# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Stephen Liddle'
_publ_contact_author_email       STEPHEN.LIDDLE@NOTTINGHAM.AC.UK

_publ_section_title              
;
Synthesis and Structure of a bis-N-Heterocyclic
Carbene Complex of Uranium Tetrachloride Exhibiting Short
Cl???Ccarbene Contacts
;
loop_
_publ_author_name
'Stephen Liddle'
'Benedict M. Gardner'
'Jonathan McMaster'

# Attachment '1.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 725414'

_refine_special_details          
;
Lattice THF was found to have high anisotropic displacement parameters.
This was treated with SIMU, DELU and DFIX. A two-part disorder model
was not workable. Data > 22.5 deg suppressed as data weak.
;

_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H72 Cl4 N4 U, C4 H8 O'
_chemical_formula_sum            'C58 H80 Cl4 N4 O U'
_chemical_formula_weight         1229.09

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'
Cl Cl 0.1484 0.1585 '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           Hexagonal
_symmetry_space_group_name_H-M   'R -3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   47.5395(12)
_cell_length_b                   47.5395(12)
_cell_length_c                   13.8960(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     27197.5(17)
_cell_formula_units_Z            18
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6677
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      21.55

_exptl_crystal_description       Block
_exptl_crystal_colour            'Pale green'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             11232
_exptl_absorpt_coefficient_mu    2.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            52807
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         22.50
_reflns_number_total             7869
_reflns_number_gt                6782
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_reduction        
'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'

_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^)+(0.0517P)^2^+279.0135P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7869
_refine_ls_number_parameters     629
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.003
_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 0.711394(6) 0.147933(6) 0.005736(18) 0.02673(11) Uani 1 1 d . . .
Cl1 Cl 0.75314(5) 0.16057(5) 0.14042(13) 0.0437(5) Uani 1 1 d . . .
Cl2 Cl 0.67155(4) 0.09363(4) 0.08822(13) 0.0399(5) Uani 1 1 d . . .
Cl3 Cl 0.66712(5) 0.14547(5) -0.10614(13) 0.0430(5) Uani 1 1 d . . .
Cl4 Cl 0.75535(5) 0.19160(5) -0.10162(14) 0.0457(5) Uani 1 1 d . . .
C1 C 0.72149(16) 0.10594(16) -0.0955(5) 0.0289(16) Uani 1 1 d . . .
N1 N 0.74277(12) 0.09562(13) -0.0772(4) 0.0251(13) Uani 1 1 d . . .
N2 N 0.70337(13) 0.08677(13) -0.1695(4) 0.0278(13) Uani 1 1 d . . .
C2 C 0.73770(17) 0.07004(16) -0.1375(5) 0.0311(17) Uani 1 1 d . . .
H2A H 0.7493 0.0586 -0.1371 0.037 Uiso 1 1 calc R . .
C3 C 0.71341(17) 0.06493(17) -0.1955(5) 0.0327(17) Uani 1 1 d . . .
H3A H 0.7045 0.0493 -0.2456 0.039 Uiso 1 1 calc R . .
C4 C 0.76842(16) 0.10786(17) -0.0053(5) 0.0316(17) Uani 1 1 d . . .
C5 C 0.76200(18) 0.09082(18) 0.0819(5) 0.0353(18) Uani 1 1 d . . .
C6 C 0.7881(2) 0.1015(2) 0.1458(6) 0.050(2) Uani 1 1 d . . .
H6A H 0.7849 0.0906 0.2055 0.061 Uiso 1 1 calc R . .
C7 C 0.8180(2) 0.1271(2) 0.1246(8) 0.061(3) Uani 1 1 d . . .
H7A H 0.8354 0.1339 0.1693 0.074 Uiso 1 1 calc R . .
C8 C 0.8231(2) 0.1431(2) 0.0388(7) 0.056(2) Uani 1 1 d . . .
H8A H 0.8441 0.1607 0.0247 0.067 Uiso 1 1 calc R . .
C9 C 0.79848(18) 0.13459(17) -0.0282(6) 0.0385(19) Uani 1 1 d . . .
C10 C 0.7294(2) 0.06214(19) 0.1053(5) 0.047(2) Uani 1 1 d . . .
H10A H 0.7131 0.0624 0.0604 0.056 Uiso 1 1 calc R . .
C11 C 0.7296(2) 0.0302(2) 0.0888(7) 0.059(2) Uani 1 1 d . . .
H11A H 0.7354 0.0291 0.0218 0.089 Uiso 1 1 calc R . .
H11B H 0.7080 0.0118 0.1025 0.089 Uiso 1 1 calc R . .
H11C H 0.7455 0.0294 0.1317 0.089 Uiso 1 1 calc R . .
C12 C 0.7183(3) 0.0629(3) 0.2090(6) 0.079(3) Uani 1 1 d . . .
H12A H 0.7186 0.0834 0.2199 0.119 Uiso 1 1 calc R . .
H12B H 0.7330 0.0611 0.2546 0.119 Uiso 1 1 calc R . .
H12C H 0.6962 0.0447 0.2184 0.119 Uiso 1 1 calc R . .
C13 C 0.8045(2) 0.15256(19) -0.1233(6) 0.053(2) Uani 1 1 d . . .
H13A H 0.7832 0.1493 -0.1466 0.064 Uiso 1 1 calc R . .
C14 C 0.8173(2) 0.1380(2) -0.1997(7) 0.076(3) Uani 1 1 d . . .
H14A H 0.8013 0.1149 -0.2090 0.114 Uiso 1 1 calc R . .
H14B H 0.8379 0.1402 -0.1777 0.114 Uiso 1 1 calc R . .
H14C H 0.8208 0.1496 -0.2607 0.114 Uiso 1 1 calc R . .
C15 C 0.8278(2) 0.1895(2) -0.1132(9) 0.087(4) Uani 1 1 d . . .
H15A H 0.8197 0.1981 -0.0631 0.130 Uiso 1 1 calc R . .
H15B H 0.8289 0.2002 -0.1746 0.130 Uiso 1 1 calc R . .
H15C H 0.8495 0.1936 -0.0956 0.130 Uiso 1 1 calc R . .
C16 C 0.67834(17) 0.08850(16) -0.2245(5) 0.0299(17) Uani 1 1 d . . .
C17 C 0.68842(18) 0.11140(16) -0.3004(5) 0.0342(18) Uani 1 1 d . . .
C18 C 0.6639(2) 0.11049(18) -0.3576(5) 0.0401(19) Uani 1 1 d . . .
H18A H 0.6695 0.1256 -0.4089 0.048 Uiso 1 1 calc R . .
C19 C 0.6320(2) 0.08838(18) -0.3415(5) 0.044(2) Uani 1 1 d . . .
H19A H 0.6158 0.0878 -0.3832 0.052 Uiso 1 1 calc R . .
C20 C 0.62283(18) 0.06702(18) -0.2661(5) 0.0388(19) Uani 1 1 d . . .
H20A H 0.6004 0.0524 -0.2546 0.047 Uiso 1 1 calc R . .
C21 C 0.64605(17) 0.06652(17) -0.2060(5) 0.0312(17) Uani 1 1 d . . .
C22 C 0.72389(18) 0.13616(17) -0.3174(5) 0.0399(19) Uani 1 1 d . . .
H22A H 0.7354 0.1400 -0.2543 0.048 Uiso 1 1 calc R . .
C23 C 0.7292(2) 0.16867(18) -0.3527(6) 0.052(2) Uani 1 1 d . . .
H23A H 0.7184 0.1765 -0.3091 0.079 Uiso 1 1 calc R . .
H23B H 0.7201 0.1661 -0.4175 0.079 Uiso 1 1 calc R . .
H23C H 0.7525 0.1844 -0.3544 0.079 Uiso 1 1 calc R . .
C24 C 0.7396(2) 0.1230(2) -0.3875(6) 0.062(3) Uani 1 1 d . . .
H24A H 0.7390 0.1038 -0.3595 0.092 Uiso 1 1 calc R . .
H24B H 0.7622 0.1398 -0.3992 0.092 Uiso 1 1 calc R . .
H24C H 0.7276 0.1171 -0.4484 0.092 Uiso 1 1 calc R . .
C25 C 0.63545(17) 0.04234(17) -0.1238(5) 0.0356(18) Uani 1 1 d . . .
H25A H 0.6544 0.0498 -0.0792 0.043 Uiso 1 1 calc R . .
C26 C 0.6269(2) 0.00859(18) -0.1604(6) 0.054(2) Uani 1 1 d . . .
H26A H 0.6211 -0.0064 -0.1058 0.081 Uiso 1 1 calc R . .
H26B H 0.6456 0.0099 -0.1941 0.081 Uiso 1 1 calc R . .
H26C H 0.6084 0.0006 -0.2047 0.081 Uiso 1 1 calc R . .
C27 C 0.60762(17) 0.04074(18) -0.0662(6) 0.0411(19) Uani 1 1 d . . .
H27A H 0.6129 0.0627 -0.0476 0.062 Uiso 1 1 calc R . .
H27B H 0.6041 0.0276 -0.0083 0.062 Uiso 1 1 calc R . .
H27C H 0.5879 0.0308 -0.1055 0.062 Uiso 1 1 calc R . .
C28 C 0.69462(16) 0.18703(17) 0.0981(5) 0.0276(16) Uani 1 1 d . . .
N3 N 0.70671(12) 0.21941(13) 0.0893(4) 0.0248(13) Uani 1 1 d . . .
N4 N 0.66869(12) 0.17750(12) 0.1577(4) 0.0222(12) Uani 1 1 d . . .
C29 C 0.68892(16) 0.22974(16) 0.1420(5) 0.0321(17) Uani 1 1 d . . .
H29A H 0.6928 0.2513 0.1471 0.038 Uiso 1 1 calc R . .
C30 C 0.66515(16) 0.20333(16) 0.1843(5) 0.0282(16) Uani 1 1 d . . .
H30A H 0.6488 0.2026 0.2252 0.034 Uiso 1 1 calc R . .
C31 C 0.73633(16) 0.24238(15) 0.0416(5) 0.0271(16) Uani 1 1 d . . .
C32 C 0.76518(17) 0.25556(17) 0.0943(5) 0.0352(18) Uani 1 1 d . . .
C33 C 0.79296(18) 0.27896(19) 0.0494(7) 0.050(2) Uani 1 1 d . . .
H33A H 0.8129 0.2886 0.0839 0.060 Uiso 1 1 calc R . .
C34 C 0.7929(2) 0.2888(2) -0.0435(7) 0.055(2) Uani 1 1 d . . .
H34A H 0.8125 0.3045 -0.0732 0.067 Uiso 1 1 calc R . .
C35 C 0.7636(2) 0.27530(18) -0.0935(6) 0.050(2) Uani 1 1 d . . .
H35A H 0.7634 0.2825 -0.1571 0.060 Uiso 1 1 calc R . .
C36 C 0.73500(17) 0.25183(17) -0.0529(5) 0.0336(17) Uani 1 1 d . . .
C37 C 0.7663(2) 0.24513(19) 0.1960(6) 0.051(2) Uani 1 1 d . . .
H37A H 0.7468 0.2233 0.2064 0.062 Uiso 1 1 calc R . .
C38 C 0.7651(3) 0.2688(2) 0.2689(6) 0.078(3) Uani 1 1 d . . .
H38A H 0.7450 0.2694 0.2599 0.117 Uiso 1 1 calc R . .
H38B H 0.7838 0.2905 0.2589 0.117 Uiso 1 1 calc R . .
H38C H 0.7657 0.2614 0.3344 0.117 Uiso 1 1 calc R . .
C39 C 0.7964(2) 0.2423(2) 0.2145(8) 0.087(4) Uani 1 1 d . . .
H39A H 0.7987 0.2295 0.1631 0.130 Uiso 1 1 calc R . .
H39B H 0.7942 0.2316 0.2765 0.130 Uiso 1 1 calc R . .
H39C H 0.8156 0.2640 0.2158 0.130 Uiso 1 1 calc R . .
C40 C 0.70278(19) 0.23743(19) -0.1068(5) 0.043(2) Uani 1 1 d . . .
H40A H 0.6876 0.2158 -0.0775 0.052 Uiso 1 1 calc R . .
C41 C 0.6876(2) 0.2586(2) -0.0971(7) 0.062(3) Uani 1 1 d . . .
H41A H 0.6847 0.2616 -0.0288 0.094 Uiso 1 1 calc R . .
H41B H 0.6664 0.2481 -0.1293 0.094 Uiso 1 1 calc R . .
H41C H 0.7017 0.2797 -0.1270 0.094 Uiso 1 1 calc R . .
C42 C 0.7068(3) 0.2320(2) -0.2133(6) 0.066(3) Uani 1 1 d . . .
H42A H 0.7184 0.2198 -0.2191 0.098 Uiso 1 1 calc R . .
H42B H 0.7193 0.2530 -0.2457 0.098 Uiso 1 1 calc R . .
H42C H 0.6854 0.2196 -0.2434 0.098 Uiso 1 1 calc R . .
C43 C 0.64768(16) 0.14509(15) 0.1928(5) 0.0271(16) Uani 1 1 d . . .
C44 C 0.61696(15) 0.12669(16) 0.1530(5) 0.0300(17) Uani 1 1 d . . .
C45 C 0.59666(18) 0.09628(17) 0.1929(6) 0.0401(19) Uani 1 1 d . . .
H45A H 0.5757 0.0829 0.1661 0.048 Uiso 1 1 calc R . .
C46 C 0.60640(19) 0.08510(17) 0.2709(6) 0.042(2) Uani 1 1 d . . .
H46A H 0.5921 0.0643 0.2975 0.050 Uiso 1 1 calc R . .
C47 C 0.63695(19) 0.10429(17) 0.3098(5) 0.0386(19) Uani 1 1 d . . .
H47A H 0.6434 0.0964 0.3632 0.046 Uiso 1 1 calc R . .
C48 C 0.65851(17) 0.13476(17) 0.2732(5) 0.0304(17) Uani 1 1 d . . .
C49 C 0.60514(16) 0.13862(16) 0.0695(5) 0.0325(17) Uani 1 1 d . . .
H49A H 0.6246 0.1575 0.0398 0.039 Uiso 1 1 calc R . .
C50 C 0.58298(19) 0.15088(19) 0.1082(6) 0.045(2) Uani 1 1 d . . .
H50A H 0.5953 0.1691 0.1523 0.068 Uiso 1 1 calc R . .
H50B H 0.5646 0.1333 0.1426 0.068 Uiso 1 1 calc R . .
H50C H 0.5748 0.1581 0.0544 0.068 Uiso 1 1 calc R . .
C51 C 0.58776(18) 0.11308(19) -0.0099(6) 0.046(2) Uani 1 1 d . . .
H51A H 0.6027 0.1064 -0.0363 0.068 Uiso 1 1 calc R . .
H51B H 0.5809 0.1224 -0.0613 0.068 Uiso 1 1 calc R . .
H51C H 0.5687 0.0941 0.0174 0.068 Uiso 1 1 calc R . .
C52 C 0.69205(18) 0.15571(18) 0.3163(5) 0.0379(18) Uani 1 1 d . . .
H52A H 0.7070 0.1693 0.2635 0.045 Uiso 1 1 calc R . .
C53 C 0.6915(2) 0.17857(19) 0.3926(6) 0.050(2) Uani 1 1 d . . .
H53A H 0.6845 0.1928 0.3631 0.074 Uiso 1 1 calc R . .
H53B H 0.7133 0.1918 0.4199 0.074 Uiso 1 1 calc R . .
H53C H 0.6762 0.1658 0.4439 0.074 Uiso 1 1 calc R . .
C54 C 0.7056(2) 0.1355(2) 0.3596(6) 0.052(2) Uani 1 1 d . . .
H54A H 0.7064 0.1212 0.3100 0.078 Uiso 1 1 calc R . .
H54B H 0.6916 0.1223 0.4125 0.078 Uiso 1 1 calc R . .
H54C H 0.7276 0.1500 0.3841 0.078 Uiso 1 1 calc R . .
O1 O 0.7160(2) 0.30965(17) 0.1514(6) 0.116(2) Uani 1 1 d DU . .
C55 C 0.7174(3) 0.3316(2) 0.2217(9) 0.133(3) Uani 1 1 d DU . .
H55A H 0.7172 0.3230 0.2866 0.160 Uiso 1 1 calc R . .
H55B H 0.6981 0.3343 0.2158 0.160 Uiso 1 1 calc R . .
C56 C 0.7478(3) 0.3641(3) 0.2089(10) 0.148(3) Uani 1 1 d DU . .
H56A H 0.7425 0.3814 0.1950 0.178 Uiso 1 1 calc R . .
H56B H 0.7616 0.3702 0.2672 0.178 Uiso 1 1 calc R . .
C57 C 0.7644(3) 0.3588(3) 0.1243(10) 0.147(3) Uani 1 1 d DU . .
H57A H 0.7684 0.3749 0.0733 0.176 Uiso 1 1 calc R . .
H57B H 0.7855 0.3614 0.1445 0.176 Uiso 1 1 calc R . .
C58 C 0.7427(3) 0.3249(2) 0.0869(9) 0.127(3) Uani 1 1 d DU . .
H58A H 0.7349 0.3257 0.0213 0.152 Uiso 1 1 calc R . .
H58B H 0.7546 0.3128 0.0842 0.152 Uiso 1 1 calc R . .

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
U1 0.03171(18) 0.02933(17) 0.02394(16) -0.00360(12) -0.00091(11) 0.01886(14)
Cl1 0.0441(11) 0.0594(13) 0.0368(11) -0.0086(9) -0.0092(9) 0.0327(10)
Cl2 0.0445(11) 0.0404(11) 0.0340(11) 0.0015(8) 0.0106(8) 0.0205(9)
Cl3 0.0526(12) 0.0556(12) 0.0302(10) -0.0079(9) -0.0110(9) 0.0341(10)
Cl4 0.0488(12) 0.0397(11) 0.0514(13) 0.0072(9) 0.0127(10) 0.0242(10)
C1 0.032(4) 0.031(4) 0.021(4) 0.009(3) -0.005(3) 0.013(3)
N1 0.019(3) 0.032(3) 0.026(3) 0.004(3) 0.000(2) 0.014(3)
N2 0.036(3) 0.033(3) 0.020(3) 0.004(3) 0.002(3) 0.022(3)
C2 0.043(4) 0.030(4) 0.031(4) -0.003(3) 0.003(4) 0.026(4)
C3 0.045(5) 0.035(4) 0.025(4) -0.005(3) -0.001(4) 0.026(4)
C4 0.032(4) 0.037(4) 0.037(4) -0.004(3) -0.002(3) 0.026(4)
C5 0.045(5) 0.049(5) 0.026(4) -0.007(4) -0.005(4) 0.034(4)
C6 0.068(6) 0.065(6) 0.042(5) -0.014(4) -0.018(5) 0.051(6)
C7 0.062(7) 0.062(6) 0.079(7) -0.041(6) -0.039(6) 0.044(6)
C8 0.038(5) 0.045(5) 0.090(8) -0.019(5) -0.010(5) 0.024(4)
C9 0.038(5) 0.028(4) 0.055(5) -0.004(4) 0.001(4) 0.020(4)
C10 0.060(6) 0.059(5) 0.035(5) 0.016(4) 0.014(4) 0.041(5)
C11 0.051(5) 0.056(6) 0.069(6) 0.024(5) 0.029(5) 0.026(5)
C12 0.113(9) 0.137(10) 0.038(5) 0.029(6) 0.028(6) 0.100(8)
C13 0.044(5) 0.044(5) 0.076(6) 0.019(5) 0.023(5) 0.025(4)
C14 0.083(7) 0.074(7) 0.080(7) 0.040(6) 0.045(6) 0.045(6)
C15 0.049(6) 0.037(5) 0.162(11) 0.038(6) 0.021(7) 0.013(5)
C16 0.040(5) 0.023(4) 0.030(4) -0.009(3) -0.008(3) 0.018(4)
C17 0.053(5) 0.030(4) 0.023(4) -0.005(3) -0.004(4) 0.024(4)
C18 0.063(6) 0.037(5) 0.027(4) -0.002(3) -0.013(4) 0.030(4)
C19 0.053(5) 0.037(5) 0.039(5) 0.000(4) -0.015(4) 0.021(4)
C20 0.040(5) 0.038(4) 0.039(5) -0.006(4) -0.012(4) 0.020(4)
C21 0.044(5) 0.034(4) 0.018(4) -0.006(3) -0.004(3) 0.021(4)
C22 0.051(5) 0.040(5) 0.024(4) 0.006(3) -0.004(3) 0.019(4)
C23 0.074(6) 0.033(5) 0.038(5) 0.005(4) -0.002(4) 0.017(4)
C24 0.068(6) 0.061(6) 0.062(6) 0.019(5) 0.012(5) 0.038(5)
C25 0.036(4) 0.034(4) 0.038(4) -0.002(3) -0.004(3) 0.018(4)
C26 0.069(6) 0.040(5) 0.056(6) 0.008(4) 0.014(5) 0.030(5)
C27 0.037(4) 0.041(5) 0.048(5) 0.002(4) 0.005(4) 0.021(4)
C28 0.025(4) 0.040(5) 0.021(4) 0.002(3) -0.010(3) 0.019(3)
N3 0.026(3) 0.026(3) 0.019(3) -0.001(2) 0.001(2) 0.011(3)
N4 0.024(3) 0.023(3) 0.021(3) 0.003(2) 0.009(2) 0.012(3)
C29 0.035(4) 0.021(4) 0.043(5) -0.008(3) 0.000(4) 0.016(4)
C30 0.025(4) 0.033(4) 0.026(4) -0.003(3) 0.005(3) 0.014(3)
C31 0.028(4) 0.022(4) 0.029(4) -0.003(3) 0.004(3) 0.011(3)
C32 0.028(4) 0.029(4) 0.045(5) -0.001(3) 0.000(4) 0.012(4)
C33 0.028(5) 0.043(5) 0.067(6) -0.008(4) 0.008(4) 0.009(4)
C34 0.036(5) 0.043(5) 0.073(7) 0.008(5) 0.029(5) 0.009(4)
C35 0.058(6) 0.038(5) 0.046(5) 0.011(4) 0.020(5) 0.018(5)
C36 0.036(4) 0.031(4) 0.033(4) -0.001(3) 0.004(3) 0.016(4)
C37 0.047(5) 0.037(5) 0.053(6) 0.001(4) -0.018(4) 0.007(4)
C38 0.095(8) 0.062(6) 0.041(6) -0.011(5) -0.003(5) 0.013(6)
C39 0.062(7) 0.069(7) 0.112(9) -0.005(6) -0.054(6) 0.021(6)
C40 0.053(5) 0.039(5) 0.032(5) 0.006(4) 0.000(4) 0.018(4)
C41 0.060(6) 0.071(6) 0.063(6) 0.006(5) -0.011(5) 0.037(5)
C42 0.105(8) 0.062(6) 0.032(5) -0.002(4) -0.012(5) 0.043(6)
C43 0.033(4) 0.022(4) 0.028(4) 0.000(3) 0.006(3) 0.014(3)
C44 0.020(4) 0.029(4) 0.038(4) -0.001(3) 0.008(3) 0.011(3)
C45 0.036(4) 0.026(4) 0.056(5) -0.004(4) 0.009(4) 0.014(4)
C46 0.048(5) 0.025(4) 0.054(5) 0.013(4) 0.024(4) 0.019(4)
C47 0.052(5) 0.036(5) 0.034(4) 0.010(4) 0.016(4) 0.027(4)
C48 0.040(4) 0.037(4) 0.022(4) 0.002(3) 0.009(3) 0.025(4)
C49 0.029(4) 0.028(4) 0.038(4) -0.002(3) -0.003(3) 0.012(3)
C50 0.049(5) 0.050(5) 0.046(5) -0.010(4) -0.012(4) 0.031(4)
C51 0.039(5) 0.044(5) 0.052(5) -0.013(4) -0.008(4) 0.020(4)
C52 0.045(5) 0.053(5) 0.025(4) 0.008(4) 0.002(3) 0.032(4)
C53 0.055(5) 0.048(5) 0.044(5) -0.005(4) -0.015(4) 0.023(4)
C54 0.062(6) 0.078(6) 0.037(5) 0.007(4) 0.000(4) 0.050(5)
O1 0.113(5) 0.062(4) 0.151(6) -0.003(4) 0.062(4) 0.027(3)
C55 0.126(5) 0.075(4) 0.153(6) -0.015(4) 0.065(5) 0.017(4)
C56 0.135(6) 0.086(4) 0.157(6) -0.022(4) 0.063(5) 0.004(4)
C57 0.130(6) 0.087(5) 0.156(6) -0.018(5) 0.064(5) 0.004(4)
C58 0.117(5) 0.073(4) 0.152(6) -0.008(4) 0.064(4) 0.019(4)

_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 Cl4 2.5621(19) . ?
U1 Cl1 2.5711(18) . ?
U1 Cl3 2.5717(18) . ?
U1 Cl2 2.5838(18) . ?
U1 C1 2.675(7) . ?
U1 C28 2.687(7) . ?
C1 N1 1.351(8) . ?
C1 N2 1.358(8) . ?
N1 C2 1.395(8) . ?
N1 C4 1.454(8) . ?
N2 C3 1.390(8) . ?
N2 C16 1.450(8) . ?
C2 C3 1.328(9) . ?
C4 C9 1.394(10) . ?
C4 C5 1.403(10) . ?
C5 C6 1.398(10) . ?
C5 C10 1.501(11) . ?
C6 C7 1.366(12) . ?
C7 C8 1.368(13) . ?
C8 C9 1.386(11) . ?
C9 C13 1.521(11) . ?
C10 C11 1.539(11) . ?
C10 C12 1.541(10) . ?
C13 C15 1.543(12) . ?
C13 C14 1.549(12) . ?
C16 C21 1.382(10) . ?
C16 C17 1.416(9) . ?
C17 C18 1.395(10) . ?
C17 C22 1.517(10) . ?
C18 C19 1.365(10) . ?
C19 C20 1.370(10) . ?
C20 C21 1.394(10) . ?
C21 C25 1.518(9) . ?
C22 C23 1.518(10) . ?
C22 C24 1.537(11) . ?
C25 C27 1.515(9) . ?
C25 C26 1.532(10) . ?
C28 N3 1.353(8) . ?
C28 N4 1.360(8) . ?
N3 C29 1.381(8) . ?
N3 C31 1.441(8) . ?
N4 C30 1.371(8) . ?
N4 C43 1.439(8) . ?
C29 C30 1.334(9) . ?
C31 C32 1.396(9) . ?
C31 C36 1.401(9) . ?
C32 C33 1.379(10) . ?
C32 C37 1.508(10) . ?
C33 C34 1.374(12) . ?
C34 C35 1.391(12) . ?
C35 C36 1.376(10) . ?
C36 C40 1.525(10) . ?
C37 C39 1.522(12) . ?
C37 C38 1.535(12) . ?
C40 C41 1.509(11) . ?
C40 C42 1.531(11) . ?
C43 C44 1.388(9) . ?
C43 C48 1.417(9) . ?
C44 C45 1.390(10) . ?
C44 C49 1.518(10) . ?
C45 C46 1.384(10) . ?
C46 C47 1.382(11) . ?
C47 C48 1.386(10) . ?
C48 C52 1.518(10) . ?
C49 C50 1.534(10) . ?
C49 C51 1.540(9) . ?
C52 C54 1.523(10) . ?
C52 C53 1.530(10) . ?
O1 C55 1.409(5) . ?
O1 C58 1.419(5) . ?
C55 C56 1.508(5) . ?
C56 C57 1.507(5) . ?
C57 C58 1.504(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
Cl4 U1 Cl1 90.74(6) . . ?
Cl4 U1 Cl3 90.13(7) . . ?
Cl1 U1 Cl3 165.75(6) . . ?
Cl4 U1 Cl2 164.02(6) . . ?
Cl1 U1 Cl2 90.30(6) . . ?
Cl3 U1 Cl2 92.76(6) . . ?
Cl4 U1 C1 85.43(14) . . ?
Cl1 U1 C1 98.72(14) . . ?
Cl3 U1 C1 95.52(14) . . ?
Cl2 U1 C1 78.65(14) . . ?
Cl4 U1 C28 96.99(15) . . ?
Cl1 U1 C28 87.25(13) . . ?
Cl3 U1 C28 78.53(13) . . ?
Cl2 U1 C28 98.98(15) . . ?
C1 U1 C28 173.55(19) . . ?
N1 C1 N2 103.8(6) . . ?
N1 C1 U1 128.2(4) . . ?
N2 C1 U1 127.5(4) . . ?
C1 N1 C2 111.7(5) . . ?
C1 N1 C4 127.9(5) . . ?
C2 N1 C4 120.4(5) . . ?
C1 N2 C3 111.0(6) . . ?
C1 N2 C16 128.6(5) . . ?
C3 N2 C16 120.2(5) . . ?
C3 C2 N1 106.2(6) . . ?
C2 C3 N2 107.3(6) . . ?
C9 C4 C5 123.5(7) . . ?
C9 C4 N1 118.7(6) . . ?
C5 C4 N1 117.7(6) . . ?
C6 C5 C4 116.2(7) . . ?
C6 C5 C10 121.1(7) . . ?
C4 C5 C10 122.7(6) . . ?
C7 C6 C5 121.8(8) . . ?
C6 C7 C8 119.9(8) . . ?
C7 C8 C9 122.3(8) . . ?
C8 C9 C4 116.3(7) . . ?
C8 C9 C13 121.6(8) . . ?
C4 C9 C13 122.0(7) . . ?
C5 C10 C11 110.6(6) . . ?
C5 C10 C12 113.1(8) . . ?
C11 C10 C12 109.5(7) . . ?
C9 C13 C15 112.7(8) . . ?
C9 C13 C14 110.5(6) . . ?
C15 C13 C14 110.6(7) . . ?
C21 C16 C17 122.7(6) . . ?
C21 C16 N2 119.5(6) . . ?
C17 C16 N2 117.6(6) . . ?
C18 C17 C16 116.4(7) . . ?
C18 C17 C22 121.5(6) . . ?
C16 C17 C22 122.1(6) . . ?
C19 C18 C17 121.4(7) . . ?
C18 C19 C20 121.0(7) . . ?
C19 C20 C21 120.7(7) . . ?
C16 C21 C20 117.8(6) . . ?
C16 C21 C25 122.3(6) . . ?
C20 C21 C25 119.9(7) . . ?
C17 C22 C23 113.3(7) . . ?
C17 C22 C24 111.2(6) . . ?
C23 C22 C24 110.0(6) . . ?
C27 C25 C21 112.7(6) . . ?
C27 C25 C26 110.8(6) . . ?
C21 C25 C26 110.9(6) . . ?
N3 C28 N4 103.5(5) . . ?
N3 C28 U1 129.7(4) . . ?
N4 C28 U1 126.4(4) . . ?
C28 N3 C29 111.7(5) . . ?
C28 N3 C31 127.0(5) . . ?
C29 N3 C31 121.0(5) . . ?
C28 N4 C30 111.2(5) . . ?
C28 N4 C43 126.2(5) . . ?
C30 N4 C43 122.5(5) . . ?
C30 C29 N3 106.3(6) . . ?
C29 C30 N4 107.4(6) . . ?
C32 C31 C36 122.6(6) . . ?
C32 C31 N3 117.9(6) . . ?
C36 C31 N3 119.4(6) . . ?
C33 C32 C31 117.0(7) . . ?
C33 C32 C37 120.8(7) . . ?
C31 C32 C37 122.2(6) . . ?
C34 C33 C32 122.3(8) . . ?
C33 C34 C35 119.0(7) . . ?
C36 C35 C34 121.6(8) . . ?
C35 C36 C31 117.3(7) . . ?
C35 C36 C40 121.8(7) . . ?
C31 C36 C40 120.9(6) . . ?
C32 C37 C39 112.1(8) . . ?
C32 C37 C38 110.9(7) . . ?
C39 C37 C38 109.5(8) . . ?
C41 C40 C36 111.4(6) . . ?
C41 C40 C42 110.0(7) . . ?
C36 C40 C42 111.6(7) . . ?
C44 C43 C48 123.1(6) . . ?
C44 C43 N4 119.2(6) . . ?
C48 C43 N4 117.4(6) . . ?
C43 C44 C45 117.5(7) . . ?
C43 C44 C49 122.6(6) . . ?
C45 C44 C49 120.0(6) . . ?
C46 C45 C44 121.3(7) . . ?
C47 C46 C45 119.7(7) . . ?
C46 C47 C48 122.1(7) . . ?
C47 C48 C43 116.4(7) . . ?
C47 C48 C52 121.8(6) . . ?
C43 C48 C52 121.9(6) . . ?
C44 C49 C50 109.1(6) . . ?
C44 C49 C51 114.0(6) . . ?
C50 C49 C51 110.5(6) . . ?
C48 C52 C54 112.3(6) . . ?
C48 C52 C53 110.7(6) . . ?
C54 C52 C53 109.7(6) . . ?
C55 O1 C58 111.1(8) . . ?
O1 C55 C56 110.1(8) . . ?
C57 C56 C55 103.5(9) . . ?
C58 C57 C56 108.2(9) . . ?
O1 C58 C57 106.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        22.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.852
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.111