#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/52/4335207.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_4335207
loop_
_publ_author_name
'Clément Camp'
'Julie Andrez'
'Jacques Pécaut'
'Marinella Mazzanti'
_publ_section_title
;
 Synthesis of Electron-Rich Uranium(IV) Complexes Supported by Tridentate
 Schiff Base Ligands and Their Multi-Electron Redox Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7078
_journal_page_last               7086
_journal_paper_doi               10.1021/ic4006218
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C78.5 H60.5 N8.5 O4 U'
_chemical_formula_weight         1424.88
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.506(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.625(2)
_cell_length_b                   15.8387(9)
_cell_length_c                   18.5959(13)
_cell_measurement_reflns_used    3653
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4118
_cell_measurement_theta_min      3.3590
_cell_volume                     12586.7(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -92.00  -43.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  137.0000 -139.0000 49

  2 omega  -55.00   37.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  150.0000 92

  3 omega  -98.00   15.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -19.0000 -150.0000 113

  4 omega  -97.00    1.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000   30.0000 98

  5 omega  -53.00  -28.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000  -60.0000 25

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω 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  0.1193
_diffrn_reflns_av_sigmaI/netI    0.1343
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31319
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_T_max  0.9466
_exptl_absorpt_correction_T_min  0.5536
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             5720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.465
_refine_diff_density_min         -1.712
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         9013
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+79.6526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                5650
_reflns_number_total             9013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4006218_si_001_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        12586.6(13)
_cod_original_formula_sum        'C78.50 H60.50 N8.50 O4 U'
_cod_database_code               4335207
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_group
U1 U 0.163888(11) 0.21447(3) 0.72238(2) 0.02663(16) Uani 1 1 d . .
O1 O 0.11938(18) 0.1494(4) 0.6579(4) 0.0302(19) Uani 1 1 d . .
N1 N 0.1380(2) 0.2824(5) 0.5923(5) 0.022(2) Uani 1 1 d . .
N2 N 0.1748(2) 0.3701(5) 0.7148(5) 0.028(2) Uani 1 1 d U .
C1 C 0.0934(3) 0.1490(8) 0.5996(7) 0.038(3) Uani 1 1 d . .
C2 C 0.0698(3) 0.0909(7) 0.5973(7) 0.038(3) Uani 1 1 d . .
H2 H 0.0730 0.0531 0.6391 0.045 Uiso 1 1 calc R .
C3 C 0.0425(3) 0.0878(8) 0.5364(8) 0.052(4) Uani 1 1 d . .
H3 H 0.0270 0.0477 0.5368 0.063 Uiso 1 1 calc R .
C4 C 0.0363(3) 0.1421(7) 0.4727(7) 0.041(3) Uani 1 1 d . .
C5 C 0.0078(3) 0.1391(9) 0.4090(9) 0.063(4) Uani 1 1 d . .
H5 H -0.0074 0.0973 0.4073 0.075 Uiso 1 1 calc R .
C6 C 0.0020(4) 0.1953(7) 0.3503(7) 0.052(4) Uani 1 1 d . .
H6 H -0.0166 0.1866 0.3073 0.062 Uiso 1 1 calc R .
C7 C 0.0204(3) 0.2646(8) 0.3465(7) 0.050(4) Uani 1 1 d U .
H7 H 0.0144 0.3073 0.3082 0.060 Uiso 1 1 calc R .
C8 C 0.0502(3) 0.2613(9) 0.4106(8) 0.053(4) Uani 1 1 d . .
H8 H 0.0657 0.3007 0.4095 0.063 Uiso 1 1 calc R .
C9 C 0.0584(3) 0.2047(7) 0.4748(6) 0.032(3) Uani 1 1 d . .
C10 C 0.0878(3) 0.2076(7) 0.5387(6) 0.032(3) Uani 1 1 d . .
C11 C 0.1107(3) 0.2710(7) 0.5397(7) 0.032(3) Uani 1 1 d . .
H11 H 0.1052 0.3085 0.4971 0.038 Uiso 1 1 calc R .
C12 C 0.1553(3) 0.3500(7) 0.5748(7) 0.035(3) Uani 1 1 d . .
C13 C 0.1553(3) 0.3689(7) 0.5038(6) 0.033(3) Uani 1 1 d . .
H13 H 0.1439 0.3341 0.4616 0.039 Uiso 1 1 calc R .
C14 C 0.1714(3) 0.4372(8) 0.4917(7) 0.039(3) Uani 1 1 d . .
H14 H 0.1699 0.4506 0.4407 0.046 Uiso 1 1 calc R .
C15 C 0.1894(3) 0.4863(8) 0.5505(7) 0.042(3) Uani 1 1 d . .
H15 H 0.2003 0.5338 0.5411 0.050 Uiso 1 1 calc R .
C16 C 0.1916(3) 0.4652(7) 0.6247(7) 0.033(3) Uani 1 1 d . .
C17 C 0.2093(3) 0.5147(7) 0.6885(8) 0.040(3) Uani 1 1 d . .
H17 H 0.2214 0.5608 0.6815 0.048 Uiso 1 1 calc R .
C18 C 0.2092(3) 0.4963(7) 0.7594(7) 0.039(3) Uani 1 1 d . .
H18 H 0.2200 0.5314 0.8018 0.046 Uiso 1 1 calc R .
C19 C 0.1927(3) 0.4245(7) 0.7696(7) 0.036(3) Uani 1 1 d . .
C20 C 0.1753(3) 0.3971(7) 0.6396(7) 0.036(3) Uani 1 1 d . .
C21 C 0.1932(3) 0.4029(8) 0.8483(6) 0.047(4) Uani 1 1 d . .
H21A H 0.1876 0.3440 0.8502 0.056 Uiso 1 1 d R .
H21B H 0.2143 0.4127 0.8849 0.056 Uiso 1 1 d R .
H21C H 0.1784 0.4391 0.8606 0.056 Uiso 1 1 d R .
O31 O 0.13513(18) 0.2748(4) 0.7840(4) 0.033(2) Uani 1 1 d . .
N31 N 0.1636(2) 0.1253(5) 0.8335(5) 0.027(2) Uani 1 1 d . .
N32 N 0.1815(2) 0.0565(5) 0.7226(5) 0.022(2) Uani 1 1 d . .
C31 C 0.1194(3) 0.2609(7) 0.8289(7) 0.034(3) Uani 1 1 d . .
C32 C 0.0994(3) 0.3253(8) 0.8376(7) 0.042(3) Uani 1 1 d . .
H32 H 0.0970 0.3755 0.8082 0.050 Uiso 1 1 calc R .
C33 C 0.0838(4) 0.3175(9) 0.8865(8) 0.062(4) Uani 1 1 d . .
H33 H 0.0715 0.3635 0.8928 0.074 Uiso 1 1 calc R .
C34 C 0.0850(3) 0.2424(9) 0.9289(8) 0.050(4) Uani 1 1 d . .
C35 C 0.0690(4) 0.2362(11) 0.9814(9) 0.078(5) Uani 1 1 d . .
H35 H 0.0571 0.2825 0.9886 0.093 Uiso 1 1 calc R .
C36 C 0.0708(5) 0.1640(12) 1.0215(11) 0.107(8) Uani 1 1 d . .
H36 H 0.0600 0.1598 1.0565 0.129 Uiso 1 1 calc R .
C37 C 0.0884(4) 0.0960(12) 1.0120(11) 0.100(7) Uani 1 1 d . .
H37 H 0.0895 0.0458 1.0409 0.120 Uiso 1 1 calc R .
C38 C 0.1039(3) 0.1008(8) 0.9616(8) 0.053(4) Uani 1 1 d . .
H38 H 0.1154 0.0531 0.9551 0.064 Uiso 1 1 calc R .
C39 C 0.1035(3) 0.1754(7) 0.9185(6) 0.035(3) Uani 1 1 d . .
C40 C 0.1213(3) 0.1865(7) 0.8689(6) 0.032(3) Uani 1 1 d . .
C41 C 0.1450(3) 0.1247(7) 0.8720(6) 0.030(3) Uani 1 1 d . .
H41 H 0.1470 0.0785 0.9060 0.035 Uiso 1 1 calc R .
C42 C 0.1877(3) 0.0619(7) 0.8555(6) 0.030(3) Uani 1 1 d . .
C43 C 0.2035(3) 0.0371(7) 0.9290(7) 0.037(3) Uani 1 1 d . .
H43 H 0.1992 0.0641 0.9699 0.044 Uiso 1 1 calc R .
C44 C 0.2255(3) -0.0265(8) 0.9452(8) 0.048(4) Uani 1 1 d . .
H44 H 0.2364 -0.0423 0.9970 0.058 Uiso 1 1 calc R .
C45 C 0.2319(3) -0.0673(7) 0.8866(7) 0.042(3) Uani 1 1 d . .
H45 H 0.2460 -0.1136 0.8976 0.050 Uiso 1 1 calc R .
C46 C 0.2174(3) -0.0402(7) 0.8116(7) 0.034(3) Uani 1 1 d . .
C47 C 0.2222(3) -0.0789(7) 0.7482(7) 0.042(3) Uani 1 1 d . .
H47 H 0.2367 -0.1240 0.7559 0.050 Uiso 1 1 calc R .
C48 C 0.2057(3) -0.0511(7) 0.6755(7) 0.039(3) Uani 1 1 d . .
H48 H 0.2079 -0.0799 0.6328 0.046 Uiso 1 1 calc R .
C49 C 0.1860(3) 0.0179(7) 0.6628(7) 0.034(3) Uani 1 1 d . .
C50 C 0.1957(3) 0.0253(6) 0.7938(6) 0.023(3) Uani 1 1 d . .
C51 C 0.1690(3) 0.0520(8) 0.5839(6) 0.048(4) Uani 1 1 d . .
H51A H 0.1812 0.0978 0.5729 0.072 Uiso 1 1 calc R .
H51B H 0.1485 0.0736 0.5813 0.072 Uiso 1 1 calc R .
H51C H 0.1661 0.0068 0.5461 0.072 Uiso 1 1 calc R .
O61 O 0.21101(18) 0.2253(4) 0.8133(4) 0.0228(17) Uani 1 1 d . .
O62 O 0.20155(16) 0.2133(4) 0.6675(3) 0.0215(16) Uani 1 1 d . .
C61 C 0.2370(3) 0.2229(6) 0.7935(6) 0.028(3) Uani 1 1 d . .
C62 C 0.2674(2) 0.2284(6) 0.8470(6) 0.023(3) Uani 1 1 d . .
C63 C 0.2718(3) 0.2382(7) 0.9260(6) 0.032(3) Uani 1 1 d . .
H63 H 0.2541 0.2418 0.9415 0.038 Uiso 1 1 calc R .
C64 C 0.3009(3) 0.2424(8) 0.9796(7) 0.043(3) Uani 1 1 d . .
H64 H 0.3036 0.2476 1.0324 0.051 Uiso 1 1 calc R .
C65 C 0.3265(3) 0.2391(8) 0.9562(7) 0.046(4) Uani 1 1 d . .
H65 H 0.3470 0.2421 0.9936 0.056 Uiso 1 1 calc R .
C66 C 0.3229(3) 0.2315(7) 0.8796(7) 0.038(3) Uani 1 1 d . .
H66 H 0.3410 0.2296 0.8654 0.045 Uiso 1 1 calc R .
C67 C 0.2932(3) 0.2266(6) 0.8223(6) 0.022(3) Uani 1 1 d . .
C68 C 0.2880(3) 0.2156(6) 0.7428(6) 0.022(2) Uani 1 1 d . .
C69 C 0.3128(3) 0.2111(7) 0.7140(7) 0.032(3) Uani 1 1 d . .
H69 H 0.3337 0.2175 0.7484 0.038 Uiso 1 1 calc R .
C70 C 0.3073(3) 0.1977(7) 0.6372(7) 0.038(3) Uani 1 1 d . .
H70 H 0.3244 0.1922 0.6196 0.046 Uiso 1 1 calc R .
C71 C 0.2771(3) 0.1922(7) 0.5860(7) 0.036(3) Uani 1 1 d . .
H71 H 0.2735 0.1842 0.5329 0.044 Uiso 1 1 calc R .
C72 C 0.2525(3) 0.1981(7) 0.6104(6) 0.027(3) Uani 1 1 d . .
H72 H 0.2318 0.1941 0.5744 0.033 Uiso 1 1 calc R .
C73 C 0.2574(3) 0.2102(6) 0.6893(6) 0.023(2) Uani 1 1 d . .
C74 C 0.2318(2) 0.2154(6) 0.7160(5) 0.014(2) Uani 1 1 d U .
N81 N 0.1044(3) 0.3634(7) 0.3219(7) 0.059(3) Uani 1 1 d . .
C81 C 0.0899(4) 0.3155(11) 0.2501(10) 0.075(5) Uani 1 1 d U .
H81 H 0.1001 0.2671 0.2400 0.090 Uiso 1 1 calc R .
C82 C 0.0640(4) 0.3386(11) 0.2023(9) 0.074(5) Uani 1 1 d U .
H82 H 0.0555 0.3090 0.1551 0.088 Uiso 1 1 calc R .
C83 C 0.0473(4) 0.4064(10) 0.2166(9) 0.063(4) Uani 1 1 d . .
H83 H 0.0276 0.4221 0.1803 0.076 Uiso 1 1 calc R .
C84 C 0.0599(4) 0.4493(9) 0.2834(9) 0.066(5) Uani 1 1 d . .
H84 H 0.0487 0.4950 0.2946 0.079 Uiso 1 1 calc R .
C85 C 0.0887(4) 0.4274(9) 0.3349(8) 0.061(4) Uani 1 1 d . .
H85 H 0.0974 0.4591 0.3808 0.073 Uiso 1 1 calc R .
N82 N 0.0895(3) 0.4883(9) 0.0155(7) 0.069(4) Uani 1 1 d . .
C86 C 0.1140(4) 0.4450(9) 0.0634(10) 0.066(5) Uani 1 1 d . .
H86 H 0.1244 0.4059 0.0417 0.080 Uiso 1 1 calc R .
C87 C 0.1247(4) 0.4541(9) 0.1409(9) 0.058(4) Uani 1 1 d . .
H87 H 0.1416 0.4207 0.1723 0.069 Uiso 1 1 calc R .
C88 C 0.1110(5) 0.5114(12) 0.1728(10) 0.076(5) Uani 1 1 d . .
H88 H 0.1187 0.5196 0.2269 0.091 Uiso 1 1 calc R .
C89 C 0.0854(5) 0.5587(11) 0.1263(13) 0.084(6) Uani 1 1 d . .
H89 H 0.0752 0.5992 0.1468 0.101 Uiso 1 1 calc R .
C90 C 0.0763(4) 0.5427(11) 0.0503(11) 0.076(5) Uani 1 1 d . .
H90 H 0.0588 0.5733 0.0181 0.091 Uiso 1 1 calc R .
N83 N 0.0157(4) 0.6717(14) 0.1676(11) 0.136(7) Uani 1 1 d . .
C91 C 0.0178(5) 0.7108(12) 0.1002(11) 0.094(6) Uani 1 1 d . .
H91 H 0.0282 0.7633 0.1034 0.112 Uiso 1 1 calc R .
C92 C 0.0044(4) 0.6706(10) 0.0301(10) 0.063(4) Uani 1 1 d . .
H92 H 0.0051 0.6958 -0.0156 0.076 Uiso 1 1 calc R .
C93 C -0.0093(4) 0.5972(11) 0.0277(10) 0.072(5) Uani 1 1 d . .
H93 H -0.0178 0.5686 -0.0200 0.087 Uiso 1 1 calc R .
C94 C -0.0114(4) 0.5621(9) 0.0906(10) 0.063(5) Uani 1 1 d . .
H94 H -0.0218 0.5093 0.0855 0.076 Uiso 1 1 calc R .
C95 C -0.0005(4) 0.5944(10) 0.1563(11) 0.065(5) Uani 1 1 d . .
H95 H -0.0032 0.5664 0.1987 0.078 Uiso 1 1 calc R .
N84 N 0.0864(5) 0.0768(10) 0.2384(12) 0.112(6) Uani 1 1 d U .
C96 C 0.1157(6) 0.0867(11) 0.2393(13) 0.095(6) Uani 1 1 d U .
H96 H 0.1200 0.0752 0.1938 0.114 Uiso 1 1 calc R .
C97 C 0.1397(5) 0.1128(10) 0.3039(16) 0.095(6) Uani 1 1 d U .
H97 H 0.1600 0.1197 0.3018 0.114 Uiso 1 1 calc R .
C98 C 0.1351(6) 0.1281(13) 0.3667(15) 0.109(8) Uani 1 1 d U .
H98 H 0.1518 0.1477 0.4104 0.131 Uiso 1 1 calc R .
C99 C 0.1087(7) 0.1171(13) 0.3699(13) 0.100(7) Uani 1 1 d U .
H99 H 0.1058 0.1280 0.4172 0.120 Uiso 1 1 calc R .
C100 C 0.0835(6) 0.0903(12) 0.3093(17) 0.105(7) Uani 1 1 d U .
H100 H 0.0640 0.0809 0.3157 0.126 Uiso 1 1 calc R .
N85 N 0.0236(16) 0.091(4) 0.819(3) 0.11(2) Uani 0.50 1 d PDU 1
C101 C 0.0279(7) 0.083(2) 0.752(2) 0.22(2) Uani 1 1 d D .
H101 H 0.0486 0.0724 0.7540 0.266 Uiso 1 1 calc R 1
C102 C 0.0076(9) 0.089(2) 0.689(2) 0.190(17) Uani 1 1 d . .
H102 H 0.0134 0.0918 0.6449 0.228 Uiso 1 1 calc R .
C103 C 0.020(4) 0.080(10) 0.815(5) 0.24(8) Uani 0.50 1 d PDU 2
H103 H 0.0354 0.0718 0.8639 0.287 Uiso 0.50 1 calc PR 2
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0182 -0.0006 -0.0003 -1.0001 0.0326 0.0053 0.0005
0 0 1 0.0030 0.0006 0.0003 1.0001 -0.0326 -0.0053 -0.0005
0 1 -1 0.0377 0.0009 1.0000 -1.0013 0.0246 -0.0342 0.0053
0 -1 1 0.0447 -0.0009 -1.0000 1.0013 -0.0246 0.0342 -0.0053
-1 0 1 0.1164 -0.9999 0.0004 1.0003 -0.0179 0.0031 0.0439
1 0 -1 0.1144 0.9999 -0.0004 -1.0003 0.0179 -0.0031 -0.0439
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
O1 U1 O61 154.6(2) . .
O1 U1 O31 83.4(3) . .
O61 U1 O31 99.3(3) . .
O1 U1 O62 116.4(2) . .
O61 U1 O62 70.3(2) . .
O31 U1 O62 154.2(3) . .
O1 U1 N31 85.2(3) . .
O61 U1 N31 72.5(3) . .
O31 U1 N31 69.2(3) . .
O62 U1 N31 125.9(3) . .
O1 U1 N2 125.7(3) . .
O61 U1 N2 79.1(3) . .
O31 U1 N2 77.0(3) . .
O62 U1 N2 77.8(3) . .
N31 U1 N2 130.8(3) . .
O1 U1 N1 69.4(3) . .
O61 U1 N1 134.1(3) . .
O31 U1 N1 98.5(3) . .
O62 U1 N1 75.4(2) . .
N31 U1 N1 153.2(3) . .
N2 U1 N1 64.3(3) . .
O1 U1 N32 77.3(3) . .
O61 U1 N32 81.9(2) . .
O31 U1 N32 129.8(3) . .
O62 U1 N32 73.5(2) . .
N31 U1 N32 63.4(3) . .
N2 U1 N32 149.6(3) . .
N1 U1 N32 116.5(3) . .
C1 O1 U1 148.3(7) . .
C11 N1 C12 113.1(9) . .
C11 N1 U1 131.5(7) . .
C12 N1 U1 115.2(7) . .
C19 N2 C20 108.8(9) . .
C19 N2 U1 130.6(7) . .
C20 N2 U1 113.9(6) . .
O1 C1 C2 119.6(11) . .
O1 C1 C10 121.3(11) . .
C2 C1 C10 119.1(12) . .
C3 C2 C1 121.1(12) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C2 C3 C4 122.1(12) . .
C2 C3 H3 118.9 . .
C4 C3 H3 118.9 . .
C9 C4 C3 118.5(12) . .
C9 C4 C5 119.0(12) . .
C3 C4 C5 122.4(13) . .
C6 C5 C4 120.8(14) . .
C6 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
C5 C6 C7 127.0(13) . .
C5 C6 H6 116.5 . .
C7 C6 H6 116.5 . .
C6 C7 C8 109.5(12) . .
C6 C7 H7 125.2 . .
C8 C7 H7 125.2 . .
C9 C8 C7 126.8(13) . .
C9 C8 H8 116.6 . .
C7 C8 H8 116.6 . .
C4 C9 C8 116.3(11) . .
C4 C9 C10 119.6(11) . .
C8 C9 C10 124.1(11) . .
C1 C10 C11 121.4(11) . .
C1 C10 C9 119.3(11) . .
C11 C10 C9 119.4(10) . .
N1 C11 C10 127.2(10) . .
N1 C11 H11 116.4 . .
C10 C11 H11 116.4 . .
C13 C12 N1 125.1(11) . .
C13 C12 C20 119.1(12) . .
N1 C12 C20 115.8(10) . .
C12 C13 C14 121.2(12) . .
C12 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
C15 C14 C13 121.8(11) . .
C15 C14 H14 119.1 . .
C13 C14 H14 119.1 . .
C14 C15 C16 118.4(11) . .
C14 C15 H15 120.8 . .
C16 C15 H15 120.8 . .
C15 C16 C20 121.7(11) . .
C15 C16 C17 121.4(11) . .
C20 C16 C17 116.8(11) . .
C18 C17 C16 120.1(11) . .
C18 C17 H17 119.9 . .
C16 C17 H17 119.9 . .
C17 C18 C19 119.2(11) . .
C17 C18 H18 120.4 . .
C19 C18 H18 120.4 . .
N2 C19 C18 128.0(11) . .
N2 C19 C21 112.7(10) . .
C18 C19 C21 119.3(11) . .
C16 C20 C12 117.5(11) . .
C16 C20 N2 127.0(10) . .
C12 C20 N2 115.4(10) . .
C19 C21 H21A 110.0 . .
C19 C21 H21B 108.5 . .
H21A C21 H21B 109.7 . .
C19 C21 H21C 108.8 . .
H21A C21 H21C 110.1 . .
H21B C21 H21C 109.8 . .
C31 O31 U1 144.5(7) . .
C41 N31 C42 115.1(9) . .
C41 N31 U1 131.1(8) . .
C42 N31 U1 113.7(7) . .
C49 N32 C50 119.0(9) . .
C49 N32 U1 124.4(7) . .
C50 N32 U1 113.1(6) . .
O31 C31 C40 123.1(11) . .
O31 C31 C32 118.5(11) . .
C40 C31 C32 118.4(12) . .
C33 C32 C31 121.9(12) . .
C33 C32 H32 119.1 . .
C31 C32 H32 119.1 . .
C32 C33 C34 121.7(13) . .
C32 C33 H33 119.2 . .
C34 C33 H33 119.2 . .
C39 C34 C35 121.3(12) . .
C39 C34 C33 117.9(12) . .
C35 C34 C33 120.8(13) . .
C36 C35 C34 119.5(15) . .
C36 C35 H35 120.2 . .
C34 C35 H35 120.2 . .
C35 C36 C37 120.9(15) . .
C35 C36 H36 119.5 . .
C37 C36 H36 119.5 . .
C38 C37 C36 120.4(15) . .
C38 C37 H37 119.8 . .
C36 C37 H37 119.8 . .
C37 C38 C39 121.7(14) . .
C37 C38 H38 119.2 . .
C39 C38 H38 119.2 . .
C34 C39 C38 116.1(11) . .
C34 C39 C40 119.6(11) . .
C38 C39 C40 124.2(12) . .
C31 C40 C39 120.4(11) . .
C31 C40 C41 120.4(11) . .
C39 C40 C41 118.4(11) . .
N31 C41 C40 127.0(10) . .
N31 C41 H41 116.5 . .
C40 C41 H41 116.5 . .
C43 C42 N31 124.6(11) . .
C43 C42 C50 119.4(11) . .
N31 C42 C50 115.9(9) . .
C42 C43 C44 121.2(12) . .
C42 C43 H43 119.4 . .
C44 C43 H43 119.4 . .
C43 C44 C45 120.5(12) . .
C43 C44 H44 119.8 . .
C45 C44 H44 119.8 . .
C44 C45 C46 119.3(12) . .
C44 C45 H45 120.3 . .
C46 C45 H45 120.3 . .
C45 C46 C50 121.4(11) . .
C45 C46 C47 123.1(11) . .
C50 C46 C47 115.5(11) . .
C48 C47 C46 119.5(12) . .
C48 C47 H47 120.3 . .
C46 C47 H47 120.3 . .
C47 C48 C49 121.5(11) . .
C47 C48 H48 119.3 . .
C49 C48 H48 119.3 . .
N32 C49 C48 119.8(11) . .
N32 C49 C51 117.9(10) . .
C48 C49 C51 122.3(11) . .
N32 C50 C46 124.4(10) . .
N32 C50 C42 117.7(10) . .
C46 C50 C42 117.9(10) . .
C49 C51 H51A 109.5 . .
C49 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
C49 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
C61 O61 U1 119.5(6) . .
C74 O62 U1 116.8(5) . .
O61 C61 C74 116.1(10) . .
O61 C61 C62 123.2(9) . .
C74 C61 C62 120.8(11) . .
C61 C62 C67 120.1(10) . .
C61 C62 C63 119.2(11) . .
C67 C62 C63 120.6(9) . .
C64 C63 C62 120.9(12) . .
C64 C63 H63 119.5 . .
C62 C63 H63 119.5 . .
C63 C64 C65 119.1(12) . .
C63 C64 H64 120.5 . .
C65 C64 H64 120.5 . .
C66 C65 C64 121.2(12) . .
C66 C65 H65 119.4 . .
C64 C65 H65 119.4 . .
C65 C66 C67 121.6(12) . .
C65 C66 H66 119.2 . .
C67 C66 H66 119.2 . .
C66 C67 C62 116.5(10) . .
C66 C67 C68 124.0(11) . .
C62 C67 C68 119.4(10) . .
C73 C68 C69 117.3(9) . .
C73 C68 C67 120.2(10) . .
C69 C68 C67 122.5(10) . .
C70 C69 C68 121.6(10) . .
C70 C69 H69 119.2 . .
C68 C69 H69 119.2 . .
C71 C70 C69 120.1(11) . .
C71 C70 H70 120.0 . .
C69 C70 H70 120.0 . .
C72 C71 C70 120.7(11) . .
C72 C71 H71 119.7 . .
C70 C71 H71 119.7 . .
C71 C72 C73 120.5(10) . .
C71 C72 H72 119.7 . .
C73 C72 H72 119.7 . .
C68 C73 C72 119.8(10) . .
C68 C73 C74 119.0(9) . .
C72 C73 C74 121.2(9) . .
O62 C74 C61 117.2(9) . .
O62 C74 C73 122.3(8) . .
C61 C74 C73 120.5(9) . .
C85 N81 C81 117.5(13) . .
C82 C81 N81 120.2(17) . .
C82 C81 H81 119.9 . .
N81 C81 H81 119.9 . .
C81 C82 C83 121.9(17) . .
C81 C82 H82 119.0 . .
C83 C82 H82 119.0 . .
C84 C83 C82 118.5(15) . .
C84 C83 H83 120.7 . .
C82 C83 H83 120.7 . .
C83 C84 C85 120.5(15) . .
C83 C84 H84 119.7 . .
C85 C84 H84 119.7 . .
N81 C85 C84 121.2(14) . .
N81 C85 H85 119.4 . .
C84 C85 H85 119.4 . .
C90 N82 C86 114.6(15) . .
N82 C86 C87 123.6(16) . .
N82 C86 H86 118.2 . .
C87 C86 H86 118.2 . .
C88 C87 C86 119.2(16) . .
C88 C87 H87 120.4 . .
C86 C87 H87 120.4 . .
C87 C88 C89 120.0(16) . .
C87 C88 H88 120.0 . .
C89 C88 H88 120.0 . .
C90 C89 C88 115.5(17) . .
C90 C89 H89 122.3 . .
C88 C89 H89 122.3 . .
N82 C90 C89 127.0(17) . .
N82 C90 H90 116.5 . .
C89 C90 H90 116.5 . .
C95 N83 C91 115.9(18) . .
C92 C91 N83 118.9(18) . .
C92 C91 H91 120.6 . .
N83 C91 H91 120.6 . .
C93 C92 C91 119.1(17) . .
C93 C92 H92 120.4 . .
C91 C92 H92 120.4 . .
C92 C93 C94 121.4(18) . .
C92 C93 H93 119.3 . .
C94 C93 H93 119.3 . .
C95 C94 C93 124.0(17) . .
C95 C94 H94 118.0 . .
C93 C94 H94 118.0 . .
C94 C95 N83 120.6(17) . .
C94 C95 H95 119.7 . .
N83 C95 H95 119.7 . .
C96 N84 C100 113.4(19) . .
N84 C96 C97 122.1(19) . .
N84 C96 H96 118.9 . .
C97 C96 H96 118.9 . .
C98 C97 C96 121(2) . .
C98 C97 H97 119.3 . .
C96 C97 H97 119.3 . .
C99 C98 C97 119(3) . .
C99 C98 H98 120.4 . .
C97 C98 H98 120.4 . .
C98 C99 C100 124(2) . .
C98 C99 H99 118.1 . .
C100 C99 H99 118.1 . .
C99 C100 N84 120(2) . .
C99 C100 H100 120.0 . .
N84 C100 H100 120.0 . .
C102 N85 C101 112(4) 2_556 .
C102 C101 C103 119(8) . .
C102 C101 N85 126(4) . .
C103 C101 N85 10(10) . .
C102 C101 H101 117.1 . .
C103 C101 H101 122.8 . .
N85 C101 H101 117.1 . .
C101 C102 N85 121(3) . 2_556
C101 C102 C103 118(5) . 2_556
N85 C102 C103 8(10) 2_556 2_556
C101 C102 H102 119.4 . .
N85 C102 H102 119.4 2_556 .
C103 C102 H102 122.4 2_556 .
C101 C103 C102 122(10) . 2_556
C101 C103 H103 119.2 . .
C102 C103 H103 119.1 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 2.218(7) .
U1 O61 2.228(7) .
U1 O31 2.236(7) .
U1 O62 2.285(7) .
U1 N31 2.507(8) .
U1 N2 2.529(9) .
U1 N1 2.531(8) .
U1 N32 2.628(8) .
O1 C1 1.297(13) .
N1 C11 1.300(14) .
N1 C12 1.432(14) .
N2 C19 1.365(14) .
N2 C20 1.470(14) .
C1 C2 1.405(16) .
C1 C10 1.416(16) .
C2 C3 1.361(16) .
C2 H2 0.9500 .
C3 C4 1.410(17) .
C3 H3 0.9500 .
C4 C9 1.406(16) .
C4 C5 1.421(17) .
C5 C6 1.361(18) .
C5 H5 0.9500 .
C6 C7 1.398(17) .
C6 H6 0.9500 .
C7 C8 1.462(18) .
C7 H7 0.9500 .
C8 C9 1.434(17) .
C8 H8 0.9500 .
C9 C10 1.450(15) .
C10 C11 1.443(16) .
C11 H11 0.9500 .
C12 C13 1.354(15) .
C12 C20 1.440(15) .
C13 C14 1.370(16) .
C13 H13 0.9500 .
C14 C15 1.359(16) .
C14 H14 0.9500 .
C15 C16 1.389(16) .
C15 H15 0.9500 .
C16 C20 1.393(16) .
C16 C17 1.414(16) .
C17 C18 1.353(16) .
C17 H17 0.9500 .
C18 C19 1.412(16) .
C18 H18 0.9500 .
C19 C21 1.496(15) .
C21 H21A 0.9722 .
C21 H21B 0.9769 .
C21 H21C 0.9713 .
O31 C31 1.297(14) .
N31 C41 1.287(14) .
N31 C42 1.439(14) .
N32 C49 1.347(13) .
N32 C50 1.347(12) .
C31 C40 1.381(16) .
C31 C32 1.415(16) .
C32 C33 1.344(18) .
C32 H32 0.9500 .
C33 C34 1.416(18) .
C33 H33 0.9500 .
C34 C39 1.408(17) .
C34 C35 1.414(19) .
C35 C36 1.35(2) .
C35 H35 0.9500 .
C36 C37 1.39(2) .
C36 H36 0.9500 .
C37 C38 1.36(2) .
C37 H37 0.9500 .
C38 C39 1.424(16) .
C38 H38 0.9500 .
C39 C40 1.439(16) .
C40 C41 1.443(16) .
C41 H41 0.9500 .
C42 C43 1.361(15) .
C42 C50 1.441(15) .
C43 C44 1.380(17) .
C43 H43 0.9500 .
C44 C45 1.383(17) .
C44 H44 0.9500 .
C45 C46 1.385(16) .
C45 H45 0.9500 .
C46 C50 1.391(15) .
C46 C47 1.414(17) .
C47 C48 1.369(16) .
C47 H47 0.9500 .
C48 C49 1.382(16) .
C48 H48 0.9500 .
C49 C51 1.499(16) .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
O61 C61 1.358(13) .
O62 C74 1.359(11) .
C61 C74 1.382(13) .
C61 C62 1.399(15) .
C62 C67 1.405(15) .
C62 C63 1.420(15) .
C63 C64 1.352(16) .
C63 H63 0.9500 .
C64 C65 1.386(18) .
C64 H64 0.9500 .
C65 C66 1.380(16) .
C65 H65 0.9500 .
C66 C67 1.404(15) .
C66 H66 0.9500 .
C67 C68 1.424(14) .
C68 C73 1.406(14) .
C68 C69 1.410(15) .
C69 C70 1.377(15) .
C69 H69 0.9500 .
C70 C71 1.377(17) .
C70 H70 0.9500 .
C71 C72 1.355(16) .
C71 H71 0.9500 .
C72 C73 1.418(14) .
C72 H72 0.9500 .
C73 C74 1.422(14) .
N81 C85 1.312(17) .
N81 C81 1.475(19) .
C81 C82 1.26(2) .
C81 H81 0.9500 .
C82 C83 1.39(2) .
C82 H82 0.9500 .
C83 C84 1.354(19) .
C83 H83 0.9500 .
C84 C85 1.37(2) .
C84 H84 0.9500 .
C85 H85 0.9500 .
N82 C90 1.34(2) .
N82 C86 1.348(18) .
C86 C87 1.357(19) .
C86 H86 0.9500 .
C87 C88 1.35(2) .
C87 H87 0.9500 .
C88 C89 1.40(2) .
C88 H88 0.9500 .
C89 C90 1.35(2) .
C89 H89 0.9500 .
C90 H90 0.9500 .
N83 C95 1.41(2) .
N83 C91 1.43(2) .
C91 C92 1.39(2) .
C91 H91 0.9500 .
C92 C93 1.31(2) .
C92 H92 0.9500 .
C93 C94 1.33(2) .
C93 H93 0.9500 .
C94 C95 1.255(19) .
C94 H94 0.9500 .
C95 H95 0.9500 .
N84 C96 1.34(3) .
N84 C100 1.39(3) .
C96 C97 1.38(3) .
C96 H96 0.9500 .
C97 C98 1.28(3) .
C97 H97 0.9500 .
C98 C99 1.24(3) .
C98 H98 0.9500 .
C99 C100 1.36(3) .
C99 H99 0.9500 .
C100 H100 0.9500 .
N85 C102 1.37(7) 2_556
N85 C101 1.33(2) .
C101 C102 1.22(4) .
C101 C103 1.35(2) .
C101 H101 0.9500 .
C102 N85 1.37(7) 2_556
C102 C103 1.23(14) 2_556
C102 H102 0.9500 .
C103 C102 1.23(14) 2_556
C103 H103 0.9500 .
