#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:52:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179214 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314235.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_4314235
loop_
_publ_author_name
'Lydia Karmazin'
'Marinella Mazzanti'
'Jacques Pécaut'
_publ_section_title
;
 Oxidation Chemistry of Uranium(III) Complexes of Tpa: Synthesis and
 Structural Studies of Oxo, Hydroxo, and Alkoxo Complexes of Uranium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5900
_journal_page_last               5908
_journal_paper_doi               10.1021/ic0343004
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C60 H66 I6 N15 O3 U3'
_chemical_formula_weight         2520.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.4080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1347(14)
_cell_length_b                   13.8063(9)
_cell_length_c                   25.8860(16)
_cell_measurement_temperature    143(2)
_cell_volume                     7754.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36704
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    8.687
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            light_brown
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.5
_refine_diff_density_max         5.326
_refine_diff_density_min         -3.809
_refine_diff_density_rms         0.407
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         13252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                11127
_reflns_number_total             13252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343004si20030702_093145_3.cif
_cod_data_source_block           complex3,[U(tpa)(m-O)I]3(m3-I)}I2.3CH3CN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314235
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.141467(13) 0.108032(18) 0.847201(10) 0.01449(7) Uani 1 1 d . . .
U2 U 0.207080(13) -0.111719(18) 0.934883(10) 0.01617(7) Uani 1 1 d . . .
U3 U 0.204051(13) 0.144913(18) 0.995872(10) 0.01607(7) Uani 1 1 d . . .
I1 I 0.03047(2) -0.02224(3) 0.783370(18) 0.02109(12) Uani 1 1 d . . .
I2 I 0.17673(2) -0.20194(4) 1.040141(19) 0.02632(13) Uani 1 1 d . . .
I3 I 0.08732(2) 0.28398(3) 0.998962(18) 0.02186(12) Uani 1 1 d . . .
I4 I 0.08379(2) 0.01403(3) 0.944291(17) 0.01667(11) Uani 1 1 d . . .
O1 O 0.1875(2) -0.0218(3) 0.86503(17) 0.0159(12) Uani 1 1 d . . .
H1O H 0.2036 -0.0474 0.8364 0.019 Uiso 1 1 calc R . .
O2 O 0.1882(2) 0.1826(3) 0.91645(18) 0.0166(12) Uani 1 1 d . . .
H2O H 0.2046 0.2438 0.9096 0.020 Uiso 1 1 calc R . .
O3 O 0.2400(2) 0.0045(4) 0.98319(18) 0.0200(13) Uani 1 1 d . . .
H3O H 0.2796 -0.0070 1.0043 0.024 Uiso 1 1 calc R . .
N1 N 0.2483(3) 0.3045(4) 1.0452(2) 0.0200(15) Uani 1 1 d . . .
N2 N 0.1676(3) 0.0711(4) 1.0794(2) 0.0179(15) Uani 1 1 d . . .
N3 N 0.3155(3) 0.1904(4) 0.9852(2) 0.0232(16) Uani 1 1 d . . .
N4 N 0.2906(3) 0.1209(5) 1.0828(2) 0.0238(17) Uani 1 1 d . . .
N21 N 0.0482(3) 0.2280(4) 0.8501(2) 0.0228(16) Uani 1 1 d . . .
N22 N 0.1417(3) 0.1243(4) 0.7462(2) 0.0217(16) Uani 1 1 d . . .
N23 N 0.2473(3) 0.1506(4) 0.8210(2) 0.0207(15) Uani 1 1 d . . .
N24 N 0.1508(3) 0.2878(4) 0.8129(2) 0.0197(15) Uani 1 1 d . . .
N41 N 0.1119(3) -0.2213(4) 0.8901(2) 0.0203(15) Uani 1 1 d . . .
N42 N 0.3144(3) -0.0941(4) 0.9105(2) 0.0219(16) Uani 1 1 d . . .
N43 N 0.2849(3) -0.2541(5) 0.9636(3) 0.0347(19) Uani 1 1 d . . .
N44 N 0.2253(3) -0.2303(4) 0.8592(2) 0.0198(15) Uani 1 1 d . . .
C1 C 0.2923(4) 0.2030(5) 1.1191(3) 0.025(2) Uani 1 1 d . . .
H1A H 0.3316 0.2013 1.1451 0.030 Uiso 1 1 calc R . .
H1B H 0.2582 0.1961 1.1385 0.030 Uiso 1 1 calc R . .
C2 C 0.2865(4) 0.2983(6) 1.0917(3) 0.028(2) Uani 1 1 d . . .
C3 C 0.3179(4) 0.3833(6) 1.1152(3) 0.034(2) Uani 1 1 d . . .
H3 H 0.3463 0.3789 1.1478 0.040 Uiso 1 1 calc R . .
C4 C 0.3066(5) 0.4700(7) 1.0904(4) 0.052(3) Uani 1 1 d . . .
H4 H 0.3267 0.5263 1.1065 0.063 Uiso 1 1 calc R . .
C5 C 0.2662(4) 0.4784(6) 1.0420(4) 0.042(3) Uani 1 1 d . . .
H5 H 0.2576 0.5383 1.0240 0.051 Uiso 1 1 calc R . .
C6 C 0.2396(4) 0.3910(6) 1.0222(3) 0.032(2) Uani 1 1 d . . .
H6 H 0.2124 0.3935 0.9889 0.039 Uiso 1 1 calc R . .
C7 C 0.2757(3) 0.0303(5) 1.1101(3) 0.0230(19) Uani 1 1 d . . .
H7A H 0.3040 0.0247 1.1447 0.028 Uiso 1 1 calc R . .
H7B H 0.2822 -0.0268 1.0887 0.028 Uiso 1 1 calc R . .
C8 C 0.2100(4) 0.0310(5) 1.1180(3) 0.023(2) Uani 1 1 d . . .
C9 C 0.1942(4) -0.0114(5) 1.1615(3) 0.025(2) Uani 1 1 d . . .
H9 H 0.2251 -0.0390 1.1882 0.030 Uiso 1 1 calc R . .
C10 C 0.1338(4) -0.0135(5) 1.1658(3) 0.029(2) Uani 1 1 d . . .
H10 H 0.1222 -0.0426 1.1956 0.035 Uiso 1 1 calc R . .
C11 C 0.0887(4) 0.0276(5) 1.1259(3) 0.024(2) Uani 1 1 d . . .
H11 H 0.0464 0.0281 1.1284 0.029 Uiso 1 1 calc R . .
C12 C 0.1081(3) 0.0672(5) 1.0832(3) 0.0183(18) Uani 1 1 d . . .
H12 H 0.0780 0.0929 1.0552 0.022 Uiso 1 1 calc R . .
C13 C 0.3514(4) 0.1051(6) 1.0690(3) 0.028(2) Uani 1 1 d . . .
H13A H 0.3543 0.0369 1.0579 0.034 Uiso 1 1 calc R . .
H13B H 0.3840 0.1160 1.1006 0.034 Uiso 1 1 calc R . .
C14 C 0.3629(4) 0.1728(6) 1.0242(3) 0.028(2) Uani 1 1 d . . .
C15 C 0.4218(6) 0.2010(9) 1.0226(4) 0.061(3) Uani 1 1 d . . .
H15 H 0.4549 0.1854 1.0508 0.074 Uiso 1 1 calc R . .
C16 C 0.4327(5) 0.2535(10) 0.9789(5) 0.074(4) Uani 1 1 d . . .
H16 H 0.4729 0.2746 0.9766 0.089 Uiso 1 1 calc R . .
C17 C 0.3823(5) 0.2733(9) 0.9389(4) 0.057(3) Uani 1 1 d . . .
H17 H 0.3874 0.3102 0.9091 0.069 Uiso 1 1 calc R . .
C18 C 0.3262(4) 0.2399(7) 0.9428(3) 0.038(2) Uani 1 1 d . . .
H18 H 0.2926 0.2516 0.9144 0.046 Uiso 1 1 calc R . .
C21 C 0.1197(4) 0.3551(5) 0.8445(3) 0.0216(19) Uani 1 1 d . . .
H21A H 0.1456 0.3615 0.8802 0.026 Uiso 1 1 calc R . .
H21B H 0.1166 0.4199 0.8278 0.026 Uiso 1 1 calc R . .
C22 C 0.0572(4) 0.3233(5) 0.8497(3) 0.0191(18) Uani 1 1 d . . .
C23 C 0.0122(4) 0.3876(5) 0.8551(3) 0.029(2) Uani 1 1 d . . .
H23 H 0.0198 0.4551 0.8537 0.034 Uiso 1 1 calc R . .
C24 C -0.0430(4) 0.3562(6) 0.8626(3) 0.033(2) Uani 1 1 d . . .
H24 H -0.0740 0.4010 0.8673 0.040 Uiso 1 1 calc R . .
C25 C -0.0539(4) 0.2568(6) 0.8632(3) 0.030(2) Uani 1 1 d . . .
H25 H -0.0928 0.2324 0.8673 0.037 Uiso 1 1 calc R . .
C26 C -0.0068(4) 0.1949(5) 0.8577(3) 0.025(2) Uani 1 1 d . . .
H26 H -0.0132 0.1270 0.8592 0.029 Uiso 1 1 calc R . .
C27 C 0.1162(4) 0.2906(5) 0.7566(3) 0.0234(19) Uani 1 1 d . . .
H27A H 0.0715 0.2831 0.7559 0.028 Uiso 1 1 calc R . .
H27B H 0.1226 0.3544 0.7410 0.028 Uiso 1 1 calc R . .
C28 C 0.1369(3) 0.2131(5) 0.7248(3) 0.0209(19) Uani 1 1 d . . .
C29 C 0.1451(4) 0.2261(6) 0.6730(3) 0.024(2) Uani 1 1 d . . .
H29 H 0.1408 0.2888 0.6575 0.029 Uiso 1 1 calc R . .
C30 C 0.1593(4) 0.1493(6) 0.6449(3) 0.028(2) Uani 1 1 d . . .
H30 H 0.1638 0.1580 0.6094 0.034 Uiso 1 1 calc R . .
C31 C 0.1671(4) 0.0584(6) 0.6678(3) 0.027(2) Uani 1 1 d . . .
H31 H 0.1790 0.0045 0.6493 0.032 Uiso 1 1 calc R . .
C32 C 0.1570(4) 0.0492(5) 0.7182(3) 0.0219(19) Uani 1 1 d . . .
H32 H 0.1610 -0.0131 0.7341 0.026 Uiso 1 1 calc R . .
C33 C 0.2157(4) 0.3179(6) 0.8155(3) 0.029(2) Uani 1 1 d . . .
H33A H 0.2162 0.3716 0.7903 0.034 Uiso 1 1 calc R . .
H33B H 0.2321 0.3435 0.8513 0.034 Uiso 1 1 calc R . .
C34 C 0.2574(4) 0.2406(6) 0.8040(3) 0.028(2) Uani 1 1 d . . .
C35 C 0.3061(4) 0.2587(6) 0.7802(3) 0.034(2) Uani 1 1 d . . .
H35 H 0.3133 0.3225 0.7691 0.041 Uiso 1 1 calc R . .
C36 C 0.3441(4) 0.1857(7) 0.7725(4) 0.050(3) Uani 1 1 d . . .
H36 H 0.3773 0.1980 0.7551 0.060 Uiso 1 1 calc R . .
C37 C 0.3350(4) 0.0946(6) 0.7897(4) 0.041(3) Uani 1 1 d . . .
H37 H 0.3610 0.0424 0.7842 0.049 Uiso 1 1 calc R . .
C38 C 0.2868(4) 0.0809(6) 0.8153(3) 0.032(2) Uani 1 1 d . . .
H38 H 0.2816 0.0188 0.8296 0.038 Uiso 1 1 calc R . .
C41 C 0.1672(4) -0.2356(6) 0.8184(3) 0.027(2) Uani 1 1 d . . .
H41A H 0.1602 -0.1726 0.7999 0.033 Uiso 1 1 calc R . .
H41B H 0.1719 -0.2856 0.7920 0.033 Uiso 1 1 calc R . .
C42 C 0.1137(4) -0.2590(5) 0.8412(3) 0.023(2) Uani 1 1 d . . .
C43 C 0.0653(4) -0.3151(5) 0.8147(3) 0.029(2) Uani 1 1 d . . .
H43 H 0.0674 -0.3424 0.7814 0.035 Uiso 1 1 calc R . .
C44 C 0.0137(4) -0.3315(5) 0.8368(3) 0.025(2) Uani 1 1 d . . .
H44 H -0.0202 -0.3684 0.8187 0.030 Uiso 1 1 calc R . .
C45 C 0.0131(4) -0.2924(5) 0.8861(3) 0.026(2) Uani 1 1 d . . .
H45 H -0.0210 -0.3027 0.9027 0.031 Uiso 1 1 calc R . .
C46 C 0.0635(4) -0.2378(5) 0.9108(3) 0.0230(19) Uani 1 1 d . . .
H46 H 0.0627 -0.2111 0.9445 0.028 Uiso 1 1 calc R . .
C47 C 0.2749(4) -0.1967(5) 0.8333(3) 0.027(2) Uani 1 1 d . . .
H47A H 0.2569 -0.1522 0.8043 0.032 Uiso 1 1 calc R . .
H47B H 0.2917 -0.2533 0.8173 0.032 Uiso 1 1 calc R . .
C48 C 0.3273(4) -0.1456(5) 0.8688(3) 0.027(2) Uani 1 1 d . . .
C49 C 0.3871(4) -0.1453(6) 0.8580(3) 0.034(2) Uani 1 1 d . . .
H49 H 0.3970 -0.1855 0.8311 0.041 Uiso 1 1 calc R . .
C50 C 0.4313(4) -0.0860(7) 0.8869(4) 0.042(3) Uani 1 1 d . . .
H50 H 0.4713 -0.0827 0.8788 0.051 Uiso 1 1 calc R . .
C51 C 0.4174(4) -0.0316(8) 0.9276(3) 0.044(3) Uani 1 1 d . . .
H51 H 0.4470 0.0101 0.9480 0.052 Uiso 1 1 calc R . .
C52 C 0.3581(4) -0.0403(6) 0.9375(4) 0.037(2) Uani 1 1 d . . .
H52 H 0.3487 -0.0042 0.9661 0.045 Uiso 1 1 calc R . .
C53 C 0.2379(4) -0.3301(5) 0.8820(3) 0.035(2) Uani 1 1 d . . .
H53A H 0.2001 -0.3562 0.8918 0.042 Uiso 1 1 calc R . .
H53B H 0.2495 -0.3736 0.8552 0.042 Uiso 1 1 calc R . .
C54 C 0.2884(4) -0.3276(6) 0.9292(3) 0.035(2) Uani 1 1 d . . .
C55 C 0.3333(5) -0.3977(7) 0.9386(4) 0.056(3) Uani 1 1 d . . .
H55 H 0.3334 -0.4487 0.9140 0.067 Uiso 1 1 calc R . .
C56 C 0.3783(6) -0.3938(8) 0.9838(5) 0.071(4) Uani 1 1 d . . .
H56 H 0.4107 -0.4400 0.9899 0.085 Uiso 1 1 calc R . .
C57 C 0.3753(5) -0.3207(9) 1.0207(4) 0.069(4) Uani 1 1 d . . .
H57 H 0.4052 -0.3177 1.0525 0.083 Uiso 1 1 calc R . .
C58 C 0.3269(4) -0.2502(7) 1.0099(4) 0.048(3) Uani 1 1 d . . .
H58 H 0.3240 -0.2010 1.0350 0.057 Uiso 1 1 calc R . .
I5 I 0.32910(3) 0.54150(4) 0.78368(2) 0.04028(16) Uani 1 1 d . . .
I6 I 0.53244(4) 0.77721(10) 0.80719(5) 0.0968(4) Uani 0.6932(13) 1 d P . .
I7 I 0.44733(9) 0.62973(14) 0.60102(9) 0.0420(6) Uani 0.3068(13) 1 d P . .
N61 N 0.2187(6) -0.3349(8) 1.1975(4) 0.090(4) Uani 1 1 d . . .
C61 C 0.2584(6) -0.2975(7) 1.1851(4) 0.064(4) Uani 1 1 d . . .
C62 C 0.3091(6) -0.2513(9) 1.1694(5) 0.075(4) Uani 1 1 d . . .
N63 N 0.4893(7) 0.4619(14) 0.9368(7) 0.126(10) Uani 0.50 1 d PG . .
C65 C 0.4867(7) 0.5283(15) 0.9167(6) 0.067(7) Uani 0.50 1 d PG . .
C66 C 0.4849(13) 0.614(2) 0.8911(10) 0.103(10) Uani 0.50 1 d PG . .
N62 N 0.1409(4) -0.0353(5) 0.4341(3) 0.045(2) Uani 1 1 d . . .
C63 C 0.1140(4) -0.0482(6) 0.4670(4) 0.037(3) Uani 1 1 d . . .
C64 C 0.0790(5) -0.0662(6) 0.5095(4) 0.052(3) Uani 1 1 d . . .
N64 N 0.5714(5) 0.4306(8) 0.7887(5) 0.019(3) Uiso 0.50 1 d PG . .
C67 C 0.5460(10) 0.420(2) 0.8213(7) 0.102(10) Uiso 0.50 1 d PG . .
C68 C 0.513(2) 0.405(5) 0.8623(15) 0.30(4) Uiso 0.50 1 d PG . .
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'
I I -0.4742 1.8119 '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
O1 U1 O2 95.41(17) . . ?
O1 U1 N22 101.43(19) . . ?
O2 U1 N22 134.06(19) . . ?
O1 U1 N23 79.99(19) . . ?
O2 U1 N23 78.58(18) . . ?
N22 U1 N23 63.06(19) . . ?
O1 U1 N24 144.7(2) . . ?
O2 U1 N24 76.99(17) . . ?
N22 U1 N24 64.66(18) . . ?
N23 U1 N24 64.73(19) . . ?
O1 U1 N21 152.2(2) . . ?
O2 U1 N21 85.76(18) . . ?
N22 U1 N21 97.43(19) . . ?
N23 U1 N21 127.15(19) . . ?
N24 U1 N21 62.61(19) . . ?
O1 U1 I1 85.59(13) . . ?
O2 U1 I1 152.59(13) . . ?
N22 U1 I1 71.84(14) . . ?
N23 U1 I1 128.27(13) . . ?
N24 U1 I1 116.84(13) . . ?
N21 U1 I1 81.08(13) . . ?
O1 U1 I4 74.78(13) . . ?
O2 U1 I4 75.39(13) . . ?
N22 U1 I4 150.32(14) . . ?
N23 U1 I4 141.48(13) . . ?
N24 U1 I4 133.53(13) . . ?
N21 U1 I4 78.70(13) . . ?
I1 U1 I4 78.499(14) . . ?
O1 U1 U3 80.09(12) . . ?
O2 U1 U3 23.80(12) . . ?
N22 U1 U3 155.70(14) . . ?
N23 U1 U3 93.77(13) . . ?
N24 U1 U3 100.01(12) . . ?
N21 U1 U3 90.97(12) . . ?
I1 U1 U3 132.205(12) . . ?
I4 U1 U3 53.776(10) . . ?
O1 U1 U2 23.69(13) . . ?
O2 U1 U2 79.88(12) . . ?
N22 U1 U2 124.97(14) . . ?
N23 U1 U2 94.36(12) . . ?
N24 U1 U2 151.36(13) . . ?
N21 U1 U2 132.13(13) . . ?
I1 U1 U2 91.296(12) . . ?
I4 U1 U2 53.544(10) . . ?
U3 U1 U2 60.156(7) . . ?
O3 U2 O1 92.76(18) . . ?
O3 U2 N42 81.03(19) . . ?
O1 U2 N42 77.49(19) . . ?
O3 U2 N43 106.0(2) . . ?
O1 U2 N43 132.7(2) . . ?
N42 U2 N43 63.7(2) . . ?
O3 U2 N44 146.9(2) . . ?
O1 U2 N44 76.77(17) . . ?
N42 U2 N44 66.15(19) . . ?
N43 U2 N44 63.8(2) . . ?
O3 U2 N41 148.64(19) . . ?
O1 U2 N41 87.25(18) . . ?
N42 U2 N41 129.21(19) . . ?
N43 U2 N41 96.7(2) . . ?
N44 U2 N41 63.24(19) . . ?
O3 U2 I2 83.99(14) . . ?
O1 U2 I2 153.80(13) . . ?
N42 U2 I2 127.20(13) . . ?
N43 U2 I2 72.66(16) . . ?
N44 U2 I2 118.70(13) . . ?
N41 U2 I2 82.42(13) . . ?
O3 U2 I4 75.21(13) . . ?
O1 U2 I4 74.17(13) . . ?
N42 U2 I4 141.70(14) . . ?
N43 U2 I4 152.13(16) . . ?
N44 U2 I4 129.28(13) . . ?
N41 U2 I4 74.66(13) . . ?
I2 U2 I4 79.885(14) . . ?
O3 U2 U3 23.43(13) . . ?
O1 U2 U3 78.45(12) . . ?
N42 U2 U3 95.95(14) . . ?
N43 U2 U3 129.15(15) . . ?
N44 U2 U3 152.02(13) . . ?
N41 U2 U3 128.22(13) . . ?
I2 U2 U3 89.170(12) . . ?
I4 U2 U3 53.580(10) . . ?
O3 U2 U1 78.17(13) . . ?
O1 U2 U1 22.57(12) . . ?
N42 U2 U1 92.23(13) . . ?
N43 U2 U1 153.87(16) . . ?
N44 U2 U1 98.32(12) . . ?
N41 U2 U1 90.97(12) . . ?
I2 U2 U1 133.290(13) . . ?
I4 U2 U1 53.962(10) . . ?
U3 U2 U1 59.458(8) . . ?
O2 U3 O3 94.00(18) . . ?
O2 U3 N3 79.29(19) . . ?
O3 U3 N3 79.30(19) . . ?
O2 U3 N1 104.08(18) . . ?
O3 U3 N1 135.70(18) . . ?
N3 U3 N1 65.29(19) . . ?
O2 U3 N2 151.74(18) . . ?
O3 U3 N2 87.68(18) . . ?
N3 U3 N2 128.54(18) . . ?
N1 U3 N2 94.01(18) . . ?
O2 U3 N4 144.6(2) . . ?
O3 U3 N4 77.95(18) . . ?
N3 U3 N4 65.42(19) . . ?
N1 U3 N4 63.88(19) . . ?
N2 U3 N4 63.19(19) . . ?
O2 U3 I3 84.07(13) . . ?
O3 U3 I3 149.65(13) . . ?
N3 U3 I3 129.49(14) . . ?
N1 U3 I3 73.38(13) . . ?
N2 U3 I3 80.50(13) . . ?
N4 U3 I3 119.74(14) . . ?
O2 U3 I4 76.74(13) . . ?
O3 U3 I4 74.65(13) . . ?
N3 U3 I4 142.92(13) . . ?
N1 U3 I4 148.52(14) . . ?
N2 U3 I4 76.54(12) . . ?
N4 U3 I4 131.64(14) . . ?
I3 U3 I4 75.441(14) . . ?
O2 U3 U1 24.59(12) . . ?
O3 U3 U1 78.40(12) . . ?
N3 U3 U1 94.97(13) . . ?
N1 U3 U1 128.25(12) . . ?
N2 U3 U1 130.90(12) . . ?
N4 U3 U1 151.67(14) . . ?
I3 U3 U1 88.397(11) . . ?
I4 U3 U1 54.405(10) . . ?
O2 U3 U2 80.77(12) . . ?
O3 U3 U2 22.63(12) . . ?
N3 U3 U2 94.80(14) . . ?
N1 U3 U2 157.58(13) . . ?
N2 U3 U2 90.77(12) . . ?
N4 U3 U2 99.34(14) . . ?
I3 U3 U2 129.039(12) . . ?
I4 U3 U2 53.783(10) . . ?
U1 U3 U2 60.386(7) . . ?
U3 I4 U2 72.637(13) . . ?
U3 I4 U1 71.819(12) . . ?
U2 I4 U1 72.494(12) . . ?
U1 O1 U2 133.7(2) . . ?
U3 O2 U1 131.6(2) . . ?
U2 O3 U3 133.9(2) . . ?
C2 N1 C6 118.2(7) . . ?
C2 N1 U3 119.6(5) . . ?
C6 N1 U3 121.8(5) . . ?
C12 N2 C8 118.6(6) . . ?
C12 N2 U3 122.4(4) . . ?
C8 N2 U3 118.8(5) . . ?
C14 N3 C18 118.1(7) . . ?
C14 N3 U3 119.8(5) . . ?
C18 N3 U3 121.8(5) . . ?
C1 N4 C13 111.2(6) . . ?
C1 N4 C7 108.9(6) . . ?
C13 N4 C7 106.6(6) . . ?
C1 N4 U3 111.5(4) . . ?
C13 N4 U3 110.4(4) . . ?
C7 N4 U3 108.1(4) . . ?
C22 N21 C26 118.4(7) . . ?
C22 N21 U1 119.8(5) . . ?
C26 N21 U1 121.4(5) . . ?
C28 N22 C32 119.3(6) . . ?
C28 N22 U1 118.3(5) . . ?
C32 N22 U1 121.4(4) . . ?
C38 N23 C34 118.5(7) . . ?
C38 N23 U1 120.4(5) . . ?
C34 N23 U1 120.1(5) . . ?
C33 N24 C21 110.3(6) . . ?
C33 N24 C27 109.9(6) . . ?
C21 N24 C27 108.2(5) . . ?
C33 N24 U1 112.7(4) . . ?
C21 N24 U1 108.8(4) . . ?
C27 N24 U1 106.8(4) . . ?
C46 N41 C42 119.0(6) . . ?
C46 N41 U2 124.1(5) . . ?
C42 N41 U2 116.8(5) . . ?
C52 N42 C48 117.9(7) . . ?
C52 N42 U2 122.9(6) . . ?
C48 N42 U2 119.2(5) . . ?
C54 N43 C58 119.1(8) . . ?
C54 N43 U2 119.4(5) . . ?
C58 N43 U2 121.0(6) . . ?
C47 N44 C41 108.0(6) . . ?
C47 N44 C53 111.8(6) . . ?
C41 N44 C53 107.4(6) . . ?
C47 N44 U2 112.3(4) . . ?
C41 N44 U2 108.5(4) . . ?
C53 N44 U2 108.7(4) . . ?
N4 C1 C2 112.9(6) . . ?
N1 C2 C3 119.9(7) . . ?
N1 C2 C1 117.8(7) . . ?
C3 C2 C1 122.2(7) . . ?
C4 C3 C2 119.5(8) . . ?
C3 C4 C5 121.6(8) . . ?
C4 C5 C6 114.1(8) . . ?
N1 C6 C5 126.8(8) . . ?
N4 C7 C8 111.4(6) . . ?
N2 C8 C9 122.0(8) . . ?
N2 C8 C7 116.8(7) . . ?
C9 C8 C7 121.1(7) . . ?
C10 C9 C8 119.2(7) . . ?
C9 C10 C11 119.8(8) . . ?
C12 C11 C10 117.5(8) . . ?
N2 C12 C11 122.8(7) . . ?
N4 C13 C14 112.7(6) . . ?
N3 C14 C15 122.6(8) . . ?
N3 C14 C13 117.3(7) . . ?
C15 C14 C13 119.5(8) . . ?
C14 C15 C16 119.1(10) . . ?
C17 C16 C15 117.5(10) . . ?
C18 C17 C16 119.5(10) . . ?
C17 C18 N3 123.1(8) . . ?
C22 C21 N24 113.9(6) . . ?
N21 C22 C23 122.0(7) . . ?
N21 C22 C21 115.9(6) . . ?
C23 C22 C21 122.1(7) . . ?
C24 C23 C22 120.6(7) . . ?
C23 C24 C25 118.9(8) . . ?
C26 C25 C24 118.2(8) . . ?
N21 C26 C25 121.9(7) . . ?
C28 C27 N24 111.5(6) . . ?
N22 C28 C29 119.9(7) . . ?
N22 C28 C27 116.1(7) . . ?
C29 C28 C27 123.6(6) . . ?
C30 C29 C28 120.0(7) . . ?
C29 C30 C31 120.1(7) . . ?
C32 C31 C30 117.4(7) . . ?
N22 C32 C31 123.1(7) . . ?
C34 C33 N24 115.2(6) . . ?
N23 C34 C35 120.6(8) . . ?
N23 C34 C33 116.6(7) . . ?
C35 C34 C33 122.6(7) . . ?
C36 C35 C34 120.0(8) . . ?
C35 C36 C37 120.2(9) . . ?
C36 C37 C38 117.6(9) . . ?
N23 C38 C37 122.9(8) . . ?
C42 C41 N44 112.3(6) . . ?
N41 C42 C43 120.4(8) . . ?
N41 C42 C41 117.4(6) . . ?
C43 C42 C41 122.1(7) . . ?
C42 C43 C44 120.1(7) . . ?
C45 C44 C43 118.2(7) . . ?
C44 C45 C46 118.7(8) . . ?
N41 C46 C45 123.6(7) . . ?
N44 C47 C48 115.0(7) . . ?
N42 C48 C49 120.4(7) . . ?
N42 C48 C47 118.1(7) . . ?
C49 C48 C47 121.5(7) . . ?
C50 C49 C48 119.3(8) . . ?
C49 C50 C51 119.8(9) . . ?
C50 C51 C52 117.1(9) . . ?
N42 C52 C51 125.2(9) . . ?
C54 C53 N44 110.6(7) . . ?
N43 C54 C55 122.8(8) . . ?
N43 C54 C53 115.1(7) . . ?
C55 C54 C53 122.0(8) . . ?
C54 C55 C56 119.9(10) . . ?
C55 C56 C57 118.9(10) . . ?
C56 C57 C58 119.4(10) . . ?
N43 C58 C57 119.8(10) . . ?
N61 C61 C62 179.2(14) . . ?
N63 C65 C66 178.66(13) . . ?
N62 C63 C64 179.3(9) . . ?
N64 C67 C68 178.66(15) . . ?
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 O1 2.069(4) . ?
U1 O2 2.147(4) . ?
U1 N22 2.625(6) . ?
U1 N23 2.632(6) . ?
U1 N24 2.657(6) . ?
U1 N21 2.659(6) . ?
U1 I1 3.2242(5) . ?
U1 I4 3.3016(6) . ?
U1 U3 3.8575(4) . ?
U1 U2 3.8938(4) . ?
U2 O3 2.076(5) . ?
U2 O1 2.166(4) . ?
U2 N42 2.587(6) . ?
U2 N43 2.622(7) . ?
U2 N44 2.645(6) . ?
U2 N41 2.666(6) . ?
U2 I2 3.1861(6) . ?
U2 I4 3.2840(6) . ?
U2 U3 3.8849(4) . ?
U3 O2 2.082(5) . ?
U3 O3 2.146(5) . ?
U3 N3 2.613(7) . ?
U3 N1 2.636(6) . ?
U3 N2 2.656(6) . ?
U3 N4 2.673(6) . ?
U3 I3 3.2326(6) . ?
U3 I4 3.2754(5) . ?
N1 C2 1.330(9) . ?
N1 C6 1.332(10) . ?
N2 C12 1.342(10) . ?
N2 C8 1.346(9) . ?
N3 C14 1.325(10) . ?
N3 C18 1.353(11) . ?
N4 C1 1.467(10) . ?
N4 C13 1.475(10) . ?
N4 C7 1.504(10) . ?
N21 C22 1.331(9) . ?
N21 C26 1.351(10) . ?
N22 C28 1.341(9) . ?
N22 C32 1.346(9) . ?
N23 C38 1.327(10) . ?
N23 C34 1.351(10) . ?
N24 C33 1.483(10) . ?
N24 C21 1.494(10) . ?
N24 C27 1.507(9) . ?
N41 C46 1.309(10) . ?
N41 C42 1.376(9) . ?
N42 C52 1.308(10) . ?
N42 C48 1.370(10) . ?
N43 C54 1.363(11) . ?
N43 C58 1.364(11) . ?
N44 C47 1.470(10) . ?
N44 C41 1.496(10) . ?
N44 C53 1.503(9) . ?
C1 C2 1.488(11) . ?
C2 C3 1.436(11) . ?
C3 C4 1.358(13) . ?
C4 C5 1.392(13) . ?
C5 C6 1.395(12) . ?
C7 C8 1.509(11) . ?
C8 C9 1.374(11) . ?
C9 C10 1.365(12) . ?
C10 C11 1.406(11) . ?
C11 C12 1.375(11) . ?
C13 C14 1.549(11) . ?
C14 C15 1.370(14) . ?
C15 C16 1.405(16) . ?
C16 C17 1.390(14) . ?
C17 C18 1.347(14) . ?
C21 C22 1.482(11) . ?
C22 C23 1.362(11) . ?
C23 C24 1.345(13) . ?
C24 C25 1.394(12) . ?
C25 C26 1.376(11) . ?
C27 C28 1.478(11) . ?
C28 C29 1.399(11) . ?
C29 C30 1.358(11) . ?
C30 C31 1.384(11) . ?
C31 C32 1.374(10) . ?
C33 C34 1.480(11) . ?
C34 C35 1.367(12) . ?
C35 C36 1.352(13) . ?
C36 C37 1.363(13) . ?
C37 C38 1.375(13) . ?
C41 C42 1.460(12) . ?
C42 C43 1.387(11) . ?
C43 C44 1.396(12) . ?
C44 C45 1.386(11) . ?
C45 C46 1.393(11) . ?
C47 C48 1.505(11) . ?
C48 C49 1.408(12) . ?
C49 C50 1.377(13) . ?
C50 C51 1.377(13) . ?
C51 C52 1.390(13) . ?
C53 C54 1.485(12) . ?
C54 C55 1.373(13) . ?
C55 C56 1.380(15) . ?
C56 C57 1.399(17) . ?
C57 C58 1.433(15) . ?
N61 C61 1.120(16) . ?
C61 C62 1.419(18) . ?
N63 C65 1.051(15) . ?
C65 C66 1.35(2) . ?
N62 C63 1.145(13) . ?
C63 C64 1.488(14) . ?
N64 C67 1.1122 . ?
C67 C68 1.4255 . ?
