2 57.6(2) . . ?
C5 U C2 81.3(2) . . ?
O3 U C28 83.8(4) 2_666 . ?
O1 U C28 75.6(3) . . ?
O2 U C28 96.8(3) . . ?
C6 U C28 100.5(3) . . ?
C4 U C28 135.4(2) . . ?
C3 U C28 162.5(2) . . ?
C9 U C28 140.1(3) . . ?
C7 U C28 103.3(3) . . ?
C8 U C28 117.8(3) . . ?
C5 U C28 112.0(3) . . ?
C2 U C28 165.6(2) . . ?
O3 U C32 74.2(3) 2_666 . ?
O1 U C32 76.0(3) . . ?
O2 U C32 72.8(3) . . ?
C6 U C32 129.2(2) . . ?
C4 U C32 153.0(2) . . ?
C3 U C32 151.3(2) . . ?
C9 U C32 126.5(2) . . ?
C7 U C32 122.3(2) . . ?
C8 U C32 121.2(2) . . ?
C5 U C32 140.8(2) . . ?
C2 U C32 137.7(2) . . ?
C28 U C32 30.1(3) . . ?
O3 U C31 98.4(4) 2_666 . ?
O1 U C31 104.5(3) . . ?
O2 U C31 83.2(3) . . ?
C6 U C31 124.1(3) . . ?
C4 U C31 175.7(2) . . ?
C3 U C31 145.1(2) . . ?
C9 U C31 97.6(2) . . ?
C7 U C31 102.8(3) . . ?
C8 U C31 92.8(2) . . ?
C5 U C31 152.3(3) . . ?
C2 U C31 116.8(2) . . ?
C28 U C31 48.8(3) . . ?
C32 U C31 29.8(2) . . ?
O3 U C29 113.2(4) 2_666 . ?
O1 U C29 103.3(3) . . ?
O2 U C29 121.8(3) . . ?
C6 U C29 81.6(3) . . ?
C4 U C29 135.3(3) . . ?
C3 U C29 159.6(2) . . ?
C9 U C29 114.4(3) . . ?
C7 U C29 75.6(3) . . ?
C8 U C29 88.6(3) . . ?
C5 U C29 104.6(3) . . ?
C2 U C29 144.5(3) . . ?
C28 U C29 29.4(3) . . ?
C32 U C29 49.0(3) . . ?
C31 U C29 48.3(3) . . ?
O3 U C30 123.4(3) 2_666 . ?
O1 U C30 122.2(3) . . ?
O2 U C30 112.9(3) . . ?
C6 U C30 94.5(3) . . ?
C4 U C30 151.7(3) . . ?
C3 U C30 148.9(2) . . ?
C9 U C30 91.7(2) . . ?
C7 U C30 75.0(2) . . ?
C8 U C30 73.8(2) . . ?
C5 U C30 123.8(3) . . ?
C2 U C30 120.1(2) . . ?
C28 U C30 48.4(3) . . ?
C32 U C30 49.2(2) . . ?
C31 U C30 29.7(3) . . ?
C29 U C30 28.7(3) . . ?
C2 Si1 C10 110.4(4) . . ?
C2 Si1 C13 113.0(3) . . ?
C10 Si1 C13 113.4(4) . . ?
C2 Si1 C16 104.6(3) . . ?
C10 Si1 C16 106.7(3) . . ?
C13 Si1 C16 108.1(4) . . ?
C22 Si2 C25 113.0(4) . . ?
C22 Si2 C19 107.5(4) . . ?
C25 Si2 C19 108.5(4) . . ?
C22 Si2 C5 111.4(3) . . ?
C25 Si2 C5 110.8(4) . . ?
C19 Si2 C5 105.2(3) . . ?
C1 O1 U 93.3(9) . . ?
C1 O2 U 97.2(12) . . ?
C1 O3 U 175.3(14) . 2_666 ?
O2 C1 O3 127(2) . . ?
O2 C1 O1 115.5(17) . . ?
O3 C1 O1 117.2(13) . . ?
C9 C2 C3 130.7(7) . . ?
C9 C2 Si1 113.3(5) . . ?
C3 C2 Si1 115.2(6) . . ?
C9 C2 U 73.5(4) . . ?
C3 C2 U 73.2(4) . . ?
Si1 C2 U 143.7(3) . . ?
C4 C3 C2 137.9(7) . . ?
C4 C3 U 74.0(4) . . ?
C2 C3 U 76.3(4) . . ?
C4 C3 H3 111.1 . . ?
C2 C3 H3 111.1 . . ?
U C3 H3 135.6 . . ?
C3 C4 C5 138.1(7) . . ?
C3 C4 U 75.3(4) . . ?
C5 C4 U 76.2(4) . . ?
C3 C4 H4 111 . . ?
C5 C4 H4 111 . . ?
U C4 H4 133.4 . . ?
C6 C5 C4 129.4(7) . . ?
C6 C5 Si2 113.5(5) . . ?
C4 C5 Si2 116.4(5) . . ?
C6 C5 U 72.9(4) . . ?
C4 C5 U 73.0(4) . . ?
Si2 C5 U 142.7(3) . . ?
C7 C6 C5 136.3(7) . . ?
C7 C6 U 76.1(4) . . ?
C5 C6 U 76.4(4) . . ?
C7 C6 H6 111.8 . . ?
C5 C6 H6 111.8 . . ?
U C6 H6 129.6 . . ?
C8 C7 C6 135.9(8) . . ?
C8 C7 U 75.1(4) . . ?
C6 C7 U 73.3(4) . . ?
C8 C7 H7 112 . . ?
C6 C7 H7 112 . . ?
U C7 H7 136.5 . . ?
C7 C8 C9 136.1(7) . . ?
C7 C8 U 74.8(4) . . ?
C9 C8 U 74.1(4) . . ?
C7 C8 H8 112 . . ?
C9 C8 H8 112 . . ?
U C8 H8 135.7 . . ?
C2 C9 C8 135.3(7) . . ?
C2 C9 U 76.4(4) . . ?
C8 C9 U 75.3(4) . . ?
C2 C9 H9 112.4 . . ?
C8 C9 H9 112.4 . . ?
U C9 H9 130 . . ?
C12 C10 C11 110.7(7) . . ?
C12 C10 Si1 112.6(6) . . ?
C11 C10 Si1 114.5(6) . . ?
C12 C10 H10 106.1 . . ?
C11 C10 H10 106.1 . . ?
Si1 C10 H10 106.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C13 C14 109.4(7) . . ?
C15 C13 Si1 113.1(6) . . ?
C14 C13 Si1 113.5(6) . . ?
C15 C13 H13 106.8 . . ?
C14 C13 H13 106.8 . . ?
Si1 C13 H13 106.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 C17 110.4(7) . . ?
C18 C16 Si1 113.5(6) . . ?
C17 C16 Si1 111.0(5) . . ?
C18 C16 H16 107.2 . . ?
C17 C16 H16 107.2 . . ?
Si1 C16 H16 107.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C20 109.5(8) . . ?
C21 C19 Si2 114.6(6) . . ?
C20 C19 Si2 111.2(6) . . ?
C21 C19 H19 107.1 . . ?
C20 C19 H19 107.1 . . ?
Si2 C19 H19 107.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C24 110.1(7) . . ?
C23 C22 Si2 114.7(7) . . ?
C24 C22 Si2 113.8(6) . . ?
C23 C22 H22 105.8 . . ?
C24 C22 H22 105.8 . . ?
Si2 C22 H22 105.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C27 110.0(8) . . ?
C26 C25 Si2 115.0(6) . . ?
C27 C25 Si2 114.2(7) . . ?
C26 C25 H25 105.6 . . ?
C27 C25 H25 105.6 . . ?
Si2 C25 H25 105.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C32 109.1(8) . . ?
C29 C28 U 78.2(5) . . ?
C32 C28 U 75.6(5) . . ?
C29 C28 H28 125.5 . . ?
C32 C28 H28 125.5 . . ?
U C28 H28 112.9 . . ?
C30 C29 C28 108.8(8) . . ?
C30 C29 C33 126.0(10) . . ?
C28 C29 C33 124.6(10) . . ?
C30 C29 U 76.9(5) . . ?
C28 C29 U 72.3(5) . . ?
C33 C29 U 124.1(6) . . ?
C29 C30 C31 107.3(8) . . ?
C29 C30 C34 126.3(10) . . ?
C31 C30 C34 125.3(9) . . ?
C29 C30 U 74.4(5) . . ?
C31 C30 U 73.5(5) . . ?
C34 C30 U 127.0(6) . . ?
C32 C31 C30 108.1(8) . . ?
C32 C31 C35 125.3(9) . . ?
C30 C31 C35 126.1(8) . . ?
C32 C31 U 73.3(4) . . ?
C30 C31 U 76.8(5) . . ?
C35 C31 U 122.5(6) . . ?
C28 C32 C31 106.7(8) . . ?
C28 C32 C36 125.2(8) . . ?
C31 C32 C36 127.7(8) . . ?
C28 C32 U 74.3(4) . . ?
C31 C32 U 76.8(4) . . ?
C36 C32 U 120.7(5) . . ?
C1S O1S C1S 128.4(17) . 2 ?
C2S C1S O1S 117(3) . . ?

#===END