#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:28:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014276.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_7014276
loop_
_publ_author_name
'Salmon, Lionel'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis and crystal structure of tetra- and hexanuclear uranium(IV)
 complexes with hexadentate compartmental Schiff-base ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4139
_journal_page_last               4145
_journal_paper_doi               10.1039/b414626c
_journal_year                    2004
_chemical_formula_sum            'C132 H126 Cl10 N20 O16 U6'
_chemical_formula_weight         4031.21
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.342(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   42.8614(16)
_cell_length_b                   10.6024(4)
_cell_length_c                   29.6703(11)
_cell_measurement_reflns_used    45361
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.73
_cell_volume                     13471.9(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ 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  0.1191
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45361
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    7.455
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             7632
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.120
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         12714
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0478
_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)+(0.0095P)²+52.7644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                8047
_reflns_number_total             12714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414626c.txt
_cod_data_source_block           8.6py
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7014276
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.193993(9) 0.46536(3) 0.833544(11) 0.03057(10) Uani 1 1 d . . .
U2 U 0.110857(9) 0.53850(3) 0.851621(11) 0.02867(10) Uani 1 1 d . . .
U3 U 0.074764(9) 0.51032(3) 0.963733(11) 0.03134(10) Uani 1 1 d . . .
Cl1 Cl 0.20817(6) 0.4061(2) 0.92069(8) 0.0365(6) Uani 1 1 d . . .
Cl2 Cl 0.25255(6) 0.3666(2) 0.83034(8) 0.0404(6) Uani 1 1 d . . .
Cl3 Cl 0.18509(7) 0.2826(3) 0.77217(9) 0.0492(7) Uani 1 1 d . . .
Cl4 Cl 0.11983(6) 0.4811(2) 1.02712(8) 0.0371(6) Uani 1 1 d . . .
Cl5 Cl 0.06220(7) 0.7469(3) 0.98928(9) 0.0466(7) Uani 1 1 d . . .
O1A O 0.11689(17) 0.6200(6) 0.9275(2) 0.0364(17) Uani 1 1 d . . .
O2A O 0.16383(15) 0.6035(5) 0.8738(2) 0.0310(16) Uani 1 1 d . . .
O3A O 0.15051(15) 0.5444(6) 0.7939(2) 0.0354(16) Uani 1 1 d . . .
O4A O 0.09164(16) 0.5929(6) 0.7828(2) 0.0351(17) Uani 1 1 d . . .
N1A N 0.2236(2) 0.6718(8) 0.8518(3) 0.038(2) Uani 1 1 d . . .
N2A N 0.2106(2) 0.6032(7) 0.7682(3) 0.038(2) Uani 1 1 d . . .
C1A C 0.1439(2) 0.6801(9) 0.9410(3) 0.031(2) Uani 1 1 d . . .
C2A C 0.1688(2) 0.6711(8) 0.9120(3) 0.031(2) Uani 1 1 d . . .
C3A C 0.1974(3) 0.7309(9) 0.9219(3) 0.036(3) Uani 1 1 d . . .
C4A C 0.2002(3) 0.8031(9) 0.9623(3) 0.037(3) Uani 1 1 d . . .
H4A H 0.2187 0.8460 0.9692 0.045 Uiso 1 1 calc R . .
C5A C 0.1763(3) 0.8108(9) 0.9909(3) 0.039(3) Uani 1 1 d . . .
H5A H 0.1789 0.8561 1.0176 0.046 Uiso 1 1 calc R . .
C6A C 0.1478(2) 0.7511(9) 0.9804(3) 0.032(2) Uani 1 1 d . . .
H6A H 0.1314 0.7587 0.9998 0.038 Uiso 1 1 calc R . .
C7A C 0.2215(3) 0.7365(9) 0.8886(3) 0.037(3) Uani 1 1 d . . .
H7A H 0.2375 0.7941 0.8946 0.044 Uiso 1 1 calc R . .
C8A C 0.2469(3) 0.7201(10) 0.8179(4) 0.044(3) Uani 1 1 d . . .
C9A C 0.2434(3) 0.6375(10) 0.7762(3) 0.043(3) Uani 1 1 d . . .
H9A1 H 0.2508 0.6826 0.7502 0.051 Uiso 1 1 calc R . .
H9A2 H 0.2559 0.5618 0.7803 0.051 Uiso 1 1 calc R . .
C10A C 0.1954(3) 0.6436(10) 0.7330(3) 0.042(3) Uani 1 1 d . . .
H10A H 0.2073 0.6828 0.7117 0.051 Uiso 1 1 calc R . .
C11A C 0.1628(3) 0.6370(9) 0.7221(3) 0.038(3) Uani 1 1 d . . .
C12A C 0.1419(3) 0.5956(9) 0.7542(3) 0.038(3) Uani 1 1 d . . .
C13A C 0.1094(3) 0.6207(9) 0.7480(3) 0.037(3) Uani 1 1 d . . .
C14A C 0.0986(3) 0.6716(12) 0.7076(4) 0.061(3) Uani 1 1 d U . .
H14A H 0.0773 0.6839 0.7021 0.073 Uiso 1 1 calc R . .
C15A C 0.1197(3) 0.7045(13) 0.6750(4) 0.069(4) Uani 1 1 d U . .
H15A H 0.1121 0.7355 0.6474 0.083 Uiso 1 1 calc R . .
C16A C 0.1510(3) 0.6924(11) 0.6827(4) 0.055(3) Uani 1 1 d . . .
H16A H 0.1646 0.7215 0.6613 0.066 Uiso 1 1 calc R . .
C17A C 0.2802(3) 0.7090(11) 0.8377(4) 0.050(3) Uani 1 1 d . . .
H17A H 0.2845 0.6227 0.8455 0.075 Uiso 1 1 calc R . .
H17B H 0.2824 0.7605 0.8643 0.075 Uiso 1 1 calc R . .
H17C H 0.2946 0.7370 0.8159 0.075 Uiso 1 1 calc R . .
C18A C 0.2382(3) 0.8550(9) 0.8039(3) 0.044(3) Uani 1 1 d . . .
H18A H 0.2423 0.9110 0.8288 0.066 Uiso 1 1 calc R . .
H18B H 0.2164 0.8584 0.7949 0.066 Uiso 1 1 calc R . .
H18C H 0.2505 0.8802 0.7790 0.066 Uiso 1 1 calc R . .
O1B O 0.14695(15) 0.3669(5) 0.8567(2) 0.0277(15) Uani 1 1 d . . .
O2B O 0.09921(16) 0.3821(5) 0.91047(19) 0.0291(16) Uani 1 1 d . . .
O3B O -0.02637(14) 0.5161(6) 1.05865(18) 0.0381(17) Uani 1 1 d . . .
O4B O -0.06257(15) 0.4260(6) 1.11911(19) 0.0326(16) Uani 1 1 d . . .
N1B N 0.06801(19) 0.2697(8) 0.9847(2) 0.031(2) Uani 1 1 d . . .
N2B N 0.04247(18) 0.4665(8) 1.0347(2) 0.0351(19) Uani 1 1 d . . .
C1B C 0.1416(2) 0.2671(8) 0.8833(3) 0.032(2) Uani 1 1 d . . .
C2B C 0.1160(2) 0.2751(8) 0.9124(3) 0.030(2) Uani 1 1 d . . .
C3B C 0.1088(2) 0.1757(9) 0.9400(3) 0.038(3) Uani 1 1 d . . .
C4B C 0.1274(3) 0.0661(9) 0.9384(4) 0.045(3) Uani 1 1 d . . .
H4B H 0.1226 -0.0021 0.9565 0.054 Uiso 1 1 calc R . .
C5B C 0.1523(3) 0.0564(9) 0.9111(3) 0.042(3) Uani 1 1 d . . .
H5B H 0.1643 -0.0168 0.9108 0.051 Uiso 1 1 calc R . .
C6B C 0.1593(2) 0.1587(8) 0.8839(3) 0.034(2) Uani 1 1 d . . .
H6B H 0.1764 0.1538 0.8657 0.041 Uiso 1 1 calc R . .
C7B C 0.0844(2) 0.1773(10) 0.9719(3) 0.039(3) Uani 1 1 d . . .
H7B H 0.0800 0.0999 0.9850 0.047 Uiso 1 1 calc R . .
C8B C 0.0468(2) 0.2393(9) 1.0233(3) 0.035(2) Uani 1 1 d . . .
C9B C 0.0244(2) 0.3519(10) 1.0284(3) 0.039(3) Uani 1 1 d . . .
H9B1 H 0.0108 0.3593 1.0016 0.046 Uiso 1 1 calc R . .
H9B2 H 0.0116 0.3384 1.0541 0.046 Uiso 1 1 calc R . .
C10B C 0.0401(2) 0.5328(10) 1.0708(3) 0.038(2) Uani 1 1 d . . .
H10B H 0.0527 0.6039 1.0736 0.045 Uiso 1 1 calc R . .
C11B C 0.0190(2) 0.5068(10) 1.1083(3) 0.039(3) Uani 1 1 d . . .
C12B C -0.0131(2) 0.4895(10) 1.0989(3) 0.041(3) Uani 1 1 d . . .
C13B C -0.0322(2) 0.4466(9) 1.1331(3) 0.035(2) Uani 1 1 d . . .
C14B C -0.0200(3) 0.4278(11) 1.1762(3) 0.049(3) Uani 1 1 d . . .
H14B H -0.0328 0.3993 1.1987 0.059 Uiso 1 1 calc R . .
C15B C 0.0115(3) 0.4518(12) 1.1859(3) 0.059(4) Uani 1 1 d . . .
H15B H 0.0194 0.4427 1.2154 0.071 Uiso 1 1 calc R . .
C16B C 0.0312(3) 0.4886(10) 1.1530(3) 0.046(3) Uani 1 1 d . . .
H16B H 0.0524 0.5015 1.1600 0.055 Uiso 1 1 calc R . .
C17B C 0.0269(3) 0.1239(11) 1.0126(4) 0.062(4) Uani 1 1 d . . .
H17D H 0.0101 0.1198 1.0331 0.092 Uiso 1 1 calc R . .
H17E H 0.0395 0.0494 1.0157 0.092 Uiso 1 1 calc R . .
H17F H 0.0184 0.1297 0.9822 0.092 Uiso 1 1 calc R . .
C18B C 0.0676(3) 0.2217(10) 1.0662(3) 0.048(3) Uani 1 1 d . . .
H18D H 0.0547 0.2123 1.0917 0.072 Uiso 1 1 calc R . .
H18E H 0.0808 0.2940 1.0705 0.072 Uiso 1 1 calc R . .
H18F H 0.0802 0.1476 1.0632 0.072 Uiso 1 1 calc R . .
N1 N 0.1171(2) 0.7811(8) 0.8426(3) 0.049(3) Uani 1 1 d . . .
C1 C 0.0928(4) 0.8504(12) 0.8514(5) 0.080(4) Uani 1 1 d U . .
H1 H 0.0766 0.8149 0.8670 0.095 Uiso 1 1 calc R . .
C2 C 0.0905(5) 0.9796(16) 0.8375(7) 0.112(6) Uani 1 1 d U . .
H2 H 0.0745 1.0315 0.8467 0.134 Uiso 1 1 calc R . .
C3 C 0.1128(5) 1.0225(16) 0.8102(6) 0.104(5) Uani 1 1 d U . .
H3A H 0.1098 1.1012 0.7969 0.125 Uiso 1 1 calc R . .
C4 C 0.1394(4) 0.9575(12) 0.8010(5) 0.077(4) Uani 1 1 d U . .
H4 H 0.1556 0.9912 0.7850 0.093 Uiso 1 1 calc R . .
C5 C 0.1395(3) 0.8340(10) 0.8185(3) 0.054(4) Uani 1 1 d . . .
H5 H 0.1567 0.7842 0.8128 0.065 Uiso 1 1 calc R . .
N2 N 0.0803(2) 0.3477(7) 0.8124(3) 0.036(2) Uani 1 1 d . . .
C6 C 0.0552(3) 0.2928(10) 0.8296(4) 0.050(3) Uani 1 1 d . . .
H6 H 0.0511 0.3049 0.8599 0.060 Uiso 1 1 calc R . .
C7 C 0.0354(3) 0.2185(13) 0.8030(5) 0.076(4) Uani 1 1 d U . .
H7 H 0.0179 0.1820 0.8152 0.091 Uiso 1 1 calc R . .
C8 C 0.0417(4) 0.1983(14) 0.7573(5) 0.084(5) Uani 1 1 d U . .
H8 H 0.0285 0.1481 0.7392 0.101 Uiso 1 1 calc R . .
C9 C 0.0678(3) 0.2544(12) 0.7397(5) 0.071(4) Uani 1 1 d U . .
H9 H 0.0726 0.2443 0.7096 0.085 Uiso 1 1 calc R . .
C10 C 0.0863(3) 0.3260(9) 0.7690(4) 0.044(3) Uani 1 1 d . . .
H10 H 0.1043 0.3617 0.7579 0.053 Uiso 1 1 calc R . .
N3 N 0.2843(2) 0.3882(7) 0.9764(3) 0.036(2) Uani 1 1 d . . .
H3 H 0.2673 0.3974 0.9959 0.043 Uiso 1 1 d R . .
C11 C 0.2876(3) 0.4390(10) 0.9360(3) 0.043(3) Uani 1 1 d . . .
H11 H 0.2718 0.4896 0.9234 0.051 Uiso 1 1 calc R . .
C12 C 0.3136(3) 0.4179(10) 0.9129(4) 0.048(3) Uani 1 1 d . . .
H12 H 0.3157 0.4532 0.8845 0.057 Uiso 1 1 calc R . .
C13 C 0.3371(3) 0.3435(10) 0.9319(4) 0.053(3) Uani 1 1 d . . .
H13 H 0.3553 0.3298 0.9167 0.064 Uiso 1 1 calc R . .
C14 C 0.3333(3) 0.2910(11) 0.9726(4) 0.059(4) Uani 1 1 d . . .
H14 H 0.3485 0.2381 0.9854 0.071 Uiso 1 1 calc R . .
C15 C 0.3067(3) 0.3166(10) 0.9948(4) 0.045(3) Uani 1 1 d . . .
H15 H 0.3043 0.2830 1.0234 0.055 Uiso 1 1 calc R . .
N4 N 0.2391(2) 0.4399(7) 1.0362(3) 0.039(2) Uani 1 1 d . . .
C16 C 0.2438(3) 0.3862(9) 1.0774(4) 0.043(3) Uani 1 1 d . . .
H16 H 0.2608 0.3330 1.0829 0.052 Uiso 1 1 calc R . .
C17 C 0.2232(3) 0.4103(10) 1.1120(4) 0.055(3) Uani 1 1 d . . .
H17 H 0.2258 0.3688 1.1395 0.066 Uiso 1 1 calc R . .
C18 C 0.1996(3) 0.4935(10) 1.1054(4) 0.055(3) Uani 1 1 d . . .
H18 H 0.1866 0.5121 1.1287 0.066 Uiso 1 1 calc R . .
C19 C 0.1951(3) 0.5488(10) 1.0654(4) 0.047(3) Uani 1 1 d . . .
H19 H 0.1790 0.6066 1.0606 0.057 Uiso 1 1 calc R . .
C20 C 0.2147(3) 0.5194(10) 1.0309(3) 0.047(3) Uani 1 1 d . . .
H20 H 0.2108 0.5562 1.0028 0.056 Uiso 1 1 calc R . .
N5 N 0.1154(3) 0.0384(12) 0.6252(4) 0.089(4) Uani 1 1 d . . .
C21 C 0.1100(4) 0.1355(16) 0.5993(4) 0.081(5) Uani 1 1 d . . .
H21 H 0.1004 0.1197 0.5712 0.097 Uiso 1 1 calc R . .
C22 C 0.1169(3) 0.2573(15) 0.6091(5) 0.075(4) Uani 1 1 d U . .
H22 H 0.1125 0.3220 0.5886 0.090 Uiso 1 1 calc R . .
C23 C 0.1312(4) 0.2807(16) 0.6521(6) 0.099(5) Uani 1 1 d U . .
H23 H 0.1364 0.3615 0.6620 0.119 Uiso 1 1 calc R . .
C24 C 0.1369(4) 0.1725(16) 0.6789(5) 0.079(4) Uani 1 1 d U . .
H24 H 0.1475 0.1798 0.7067 0.095 Uiso 1 1 calc R . .
C25 C 0.1272(3) 0.0608(15) 0.6644(5) 0.075(4) Uani 1 1 d . . .
H25 H 0.1292 -0.0066 0.6843 0.090 Uiso 1 1 calc R . .
N6 N -0.0168(3) -0.0765(8) 0.8439(3) 0.063(6) Uani 0.50 1 d PGU . .
C26 C -0.0376(3) 0.0236(12) 0.8462(4) 0.061(7) Uani 0.50 1 d PGU . .
C27 C -0.0300(4) 0.1280(11) 0.8728(4) 0.069(8) Uani 0.50 1 d PGU . .
C28 C -0.0016(4) 0.1323(11) 0.8970(4) 0.057(7) Uani 0.50 1 d PGU . .
C29 C 0.0192(3) 0.0323(14) 0.8947(4) 0.070(7) Uani 0.50 1 d PGU . .
C30 C 0.0116(3) -0.0722(11) 0.8681(4) 0.075(8) Uani 0.50 1 d PGU . .
N7 N -0.0040(6) -0.1513(13) 0.7632(4) 0.134(12) Uani 0.50 1 d PGU . .
C31 C -0.0360(6) -0.1291(15) 0.7615(4) 0.146(16) Uani 0.50 1 d PGU . .
C32 C -0.0504(4) -0.0839(16) 0.7994(5) 0.145(16) Uani 0.50 1 d PGU . .
C33 C -0.0329(3) -0.0608(11) 0.8390(3) 0.119(14) Uani 0.50 1 d PGU . .
C34 C -0.0009(3) -0.0830(8) 0.8406(3) 0.127(16) Uani 0.50 1 d PGU . .
C35 C 0.0136(4) -0.1282(12) 0.8027(5) 0.118(13) Uani 0.50 1 d PGU . .
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
O2A U1 O3A 65.2(2) . . ?
O2A U1 O1B 68.5(2) . . ?
O3A U1 O1B 68.6(2) . . ?
O2A U1 N2A 102.0(2) . . ?
O3A U1 N2A 69.5(3) . . ?
O1B U1 N2A 137.0(2) . . ?
O2A U1 N1A 68.6(3) . . ?
O3A U1 N1A 100.3(2) . . ?
O1B U1 N1A 136.3(2) . . ?
N2A U1 N1A 61.6(3) . . ?
O2A U1 Cl3 137.87(17) . . ?
O3A U1 Cl3 80.04(17) . . ?
O1B U1 Cl3 77.37(15) . . ?
N2A U1 Cl3 86.2(2) . . ?
N1A U1 Cl3 144.5(2) . . ?
O2A U1 Cl1 76.24(16) . . ?
O3A U1 Cl1 135.50(16) . . ?
O1B U1 Cl1 77.49(15) . . ?
N2A U1 Cl1 143.2(2) . . ?
N1A U1 Cl1 84.65(19) . . ?
Cl3 U1 Cl1 120.16(8) . . ?
O2A U1 Cl2 142.64(17) . . ?
O3A U1 Cl2 147.47(16) . . ?
O1B U1 Cl2 129.01(15) . . ?
N2A U1 Cl2 84.7(2) . . ?
N1A U1 Cl2 83.6(2) . . ?
Cl3 U1 Cl2 78.68(9) . . ?
Cl1 U1 Cl2 76.87(8) . . ?
O4A U2 O4B 89.9(2) . 5_567 ?
O4A U2 O1B 117.8(2) . . ?
O4B U2 O1B 133.5(2) 5_567 . ?
O4A U2 O1A 141.0(2) . . ?
O4B U2 O1A 69.8(2) 5_567 . ?
O1B U2 O1A 99.7(2) . . ?
O4A U2 O2A 118.4(2) . . ?
O4B U2 O2A 133.8(2) 5_567 . ?
O1B U2 O2A 66.7(2) . . ?
O1A U2 O2A 65.4(2) . . ?
O4A U2 O3A 66.4(2) . . ?
O4B U2 O3A 155.9(2) 5_567 . ?
O1B U2 O3A 66.4(2) . . ?
O1A U2 O3A 126.1(2) . . ?
O2A U2 O3A 61.3(2) . . ?
O4A U2 O2B 137.5(2) . . ?
O4B U2 O2B 68.5(2) 5_567 . ?
O1B U2 O2B 66.0(2) . . ?
O1A U2 O2B 66.3(2) . . ?
O2A U2 O2B 102.2(2) . . ?
O3A U2 O2B 132.3(2) . . ?
O4A U2 N1 71.8(3) . . ?
O4B U2 N1 88.5(3) 5_567 . ?
O1B U2 N1 133.7(3) . . ?
O1A U2 N1 74.6(3) . . ?
O2A U2 N1 69.5(3) . . ?
O3A U2 N1 80.1(3) . . ?
O2B U2 N1 139.4(3) . . ?
O4A U2 N2 68.9(2) . . ?
O4B U2 N2 81.7(2) 5_567 . ?
O1B U2 N2 75.7(2) . . ?
O1A U2 N2 135.6(2) . . ?
O2A U2 N2 140.5(2) . . ?
O3A U2 N2 93.2(2) . . ?
O2B U2 N2 71.9(2) . . ?
N1 U2 N2 139.4(3) . . ?
O3B U3 O2B 99.5(2) 5_567 . ?
O3B U3 O1A 130.1(2) 5_567 . ?
O2B U3 O1A 67.8(2) . . ?
O3B U3 O4B 65.7(2) 5_567 5_567 ?
O2B U3 O4B 65.9(2) . 5_567 ?
O1A U3 O4B 65.2(2) . 5_567 ?
O3B U3 N2B 72.1(2) 5_567 . ?
O2B U3 N2B 134.6(2) . . ?
O1A U3 N2B 150.4(2) . . ?
O4B U3 N2B 136.2(2) 5_567 . ?
O3B U3 N1B 80.5(3) 5_567 . ?
O2B U3 N1B 70.0(2) . . ?
O1A U3 N1B 130.9(2) . . ?
O4B U3 N1B 117.2(2) 5_567 . ?
N2B U3 N1B 64.6(2) . . ?
O3B U3 Cl4 149.23(16) 5_567 . ?
O2B U3 Cl4 94.42(16) . . ?
O1A U3 Cl4 80.63(16) . . ?
O4B U3 Cl4 144.78(16) 5_567 . ?
N2B U3 Cl4 78.60(17) . . ?
N1B U3 Cl4 78.71(18) . . ?
O3B U3 Cl5 90.40(19) 5_567 . ?
O2B U3 Cl5 145.82(15) . . ?
O1A U3 Cl5 80.74(16) . . ?
O4B U3 Cl5 89.38(15) 5_567 . ?
N2B U3 Cl5 79.58(19) . . ?
N1B U3 Cl5 144.15(18) . . ?
Cl4 U3 Cl5 93.29(8) . . ?
C1A O1A U2 119.8(6) . . ?
C1A O1A U3 136.8(6) . . ?
U2 O1A U3 100.8(2) . . ?
C2A O2A U1 134.0(6) . . ?
C2A O2A U2 119.4(6) . . ?
U1 O2A U2 102.4(2) . . ?
C12A O3A U1 141.5(6) . . ?
C12A O3A U2 116.7(6) . . ?
U1 O3A U2 101.6(2) . . ?
C13A O4A U2 124.0(6) . . ?
C7A N1A C8A 116.4(9) . . ?
C7A N1A U1 125.2(7) . . ?
C8A N1A U1 118.3(6) . . ?
C10A N2A C9A 120.2(9) . . ?
C10A N2A U1 131.5(8) . . ?
C9A N2A U1 108.3(6) . . ?
O1A C1A C6A 124.5(9) . . ?
O1A C1A C2A 116.5(8) . . ?
C6A C1A C2A 119.0(10) . . ?
O2A C2A C3A 121.6(9) . . ?
O2A C2A C1A 116.9(9) . . ?
C3A C2A C1A 121.5(9) . . ?
C2A C3A C4A 117.6(10) . . ?
C2A C3A C7A 120.9(9) . . ?
C4A C3A C7A 120.7(10) . . ?
C5A C4A C3A 121.2(10) . . ?
C4A C5A C6A 120.5(9) . . ?
C1A C6A C5A 120.1(10) . . ?
N1A C7A C3A 128.6(10) . . ?
C9A C8A C17A 109.4(9) . . ?
C9A C8A C18A 107.5(9) . . ?
C17A C8A C18A 113.0(9) . . ?
C9A C8A N1A 107.2(8) . . ?
C17A C8A N1A 110.2(9) . . ?
C18A C8A N1A 109.3(9) . . ?
N2A C9A C8A 109.8(9) . . ?
N2A C10A C11A 129.2(10) . . ?
C16A C11A C12A 118.9(11) . . ?
C16A C11A C10A 119.6(10) . . ?
C12A C11A C10A 120.6(9) . . ?
O3A C12A C11A 124.2(10) . . ?
O3A C12A C13A 115.2(9) . . ?
C11A C12A C13A 120.2(9) . . ?
O4A C13A C14A 125.1(11) . . ?
O4A C13A C12A 116.2(8) . . ?
C14A C13A C12A 118.6(10) . . ?
C13A C14A C15A 119.8(12) . . ?
C16A C15A C14A 121.7(11) . . ?
C15A C16A C11A 120.3(11) . . ?
C1B O1B U2 120.7(6) . . ?
C1B O1B U1 132.6(6) . . ?
U2 O1B U1 101.5(2) . . ?
C2B O2B U3 135.2(5) . . ?
C2B O2B U2 118.2(5) . . ?
U3 O2B U2 101.2(2) . . ?
C12B O3B U3 128.0(6) . 5_567 ?
C13B O4B U2 135.8(5) . 5_567 ?
C13B O4B U3 113.5(5) . 5_567 ?
U2 O4B U3 99.5(2) 5_567 5_567 ?
C7B N1B C8B 114.5(8) . . ?
C7B N1B U3 127.2(7) . . ?
C8B N1B U3 117.1(6) . . ?
C10B N2B C9B 120.3(8) . . ?
C10B N2B U3 129.5(7) . . ?
C9B N2B U3 110.1(5) . . ?
O1B C1B C6B 123.8(9) . . ?
O1B C1B C2B 117.6(8) . . ?
C6B C1B C2B 118.6(9) . . ?
O2B C2B C3B 122.6(9) . . ?
O2B C2B C1B 116.7(8) . . ?
C3B C2B C1B 120.7(9) . . ?
C2B C3B C4B 118.0(10) . . ?
C2B C3B C7B 124.6(9) . . ?
C4B C3B C7B 117.3(9) . . ?
C5B C4B C3B 122.4(10) . . ?
C4B C5B C6B 118.4(10) . . ?
C1B C6B C5B 121.8(10) . . ?
N1B C7B C3B 129.1(10) . . ?
C17B C8B N1B 111.2(8) . . ?
C17B C8B C18B 112.2(9) . . ?
N1B C8B C18B 107.7(8) . . ?
C17B C8B C9B 107.3(9) . . ?
N1B C8B C9B 107.6(8) . . ?
C18B C8B C9B 110.8(8) . . ?
N2B C9B C8B 109.4(8) . . ?
N2B C10B C11B 126.3(10) . . ?
C12B C11B C16B 119.2(9) . . ?
C12B C11B C10B 119.6(8) . . ?
C16B C11B C10B 121.0(9) . . ?
O3B C12B C13B 118.3(9) . . ?
O3B C12B C11B 122.0(9) . . ?
C13B C12B C11B 119.7(8) . . ?
O4B C13B C14B 125.3(9) . . ?
O4B C13B C12B 114.2(8) . . ?
C14B C13B C12B 120.5(10) . . ?
C13B C14B C15B 119.5(10) . . ?
C16B C15B C14B 121.7(9) . . ?
C15B C16B C11B 119.2(10) . . ?
C1 N1 C5 117.5(11) . . ?
C1 N1 U2 116.8(9) . . ?
C5 N1 U2 123.1(8) . . ?
N1 C1 C2 121.7(16) . . ?
C3 C2 C1 116.8(18) . . ?
C2 C3 C4 124.3(17) . . ?
C3 C4 C5 112.6(16) . . ?
N1 C5 C4 126.4(14) . . ?
C6 N2 C10 118.7(10) . . ?
C6 N2 U2 123.5(7) . . ?
C10 N2 U2 116.1(7) . . ?
N2 C6 C7 120.8(12) . . ?
C6 C7 C8 119.9(14) . . ?
C9 C8 C7 119.0(13) . . ?
C10 C9 C8 116.8(13) . . ?
N2 C10 C9 124.7(12) . . ?
C15 N3 C11 120.2(10) . . ?
N3 C11 C12 120.7(10) . . ?
C11 C12 C13 119.4(11) . . ?
C14 C13 C12 119.4(12) . . ?
C13 C14 C15 118.9(11) . . ?
N3 C15 C14 121.4(10) . . ?
C20 N4 C16 117.0(9) . . ?
N4 C16 C17 120.4(10) . . ?
C18 C17 C16 120.2(10) . . ?
C19 C18 C17 119.9(11) . . ?
C18 C19 C20 119.3(11) . . ?
N4 C20 C19 123.1(10) . . ?
C25 N5 C21 116.6(14) . . ?
N5 C21 C22 126.7(14) . . ?
C21 C22 C23 116.3(14) . . ?
C24 C23 C22 115.1(15) . . ?
C25 C24 C23 120.0(15) . . ?
N5 C25 C24 125.0(16) . . ?
C26 N6 C30 120.0 . . ?
N6 C26 C27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 N6 120.0 . . ?
C31 N7 C35 120.0 . . ?
C32 C31 N7 120.0 . . ?
C31 C32 C33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
N7 C35 C34 120.0 . . ?
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 O2A 2.318(6) . ?
U1 O3A 2.320(6) . ?
U1 O1B 2.396(6) . ?
U1 N2A 2.553(8) . ?
U1 N1A 2.576(8) . ?
U1 Cl3 2.676(3) . ?
U1 Cl1 2.706(2) . ?
U1 Cl2 2.725(3) . ?
U1 U2 3.7071(5) . ?
U2 O4A 2.244(6) . ?
U2 O4B 2.308(6) 5_567 ?
U2 O1B 2.389(6) . ?
U2 O1A 2.416(6) . ?
U2 O2A 2.438(7) . ?
U2 O3A 2.463(6) . ?
U2 O2B 2.474(5) . ?
U2 N1 2.600(9) . ?
U2 N2 2.653(8) . ?
U2 U3 3.7374(5) . ?
U3 O3B 2.170(6) 5_567 ?
U3 O2B 2.362(6) . ?
U3 O1A 2.434(7) . ?
U3 O4B 2.582(6) 5_567 ?
U3 N2B 2.608(8) . ?
U3 N1B 2.645(8) . ?
U3 Cl4 2.658(2) . ?
U3 Cl5 2.682(3) . ?
O1A C1A 1.368(12) . ?
O2A C2A 1.350(10) . ?
O3A C12A 1.335(11) . ?
O4A C13A 1.342(12) . ?
N1A C7A 1.295(12) . ?
N1A C8A 1.536(13) . ?
N2A C10A 1.280(12) . ?
N2A C9A 1.463(13) . ?
C1A C6A 1.395(12) . ?
C1A C2A 1.401(14) . ?
C2A C3A 1.399(14) . ?
C3A C4A 1.422(13) . ?
C3A C7A 1.459(14) . ?
C4A C5A 1.359(14) . ?
C5A C6A 1.400(14) . ?
C8A C9A 1.519(14) . ?
C8A C17A 1.524(15) . ?
C8A C18A 1.532(14) . ?
C10A C11A 1.421(14) . ?
C11A C16A 1.385(14) . ?
C11A C12A 1.406(14) . ?
C12A C13A 1.421(14) . ?
C13A C14A 1.375(14) . ?
C14A C15A 1.395(16) . ?
C15A C16A 1.359(17) . ?
O1B C1B 1.345(11) . ?
O2B C2B 1.344(10) . ?
O3B C12B 1.334(10) . ?
O3B U3 2.170(6) 5_567 ?
O4B C13B 1.368(11) . ?
O4B U2 2.308(6) 5_567 ?
O4B U3 2.582(6) 5_567 ?
N1B C7B 1.273(12) . ?
N1B C8B 1.524(12) . ?
N2B C10B 1.288(11) . ?
N2B C9B 1.448(12) . ?
C1B C6B 1.377(13) . ?
C1B C2B 1.424(13) . ?
C2B C3B 1.377(13) . ?
C3B C4B 1.411(13) . ?
C3B C7B 1.441(14) . ?
C4B C5B 1.369(14) . ?
C5B C6B 1.392(13) . ?
C8B C17B 1.518(14) . ?
C8B C18B 1.536(13) . ?
C8B C9B 1.542(14) . ?
C10B C11B 1.487(13) . ?
C11B C12B 1.405(13) . ?
C11B C16B 1.419(12) . ?
C12B C13B 1.404(13) . ?
C13B C14B 1.377(13) . ?
C14B C15B 1.393(16) . ?
C15B C16B 1.375(15) . ?
N1 C1 1.308(16) . ?
N1 C5 1.344(15) . ?
C1 C2 1.433(19) . ?
C2 C3 1.35(2) . ?
C3 C4 1.37(2) . ?
C4 C5 1.408(15) . ?
N2 C6 1.343(13) . ?
N2 C10 1.343(13) . ?
C6 C7 1.382(17) . ?
C7 C8 1.409(19) . ?
C8 C9 1.390(19) . ?
C9 C10 1.379(16) . ?
N3 C15 1.324(13) . ?
N3 C11 1.328(12) . ?
C11 C12 1.353(15) . ?
C12 C13 1.379(15) . ?
C13 C14 1.345(16) . ?
C14 C15 1.365(16) . ?
N4 C20 1.347(13) . ?
N4 C16 1.357(12) . ?
C16 C17 1.404(15) . ?
C17 C18 1.349(15) . ?
C18 C19 1.331(14) . ?
C19 C20 1.386(15) . ?
N5 C25 1.271(17) . ?
N5 C21 1.299(17) . ?
C21 C22 1.353(19) . ?
C22 C23 1.41(2) . ?
C23 C24 1.41(2) . ?
C24 C25 1.321(18) . ?
N6 C26 1.3900 . ?
N6 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
N7 C31 1.3900 . ?
N7 C35 1.3900 . ?
C31 C32 1.3898 . ?
C32 C33 1.3901 . ?
C33 C34 1.3900 . ?
C34 C35 1.3902 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 N4 0.95 1.79 2.734(12) 169.6 .
