#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:05:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179775 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/71/7007181.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7007181
loop_
_publ_author_name
'Salmon, Lionel'
'Thuéry, Pierre'
'Asfari, Zouhair'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis, crystal structure and reactivity of uranium(IV) complexes
 with p-tert-butylcalix[4]arene ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3006
_journal_page_last               3014
_journal_paper_doi               10.1039/b601237j
_journal_year                    2006
_chemical_formula_sum            'C66 H78 Cl2 N4 O4 U'
_chemical_formula_weight         1300.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.4167(7)
_cell_angle_beta                 98.0981(7)
_cell_angle_gamma                119.1892(8)
_cell_formula_units_Z            2
_cell_length_a                   13.9922(3)
_cell_length_b                   14.1147(3)
_cell_length_c                   18.5727(4)
_cell_measurement_reflns_used    97131
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.92
_cell_volume                     3070.59(12)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and three ω scans with 2° steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            97131
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         11656
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+25.4564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                11201
_reflns_number_total             11656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601237j.txt
_cod_data_source_block           2.2py
_cod_database_code               7007181
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.433043(19) 0.074419(18) 0.250209(11) 0.01846(7) Uani 1 1 d . . .
Cl1 Cl 0.37274(13) -0.11443(12) 0.29965(8) 0.0262(3) Uani 1 1 d . . .
Cl2 Cl 0.62497(12) 0.13718(13) 0.20176(7) 0.0259(3) Uani 1 1 d . . .
O1 O 0.3670(3) 0.1266(3) 0.33400(19) 0.0187(8) Uani 1 1 d . . .
O2 O 0.2141(3) -0.0643(3) 0.1972(2) 0.0201(8) Uani 1 1 d . . .
O3 O 0.3789(3) 0.1374(3) 0.1662(2) 0.0194(8) Uani 1 1 d . . .
O4 O 0.5699(3) 0.2924(3) 0.3031(2) 0.0183(8) Uani 1 1 d . . .
N1 N 0.5857(4) 0.1132(4) 0.3744(3) 0.0253(11) Uani 1 1 d . . .
N2 N 0.3975(4) -0.0772(4) 0.1270(3) 0.0262(11) Uani 1 1 d . . .
C1 C 0.3849(5) 0.2580(4) 0.4395(3) 0.0181(11) Uani 1 1 d . . .
C2 C 0.3240(4) 0.1511(4) 0.3891(3) 0.0163(10) Uani 1 1 d . . .
C3 C 0.2178(5) 0.0707(5) 0.3961(3) 0.0181(11) Uani 1 1 d . . .
C4 C 0.1744(5) 0.0973(5) 0.4540(3) 0.0203(11) Uani 1 1 d . . .
H4 H 0.1047 0.0430 0.4590 0.024 Uiso 1 1 calc R . .
C5 C 0.2325(5) 0.2029(5) 0.5047(3) 0.0209(11) Uani 1 1 d . . .
C6 C 0.3372(5) 0.2806(5) 0.4963(3) 0.0207(11) Uani 1 1 d . . .
H6 H 0.3776 0.3509 0.5298 0.025 Uiso 1 1 calc R . .
C7 C 0.1788(5) 0.2291(5) 0.5653(3) 0.0244(12) Uani 1 1 d . . .
C8 C 0.1637(5) 0.1522(5) 0.6194(3) 0.0302(14) Uani 1 1 d . . .
H8A H 0.2358 0.1633 0.6417 0.045 Uiso 1 1 calc R . .
H8B H 0.1138 0.0754 0.5920 0.045 Uiso 1 1 calc R . .
H8C H 0.1321 0.1701 0.6581 0.045 Uiso 1 1 calc R . .
C9 C 0.0626(5) 0.2082(6) 0.5271(4) 0.0325(14) Uani 1 1 d . . .
H9A H 0.0145 0.1310 0.5000 0.049 Uiso 1 1 calc R . .
H9B H 0.0720 0.2551 0.4929 0.049 Uiso 1 1 calc R . .
H9C H 0.0289 0.2253 0.5647 0.049 Uiso 1 1 calc R . .
C10 C 0.2506(6) 0.3517(6) 0.6107(4) 0.0410(17) Uani 1 1 d . . .
H10A H 0.2612 0.4000 0.5773 0.061 Uiso 1 1 calc R . .
H10B H 0.3227 0.3665 0.6366 0.061 Uiso 1 1 calc R . .
H10C H 0.2127 0.3652 0.6465 0.061 Uiso 1 1 calc R . .
C11 C 0.1468(5) -0.0376(4) 0.3355(3) 0.0180(11) Uani 1 1 d . . .
H11A H 0.0829 -0.0905 0.3518 0.022 Uiso 1 1 calc R . .
H11B H 0.1915 -0.0707 0.3249 0.022 Uiso 1 1 calc R . .
C12 C 0.1057(5) -0.0107(4) 0.2654(3) 0.0187(11) Uani 1 1 d . . .
C13 C 0.1434(5) -0.0202(4) 0.2001(3) 0.0175(11) Uani 1 1 d . . .
C14 C 0.1147(5) 0.0151(5) 0.1394(3) 0.0191(11) Uani 1 1 d . . .
C15 C 0.0458(5) 0.0605(5) 0.1440(3) 0.0216(12) Uani 1 1 d . . .
H15 H 0.0283 0.0868 0.1042 0.026 Uiso 1 1 calc R . .
C16 C 0.0025(5) 0.0674(5) 0.2065(3) 0.0220(12) Uani 1 1 d . . .
C17 C 0.0338(5) 0.0304(5) 0.2660(3) 0.0209(11) Uani 1 1 d . . .
H17 H 0.0052 0.0335 0.3080 0.025 Uiso 1 1 calc R . .
C18 C -0.0838(6) 0.1048(6) 0.2090(3) 0.0307(14) Uani 1 1 d . . .
C19 C -0.0456(8) 0.1947(7) 0.2806(4) 0.050(2) Uani 1 1 d . . .
H19A H 0.0264 0.2582 0.2821 0.075 Uiso 1 1 calc R . .
H19B H -0.0390 0.1655 0.3233 0.075 Uiso 1 1 calc R . .
H19C H -0.1000 0.2174 0.2815 0.075 Uiso 1 1 calc R . .
C20 C -0.1010(6) 0.1510(6) 0.1419(4) 0.0356(16) Uani 1 1 d . . .
H20A H -0.1317 0.0930 0.0964 0.053 Uiso 1 1 calc R . .
H20B H -0.0298 0.2123 0.1399 0.053 Uiso 1 1 calc R . .
H20C H -0.1523 0.1767 0.1473 0.053 Uiso 1 1 calc R . .
C21 C -0.1963(5) 0.0048(6) 0.2087(5) 0.0407(17) Uani 1 1 d . . .
H21A H -0.1880 -0.0223 0.2522 0.061 Uiso 1 1 calc R . .
H21B H -0.2208 -0.0535 0.1642 0.061 Uiso 1 1 calc R . .
H21C H -0.2512 0.0269 0.2093 0.061 Uiso 1 1 calc R . .
C22 C 0.1563(5) 0.0059(5) 0.0689(3) 0.0204(11) Uani 1 1 d . . .
H22A H 0.1875 -0.0421 0.0702 0.025 Uiso 1 1 calc R . .
H22B H 0.0927 -0.0292 0.0254 0.025 Uiso 1 1 calc R . .
C23 C 0.2447(5) 0.1176(5) 0.0605(3) 0.0196(11) Uani 1 1 d . . .
C24 C 0.3522(5) 0.1793(4) 0.1108(3) 0.0168(11) Uani 1 1 d . . .
C25 C 0.4313(5) 0.2852(5) 0.1044(3) 0.0188(11) Uani 1 1 d . . .
C26 C 0.4035(5) 0.3275(5) 0.0469(3) 0.0206(11) Uani 1 1 d . . .
H26 H 0.4574 0.3972 0.0421 0.025 Uiso 1 1 calc R . .
C27 C 0.2971(5) 0.2687(5) -0.0040(3) 0.0206(11) Uani 1 1 d . . .
C28 C 0.2199(5) 0.1645(5) 0.0044(3) 0.0210(11) Uani 1 1 d . . .
H28 H 0.1486 0.1239 -0.0285 0.025 Uiso 1 1 calc R . .
C29 C 0.2696(5) 0.3226(5) -0.0633(3) 0.0241(12) Uani 1 1 d . . .
C30 C 0.2909(6) 0.4374(5) -0.0243(4) 0.0313(14) Uani 1 1 d . . .
H30A H 0.3692 0.4854 0.0016 0.047 Uiso 1 1 calc R . .
H30B H 0.2450 0.4280 0.0110 0.047 Uiso 1 1 calc R . .
H30C H 0.2719 0.4704 -0.0613 0.047 Uiso 1 1 calc R . .
C31 C 0.1463(5) 0.2511(5) -0.1075(4) 0.0347(16) Uani 1 1 d . . .
H31A H 0.0982 0.2414 -0.0737 0.052 Uiso 1 1 calc R . .
H31B H 0.1313 0.1792 -0.1331 0.052 Uiso 1 1 calc R . .
H31C H 0.1320 0.2877 -0.1436 0.052 Uiso 1 1 calc R . .
C32 C 0.3449(5) 0.3379(5) -0.1185(3) 0.0291(14) Uani 1 1 d . . .
H32A H 0.3305 0.2661 -0.1436 0.044 Uiso 1 1 calc R . .
H32B H 0.4228 0.3842 -0.0916 0.044 Uiso 1 1 calc R . .
H32C H 0.3284 0.3730 -0.1550 0.044 Uiso 1 1 calc R . .
C33 C 0.5404(5) 0.3569(5) 0.1648(3) 0.0196(11) Uani 1 1 d . . .
H33A H 0.5928 0.4209 0.1485 0.024 Uiso 1 1 calc R . .
H33B H 0.5752 0.3137 0.1749 0.024 Uiso 1 1 calc R . .
C34 C 0.5128(5) 0.3963(5) 0.2353(3) 0.0193(11) Uani 1 1 d . . .
C35 C 0.5224(5) 0.3597(4) 0.2995(3) 0.0185(11) Uani 1 1 d . . .
C36 C 0.4852(5) 0.3869(5) 0.3605(3) 0.0192(11) Uani 1 1 d . . .
C37 C 0.4381(5) 0.4541(5) 0.3559(3) 0.0205(11) Uani 1 1 d . . .
H37 H 0.4118 0.4716 0.3960 0.025 Uiso 1 1 calc R . .
C38 C 0.4294(5) 0.4954(5) 0.2937(3) 0.0228(12) Uani 1 1 d . . .
C39 C 0.4673(5) 0.4648(5) 0.2335(3) 0.0219(12) Uani 1 1 d . . .
H39 H 0.4618 0.4911 0.1909 0.026 Uiso 1 1 calc R . .
C40 C 0.3874(6) 0.5775(6) 0.2896(3) 0.0350(16) Uani 1 1 d . . .
C41 C 0.2950(8) 0.5357(9) 0.2195(5) 0.065(3) Uani 1 1 d U . .
H41A H 0.3242 0.5315 0.1761 0.098 Uiso 1 1 calc R . .
H41B H 0.2679 0.5864 0.2193 0.098 Uiso 1 1 calc R . .
H41C H 0.2341 0.4627 0.2184 0.098 Uiso 1 1 calc R . .
C42 C 0.3440(7) 0.5972(6) 0.3582(4) 0.0402(17) Uani 1 1 d . . .
H42A H 0.3200 0.6497 0.3538 0.060 Uiso 1 1 calc R . .
H42B H 0.4034 0.6267 0.4029 0.060 Uiso 1 1 calc R . .
H42C H 0.2814 0.5276 0.3608 0.060 Uiso 1 1 calc R . .
C43 C 0.4873(9) 0.6911(7) 0.2878(6) 0.067(3) Uani 1 1 d U . .
H43A H 0.5138 0.6821 0.2438 0.100 Uiso 1 1 calc R . .
H43B H 0.5473 0.7180 0.3318 0.100 Uiso 1 1 calc R . .
H43C H 0.4632 0.7440 0.2866 0.100 Uiso 1 1 calc R . .
C44 C 0.4975(5) 0.3481(5) 0.4312(3) 0.0187(11) Uani 1 1 d . . .
H44A H 0.5477 0.3193 0.4301 0.022 Uiso 1 1 calc R . .
H44B H 0.5313 0.4116 0.4745 0.022 Uiso 1 1 calc R . .
C45 C 0.1492(5) -0.1855(5) 0.1695(3) 0.0267(13) Uani 1 1 d . . .
H45A H 0.1055 -0.2055 0.1191 0.040 Uiso 1 1 calc R . .
H45B H 0.0994 -0.2179 0.2011 0.040 Uiso 1 1 calc R . .
H45C H 0.1996 -0.2133 0.1699 0.040 Uiso 1 1 calc R . .
C46 C 0.6912(5) 0.3587(5) 0.3308(3) 0.0238(12) Uani 1 1 d . . .
H46A H 0.7102 0.3996 0.3819 0.036 Uiso 1 1 calc R . .
H46B H 0.7228 0.4104 0.3005 0.036 Uiso 1 1 calc R . .
H46C H 0.7212 0.3103 0.3286 0.036 Uiso 1 1 calc R . .
C47 C 0.5651(5) 0.1308(5) 0.4428(3) 0.0264(13) Uani 1 1 d . . .
H47 H 0.5089 0.1473 0.4464 0.032 Uiso 1 1 calc R . .
C48 C 0.6227(6) 0.1256(5) 0.5072(3) 0.0315(14) Uani 1 1 d . . .
H48 H 0.6069 0.1403 0.5532 0.038 Uiso 1 1 calc R . .
C49 C 0.7043(6) 0.0982(6) 0.5025(4) 0.0395(17) Uani 1 1 d . . .
H49 H 0.7433 0.0926 0.5449 0.047 Uiso 1 1 calc R . .
C50 C 0.7268(7) 0.0793(7) 0.4333(4) 0.0458(19) Uani 1 1 d . . .
H50 H 0.7814 0.0608 0.4285 0.055 Uiso 1 1 calc R . .
C51 C 0.6671(6) 0.0883(6) 0.3714(4) 0.0364(16) Uani 1 1 d . . .
H51 H 0.6838 0.0766 0.3254 0.044 Uiso 1 1 calc R . .
C52 C 0.4239(6) -0.1562(6) 0.1311(4) 0.0358(15) Uani 1 1 d . . .
H52 H 0.4399 -0.1686 0.1779 0.043 Uiso 1 1 calc R . .
C53 C 0.4284(7) -0.2201(7) 0.0688(4) 0.0453(19) Uani 1 1 d . . .
H53 H 0.4476 -0.2736 0.0740 0.054 Uiso 1 1 calc R . .
C54 C 0.4038(6) -0.2028(6) -0.0010(4) 0.0407(17) Uani 1 1 d . . .
H54 H 0.4054 -0.2450 -0.0437 0.049 Uiso 1 1 calc R . .
C55 C 0.3768(5) -0.1219(6) -0.0060(3) 0.0323(14) Uani 1 1 d . . .
H55 H 0.3599 -0.1084 -0.0522 0.039 Uiso 1 1 calc R . .
C56 C 0.3752(5) -0.0613(5) 0.0587(3) 0.0256(13) Uani 1 1 d . . .
H56 H 0.3577 -0.0063 0.0547 0.031 Uiso 1 1 calc R . .
N3 N 0.8623(8) 0.5546(8) 0.2149(6) 0.077(2) Uani 1 1 d U . .
C57 C 0.9437(8) 0.6338(8) 0.2735(6) 0.058(2) Uani 1 1 d . . .
H57 H 0.9410 0.6974 0.2910 0.069 Uiso 1 1 calc R . .
C58 C 1.0282(10) 0.6258(10) 0.3077(6) 0.078(3) Uani 1 1 d U . .
H58 H 1.0833 0.6819 0.3487 0.094 Uiso 1 1 calc R . .
C59 C 1.0319(11) 0.5315(12) 0.2804(8) 0.107(4) Uani 1 1 d U . .
H59 H 1.0917 0.5248 0.3021 0.128 Uiso 1 1 calc R . .
C60 C 0.9467(12) 0.4468(12) 0.2208(8) 0.106(4) Uani 1 1 d U . .
H60 H 0.9456 0.3812 0.2029 0.127 Uiso 1 1 calc R . .
C61 C 0.8659(9) 0.4646(8) 0.1904(5) 0.064(2) Uani 1 1 d . . .
H61 H 0.8090 0.4099 0.1495 0.077 Uiso 1 1 calc R . .
C62 C 0.1089(10) -0.4490(11) 0.0401(6) 0.080(3) Uani 1 1 d U . .
C63 C 0.0764(9) -0.3935(9) -0.0038(6) 0.075(3) Uani 1 1 d . . .
C64 C -0.0336(9) -0.4452(10) -0.0452(6) 0.078(3) Uani 1 1 d . . .
C65 C 0.9374(10) 0.5309(10) 0.5406(6) 0.077(3) Uani 1 1 d . . .
C66 C 0.8943(9) 0.4214(9) 0.5026(6) 0.072(3) Uani 1 1 d U . .
C67 C 0.9553(10) 0.3931(9) 0.4624(6) 0.074(3) Uani 1 1 d U . .
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'
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 O1 95.94(14) . . ?
O3 U O2 73.15(13) . . ?
O1 U O2 77.97(13) . . ?
O3 U O4 78.05(13) . . ?
O1 U O4 73.18(13) . . ?
O2 U O4 136.40(11) . . ?
O3 U N2 80.73(14) . . ?
O1 U N2 148.75(15) . . ?
O2 U N2 71.30(13) . . ?
O4 U N2 134.91(14) . . ?
O3 U N1 148.81(15) . . ?
O1 U N1 80.43(14) . . ?
O2 U N1 134.72(13) . . ?
O4 U N1 71.22(13) . . ?
N2 U N1 117.82(15) . . ?
O3 U Cl2 88.69(11) . . ?
O1 U Cl2 142.51(11) . . ?
O2 U Cl2 138.18(8) . . ?
O4 U Cl2 71.47(8) . . ?
N2 U Cl2 68.72(11) . . ?
N1 U Cl2 76.80(11) . . ?
O3 U Cl1 142.58(11) . . ?
O1 U Cl1 88.44(10) . . ?
O2 U Cl1 71.50(9) . . ?
O4 U Cl1 137.97(8) . . ?
N2 U Cl1 76.74(11) . . ?
N1 U Cl1 68.58(11) . . ?
Cl2 U Cl1 109.93(4) . . ?
C2 O1 U 174.6(3) . . ?
C13 O2 C45 111.4(4) . . ?
C13 O2 U 118.0(3) . . ?
C45 O2 U 130.4(3) . . ?
C24 O3 U 175.3(3) . . ?
C35 O4 C46 111.8(4) . . ?
C35 O4 U 117.3(3) . . ?
C46 O4 U 130.6(3) . . ?
C51 N1 C47 116.3(5) . . ?
C51 N1 U 122.2(4) . . ?
C47 N1 U 119.4(4) . . ?
C56 N2 C52 116.8(5) . . ?
C56 N2 U 119.8(4) . . ?
C52 N2 U 122.0(4) . . ?
C6 C1 C2 118.5(5) . . ?
C6 C1 C44 120.4(5) . . ?
C2 C1 C44 121.0(5) . . ?
O1 C2 C3 120.0(5) . . ?
O1 C2 C1 120.1(5) . . ?
C3 C2 C1 119.9(5) . . ?
C4 C3 C2 119.3(5) . . ?
C4 C3 C11 121.2(5) . . ?
C2 C3 C11 119.1(5) . . ?
C3 C4 C5 122.1(5) . . ?
C6 C5 C4 117.2(5) . . ?
C6 C5 C7 122.9(5) . . ?
C4 C5 C7 120.0(5) . . ?
C5 C6 C1 123.0(5) . . ?
C10 C7 C5 112.1(5) . . ?
C10 C7 C9 107.6(5) . . ?
C5 C7 C9 109.0(5) . . ?
C10 C7 C8 109.0(5) . . ?
C5 C7 C8 109.6(5) . . ?
C9 C7 C8 109.6(5) . . ?
C3 C11 C12 107.9(4) . . ?
C17 C12 C13 117.8(5) . . ?
C17 C12 C11 120.2(5) . . ?
C13 C12 C11 121.9(5) . . ?
C14 C13 C12 121.6(5) . . ?
C14 C13 O2 119.4(5) . . ?
C12 C13 O2 119.0(5) . . ?
C13 C14 C15 118.4(5) . . ?
C13 C14 C22 121.7(5) . . ?
C15 C14 C22 119.9(5) . . ?
C16 C15 C14 122.1(5) . . ?
C17 C16 C15 117.2(5) . . ?
C17 C16 C18 119.9(5) . . ?
C15 C16 C18 122.7(5) . . ?
C12 C17 C16 122.9(5) . . ?
C21 C18 C19 108.5(6) . . ?
C21 C18 C20 108.4(6) . . ?
C19 C18 C20 108.4(6) . . ?
C21 C18 C16 108.7(5) . . ?
C19 C18 C16 110.2(5) . . ?
C20 C18 C16 112.6(5) . . ?
C23 C22 C14 112.9(5) . . ?
C28 C23 C24 118.7(5) . . ?
C28 C23 C22 120.6(5) . . ?
C24 C23 C22 120.6(5) . . ?
O3 C24 C25 119.7(5) . . ?
O3 C24 C23 120.5(5) . . ?
C25 C24 C23 119.8(5) . . ?
C26 C25 C24 119.4(5) . . ?
C26 C25 C33 121.1(5) . . ?
C24 C25 C33 119.2(5) . . ?
C25 C26 C27 122.3(5) . . ?
C28 C27 C26 117.0(5) . . ?
C28 C27 C29 123.2(5) . . ?
C26 C27 C29 119.8(5) . . ?
C27 C28 C23 122.8(5) . . ?
C31 C29 C27 111.8(5) . . ?
C31 C29 C32 108.5(5) . . ?
C27 C29 C32 109.7(5) . . ?
C31 C29 C30 108.0(5) . . ?
C27 C29 C30 109.4(5) . . ?
C32 C29 C30 109.4(5) . . ?
C25 C33 C34 108.0(4) . . ?
C35 C34 C39 118.2(5) . . ?
C35 C34 C33 122.6(5) . . ?
C39 C34 C33 119.0(5) . . ?
C34 C35 C36 121.8(5) . . ?
C34 C35 O4 119.1(5) . . ?
C36 C35 O4 119.1(5) . . ?
C35 C36 C37 118.2(5) . . ?
C35 C36 C44 121.6(5) . . ?
C37 C36 C44 120.2(5) . . ?
C38 C37 C36 122.4(5) . . ?
C37 C38 C39 117.1(5) . . ?
C37 C38 C40 123.6(5) . . ?
C39 C38 C40 119.1(5) . . ?
C34 C39 C38 122.3(5) . . ?
C41 C40 C42 109.0(6) . . ?
C41 C40 C38 111.0(6) . . ?
C42 C40 C38 112.2(5) . . ?
C41 C40 C43 108.7(7) . . ?
C42 C40 C43 107.6(6) . . ?
C38 C40 C43 108.3(6) . . ?
C1 C44 C36 112.0(4) . . ?
N1 C47 C48 123.7(6) . . ?
C47 C48 C49 118.9(6) . . ?
C48 C49 C50 118.7(6) . . ?
C51 C50 C49 119.0(6) . . ?
N1 C51 C50 123.4(6) . . ?
N2 C52 C53 123.1(6) . . ?
C54 C53 C52 118.9(6) . . ?
C55 C54 C53 118.6(6) . . ?
C54 C55 C56 119.0(6) . . ?
N2 C56 C55 123.6(6) . . ?
C61 N3 C57 118.6(9) . . ?
C58 C57 N3 122.9(9) . . ?
C57 C58 C59 117.9(11) . . ?
C58 C59 C60 120.2(11) . . ?
C61 C60 C59 116.5(11) . . ?
N3 C61 C60 123.9(11) . . ?
C64 C62 C63 121.8(11) 2_545 . ?
C64 C63 C62 120.1(10) . . ?
C62 C64 C63 118.1(11) 2_545 . ?
C67 C65 C66 116.2(11) 2_766 . ?
C67 C66 C65 120.9(10) . . ?
C66 C67 C65 122.9(10) . 2_766 ?
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 2.128(4) . ?
U O1 2.134(4) . ?
U O2 2.631(4) . ?
U O4 2.634(4) . ?
U N2 2.696(5) . ?
U N1 2.698(5) . ?
U Cl2 2.7204(14) . ?
U Cl1 2.7205(14) . ?
O1 C2 1.342(6) . ?
O2 C13 1.406(6) . ?
O2 C45 1.453(7) . ?
O3 C24 1.354(6) . ?
O4 C35 1.404(6) . ?
O4 C46 1.444(6) . ?
N1 C51 1.352(8) . ?
N1 C47 1.356(7) . ?
N2 C56 1.341(7) . ?
N2 C52 1.343(8) . ?
C1 C6 1.403(7) . ?
C1 C2 1.410(8) . ?
C1 C44 1.514(8) . ?
C2 C3 1.402(8) . ?
C3 C4 1.398(7) . ?
C3 C11 1.514(7) . ?
C4 C5 1.401(8) . ?
C5 C6 1.385(8) . ?
C5 C7 1.534(7) . ?
C7 C10 1.534(8) . ?
C7 C9 1.543(9) . ?
C7 C8 1.546(8) . ?
C11 C12 1.521(7) . ?
C12 C17 1.386(8) . ?
C12 C13 1.403(7) . ?
C13 C14 1.383(7) . ?
C14 C15 1.398(8) . ?
C14 C22 1.520(7) . ?
C15 C16 1.395(8) . ?
C16 C17 1.393(8) . ?
C16 C18 1.539(8) . ?
C18 C21 1.515(9) . ?
C18 C19 1.519(9) . ?
C18 C20 1.531(8) . ?
C22 C23 1.505(8) . ?
C23 C28 1.403(7) . ?
C23 C24 1.408(8) . ?
C24 C25 1.396(8) . ?
C25 C26 1.395(7) . ?
C25 C33 1.514(7) . ?
C26 C27 1.402(8) . ?
C27 C28 1.386(8) . ?
C27 C29 1.533(7) . ?
C29 C31 1.526(8) . ?
C29 C32 1.535(8) . ?
C29 C30 1.537(8) . ?
C33 C34 1.520(7) . ?
C34 C35 1.383(7) . ?
C34 C39 1.395(8) . ?
C35 C36 1.390(7) . ?
C36 C37 1.399(8) . ?
C36 C44 1.514(7) . ?
C37 C38 1.384(8) . ?
C38 C39 1.402(8) . ?
C38 C40 1.538(8) . ?
C40 C41 1.507(10) . ?
C40 C42 1.533(9) . ?
C40 C43 1.539(12) . ?
C47 C48 1.378(8) . ?
C48 C49 1.381(10) . ?
C49 C50 1.385(10) . ?
C50 C51 1.382(9) . ?
C52 C53 1.388(9) . ?
C53 C54 1.381(10) . ?
C54 C55 1.377(10) . ?
C55 C56 1.379(8) . ?
N3 C61 1.312(12) . ?
N3 C57 1.335(13) . ?
C57 C58 1.324(13) . ?
C58 C59 1.380(15) . ?
C59 C60 1.388(17) . ?
C60 C61 1.341(15) . ?
C62 C64 1.373(16) 2_545 ?
C62 C63 1.384(16) . ?
C63 C64 1.378(15) . ?
C64 C62 1.373(16) 2_545 ?
C65 C67 1.370(16) 2_766 ?
C65 C66 1.379(15) . ?
C66 C67 1.368(15) . ?
C67 C65 1.370(16) 2_766 ?
