#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308549.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_4308549
loop_
_publ_author_name
'Jean-Claude Berthet'
'Pierre Thuéry'
'Michel Ephritikhine'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      Bât. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       ephri@drecam.cea.fr
_publ_contact_author_fax         '33 (1) 69 08 66 40'
_publ_contact_author_name        'M. Ephritikhine'
_publ_contact_author_phone       '33 (1) 69 08 64 36'
_publ_section_title
;
New Efficient Synthesis of [UI4(MeCN)4]. X-ray Crystal Structures of
[UI2(MeCN)7][UI6], [UI4(py)3], and [U(dmf)9]I4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1142
_journal_page_last               1146
_journal_paper_doi               10.1021/ic048603p
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C27 H63 I4 N9 O9 U'
_chemical_formula_weight         1403.49
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5474(2)
_cell_length_b                   13.5474(2)
_cell_length_c                   53.2687(14)
_cell_measurement_reflns_used    37438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.41
_cell_volume                     9776.5(3)
_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 0.799
_diffrn_measured_fraction_theta_max 0.799
_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  0.1036
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            37438
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    5.895
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         13580
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0692
_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)+(0.0965P)²+126.9394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                11799
_reflns_number_total             13580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048603psi20041007_101646_1.cif
_cod_data_source_block           5
_cod_database_code               4308549
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
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 0.54194(5) 0.58748(6) 0.815676(12) 0.03277(18) Uani 1 1 d . . .
U2 U 0.13397(5) 0.06855(5) 0.683863(12) 0.03244(18) Uani 1 1 d . . .
I1 I 0.20076(16) 0.78863(13) 0.94115(4) 0.0747(6) Uani 1 1 d . . .
I2 I 0.04958(19) 0.44176(14) 0.62839(3) 0.0771(6) Uani 1 1 d . . .
I3 I 0.42944(14) 0.02125(12) 0.76730(3) 0.0582(4) Uani 1 1 d . . .
I4 I 0.77806(15) 0.67259(12) 0.90775(3) 0.0616(5) Uani 1 1 d . . .
I5 I 0.27056(12) 0.53076(11) 0.72241(3) 0.0495(4) Uani 1 1 d . . .
I6 I 0.35623(11) 0.83526(11) 0.60124(3) 0.0477(4) Uani 1 1 d . . .
I7 I 0.97696(15) 0.83132(15) 0.80498(3) 0.0709(5) Uani 1 1 d . . .
I8 I 0.84515(13) 0.34457(16) 0.77872(5) 0.0777(6) Uani 1 1 d . . .
O1 O 0.7011(9) 0.5417(10) 0.8304(3) 0.038(3) Uani 1 1 d . . .
O2 O 0.6557(9) 0.5894(10) 0.7818(2) 0.037(3) Uani 1 1 d . . .
O3 O 0.4931(9) 0.4734(10) 0.7816(2) 0.034(3) Uani 1 1 d . . .
O4 O 0.5423(11) 0.4186(10) 0.8281(3) 0.046(4) Uani 1 1 d . . .
O5 O 0.6410(11) 0.7322(11) 0.8198(2) 0.044(4) Uani 1 1 d . . .
O6 O 0.4767(9) 0.6847(10) 0.7831(2) 0.033(3) Uani 1 1 d . . .
O7 O 0.3702(10) 0.5481(10) 0.8190(2) 0.040(3) Uani 1 1 d . . .
O8 O 0.5302(13) 0.5735(13) 0.8596(3) 0.058(4) Uani 1 1 d . . .
O9 O 0.4509(12) 0.7218(12) 0.8346(3) 0.050(4) Uani 1 1 d . . .
O10 O -0.0012(11) 0.0561(11) 0.6554(3) 0.044(3) Uani 1 1 d U . .
O11 O -0.0208(11) 0.0587(12) 0.7056(3) 0.048(4) Uani 1 1 d . . .
O12 O 0.1370(10) -0.0665(10) 0.7125(2) 0.040(3) Uani 1 1 d . . .
O13 O 0.1363(11) -0.0892(9) 0.6637(3) 0.037(3) Uani 1 1 d . . .
O14 O 0.0627(14) 0.2252(12) 0.6852(3) 0.060(4) Uani 1 1 d . . .
O15 O 0.1721(13) 0.1253(12) 0.7255(3) 0.053(4) Uani 1 1 d . . .
O16 O 0.2990(10) 0.0055(10) 0.6864(3) 0.041(3) Uani 1 1 d . . .
O17 O 0.1892(11) 0.0971(12) 0.6422(2) 0.048(4) Uani 1 1 d . . .
O18 O 0.2556(10) 0.2057(10) 0.6817(3) 0.040(3) Uani 1 1 d . . .
N1 N 0.8308(11) 0.4793(12) 0.8531(3) 0.034(4) Uani 1 1 d . . .
N2 N 0.7865(13) 0.6025(13) 0.7563(3) 0.043(4) Uani 1 1 d . . .
N3 N 0.5150(14) 0.3362(14) 0.7581(4) 0.050(5) Uani 1 1 d . . .
N4 N 0.4820(11) 0.2656(13) 0.8252(3) 0.039(4) Uani 1 1 d . . .
N5 N 0.7210(13) 0.8595(14) 0.8375(3) 0.044(4) Uani 1 1 d . . .
N6 N 0.5198(12) 0.7395(11) 0.7451(3) 0.030(3) Uani 1 1 d . . .
N7 N 0.2109(13) 0.5791(11) 0.8087(3) 0.035(4) Uani 1 1 d . . .
N8 N 0.4524(14) 0.5888(16) 0.8973(3) 0.052(5) Uani 1 1 d . . .
N9 N 0.3643(15) 0.8573(14) 0.8436(4) 0.053(5) Uani 1 1 d . . .
N10 N -0.1278(14) -0.0206(14) 0.6357(3) 0.043(4) Uani 1 1 d . . .
N11 N -0.1406(13) 0.0496(15) 0.7349(3) 0.047(5) Uani 1 1 d . . .
N12 N 0.1756(12) -0.1772(12) 0.7442(3) 0.038(4) Uani 1 1 d . . .
N13 N 0.1172(19) -0.2617(19) 0.6684(4) 0.072(6) Uani 1 1 d U . .
N14 N -0.0447(13) 0.3523(13) 0.6923(3) 0.044(4) Uani 1 1 d . . .
N15 N 0.1575(14) 0.2115(17) 0.7600(3) 0.054(5) Uani 1 1 d . . .
N16 N 0.4589(16) -0.0187(16) 0.6813(4) 0.058(5) Uani 1 1 d U . .
N17 N 0.1689(14) 0.0846(14) 0.5997(3) 0.046(5) Uani 1 1 d . . .
N18 N 0.3344(14) 0.3372(14) 0.6671(4) 0.051(5) Uani 1 1 d . . .
C1 C 0.7356(16) 0.4855(17) 0.8466(4) 0.041(5) Uani 1 1 d . . .
H1 H 0.6916 0.4441 0.8549 0.049 Uiso 1 1 calc R . .
C2 C 0.8648(19) 0.4176(18) 0.8730(5) 0.056(6) Uani 1 1 d . . .
H2A H 0.8114 0.3773 0.8789 0.085 Uiso 1 1 calc R . .
H2B H 0.8890 0.4578 0.8865 0.085 Uiso 1 1 calc R . .
H2C H 0.9171 0.3760 0.8669 0.085 Uiso 1 1 calc R . .
C3 C 0.8993(15) 0.550(2) 0.8407(5) 0.062(7) Uani 1 1 d . . .
H3A H 0.8643 0.5861 0.8280 0.093 Uiso 1 1 calc R . .
H3B H 0.9528 0.5143 0.8331 0.093 Uiso 1 1 calc R . .
H3C H 0.9250 0.5951 0.8530 0.093 Uiso 1 1 calc R . .
C4 C 0.7455(17) 0.6112(16) 0.7782(4) 0.043(5) Uani 1 1 d . . .
H4 H 0.7830 0.6340 0.7916 0.052 Uiso 1 1 calc R . .
C5 C 0.8901(14) 0.622(2) 0.7532(4) 0.052(6) Uani 1 1 d . . .
H5A H 0.9162 0.6497 0.7684 0.078 Uiso 1 1 calc R . .
H5B H 0.8993 0.6679 0.7396 0.078 Uiso 1 1 calc R . .
H5C H 0.9239 0.5616 0.7494 0.078 Uiso 1 1 calc R . .
C6 C 0.7343(16) 0.5611(19) 0.7351(4) 0.050(6) Uani 1 1 d . . .
H6A H 0.6657 0.5536 0.7393 0.075 Uiso 1 1 calc R . .
H6B H 0.7618 0.4977 0.7310 0.075 Uiso 1 1 calc R . .
H6C H 0.7406 0.6043 0.7209 0.075 Uiso 1 1 calc R . .
C7 C 0.5503(14) 0.4132(13) 0.7705(4) 0.035(4) Uani 1 1 d . . .
H7 H 0.6182 0.4234 0.7712 0.042 Uiso 1 1 calc R . .
C8 C 0.5817(17) 0.2736(19) 0.7441(5) 0.055(6) Uani 1 1 d . . .
H8A H 0.6484 0.2953 0.7467 0.083 Uiso 1 1 calc R . .
H8B H 0.5661 0.2773 0.7266 0.083 Uiso 1 1 calc R . .
H8C H 0.5749 0.2066 0.7497 0.083 Uiso 1 1 calc R . .
C9 C 0.4075(18) 0.3150(18) 0.7571(5) 0.055(6) Uani 1 1 d . . .
H9A H 0.3726 0.3620 0.7672 0.082 Uiso 1 1 calc R . .
H9B H 0.3954 0.2496 0.7633 0.082 Uiso 1 1 calc R . .
H9C H 0.3850 0.3198 0.7400 0.082 Uiso 1 1 calc R . .
C10 C 0.472(2) 0.3556(16) 0.8297(4) 0.046(6) Uani 1 1 d . . .
H10 H 0.4099 0.3781 0.8346 0.055 Uiso 1 1 calc R . .
C11 C 0.403(2) 0.194(2) 0.8280(5) 0.065(7) Uani 1 1 d U . .
H11A H 0.3448 0.2261 0.8342 0.097 Uiso 1 1 calc R . .
H11B H 0.4230 0.1436 0.8397 0.097 Uiso 1 1 calc R . .
H11C H 0.3890 0.1639 0.8121 0.097 Uiso 1 1 calc R . .
C12 C 0.5748(17) 0.2191(18) 0.8161(5) 0.058(6) Uani 1 1 d . . .
H12A H 0.6250 0.2686 0.8144 0.087 Uiso 1 1 calc R . .
H12B H 0.5633 0.1884 0.8001 0.087 Uiso 1 1 calc R . .
H12C H 0.5960 0.1701 0.8280 0.087 Uiso 1 1 calc R . .
C13 C 0.6987(14) 0.7678(13) 0.8372(3) 0.030(4) Uani 1 1 d . . .
H13 H 0.7238 0.7261 0.8495 0.035 Uiso 1 1 calc R . .
C14 C 0.7894(17) 0.8978(14) 0.8563(4) 0.042(5) Uani 1 1 d . . .
H14A H 0.8062 0.8462 0.8679 0.063 Uiso 1 1 calc R . .
H14B H 0.7588 0.9512 0.8652 0.063 Uiso 1 1 calc R . .
H14C H 0.8481 0.9210 0.8481 0.063 Uiso 1 1 calc R . .
C15 C 0.6852(19) 0.930(2) 0.8172(5) 0.061(7) Uani 1 1 d . . .
H15A H 0.6410 0.8965 0.8061 0.092 Uiso 1 1 calc R . .
H15B H 0.7407 0.9547 0.8079 0.092 Uiso 1 1 calc R . .
H15C H 0.6513 0.9848 0.8249 0.092 Uiso 1 1 calc R . .
C16 C 0.4709(13) 0.6860(15) 0.7602(3) 0.032(4) Uani 1 1 d . . .
H16 H 0.4256 0.6428 0.7531 0.039 Uiso 1 1 calc R . .
C17 C 0.6004(17) 0.8004(17) 0.7539(5) 0.049(6) Uani 1 1 d . . .
H17A H 0.6099 0.7897 0.7716 0.074 Uiso 1 1 calc R . .
H17B H 0.5851 0.8686 0.7510 0.074 Uiso 1 1 calc R . .
H17C H 0.6596 0.7833 0.7450 0.074 Uiso 1 1 calc R . .
C18 C 0.4971(18) 0.749(2) 0.7182(4) 0.059(7) Uani 1 1 d . . .
H18A H 0.4445 0.7044 0.7139 0.088 Uiso 1 1 calc R . .
H18B H 0.5547 0.7329 0.7085 0.088 Uiso 1 1 calc R . .
H18C H 0.4772 0.8154 0.7146 0.088 Uiso 1 1 calc R . .
C19 C 0.2982(13) 0.5447(14) 0.8042(4) 0.032(4) Uani 1 1 d . . .
H19 H 0.3084 0.5149 0.7887 0.038 Uiso 1 1 calc R . .
C20 C 0.1894(17) 0.6300(13) 0.8331(4) 0.040(5) Uani 1 1 d . . .
H20A H 0.2497 0.6388 0.8423 0.060 Uiso 1 1 calc R . .
H20B H 0.1446 0.5905 0.8428 0.060 Uiso 1 1 calc R . .
H20C H 0.1601 0.6932 0.8298 0.060 Uiso 1 1 calc R . .
C21 C 0.1285(14) 0.5574(18) 0.7927(4) 0.046(5) Uani 1 1 d . . .
H21A H 0.1514 0.5246 0.7778 0.069 Uiso 1 1 calc R . .
H21B H 0.0960 0.6178 0.7881 0.069 Uiso 1 1 calc R . .
H21C H 0.0829 0.5154 0.8014 0.069 Uiso 1 1 calc R . .
C22 C 0.5259(18) 0.6031(19) 0.8811(5) 0.055(6) Uani 1 1 d . . .
H22 H 0.5795 0.6396 0.8868 0.066 Uiso 1 1 calc R . .
C23 C 0.367(2) 0.536(2) 0.8893(7) 0.078(9) Uani 1 1 d . . .
H23A H 0.3741 0.5183 0.8719 0.117 Uiso 1 1 calc R . .
H23B H 0.3096 0.5764 0.8914 0.117 Uiso 1 1 calc R . .
H23C H 0.3602 0.4768 0.8992 0.117 Uiso 1 1 calc R . .
C24 C 0.459(2) 0.621(2) 0.9233(5) 0.065(7) Uani 1 1 d U . .
H24A H 0.5200 0.6563 0.9257 0.098 Uiso 1 1 calc R . .
H24B H 0.4579 0.5644 0.9342 0.098 Uiso 1 1 calc R . .
H24C H 0.4046 0.6634 0.9271 0.098 Uiso 1 1 calc R . .
C25 C 0.4152(15) 0.8020(15) 0.8279(4) 0.037(5) Uani 1 1 d . . .
H25 H 0.4246 0.8235 0.8115 0.044 Uiso 1 1 calc R . .
C26 C 0.350(2) 0.831(2) 0.8689(5) 0.069(7) Uani 1 1 d . . .
H26A H 0.3820 0.7693 0.8722 0.104 Uiso 1 1 calc R . .
H26B H 0.2806 0.8250 0.8722 0.104 Uiso 1 1 calc R . .
H26C H 0.3775 0.8812 0.8796 0.104 Uiso 1 1 calc R . .
C27 C 0.317(2) 0.947(2) 0.8340(6) 0.077(8) Uani 1 1 d U . .
H27A H 0.3318 0.9544 0.8165 0.116 Uiso 1 1 calc R . .
H27B H 0.3406 1.0033 0.8430 0.116 Uiso 1 1 calc R . .
H27C H 0.2465 0.9417 0.8361 0.116 Uiso 1 1 calc R . .
C28 C -0.0917(17) 0.0389(18) 0.6532(4) 0.050(6) Uani 1 1 d . . .
H28 H -0.1352 0.0691 0.6643 0.060 Uiso 1 1 calc R . .
C29 C -0.060(2) -0.074(2) 0.6199(5) 0.064(7) Uani 1 1 d U . .
H29A H 0.0063 -0.0576 0.6245 0.096 Uiso 1 1 calc R . .
H29B H -0.0712 -0.0555 0.6027 0.096 Uiso 1 1 calc R . .
H29C H -0.0707 -0.1433 0.6219 0.096 Uiso 1 1 calc R . .
C30 C -0.2378(18) -0.028(2) 0.6335(4) 0.066(8) Uani 1 1 d . . .
H30A H -0.2681 0.0142 0.6458 0.099 Uiso 1 1 calc R . .
H30B H -0.2579 -0.0949 0.6363 0.099 Uiso 1 1 calc R . .
H30C H -0.2577 -0.0075 0.6170 0.099 Uiso 1 1 calc R . .
C31 C -0.0522(17) 0.0254(18) 0.7246(4) 0.049(6) Uani 1 1 d . . .
H31 H -0.0134 -0.0205 0.7331 0.059 Uiso 1 1 calc R . .
C32 C -0.175(2) 0.015(2) 0.7583(6) 0.079(8) Uani 1 1 d U . .
H32A H -0.1310 -0.0347 0.7646 0.118 Uiso 1 1 calc R . .
H32B H -0.2398 -0.0137 0.7561 0.118 Uiso 1 1 calc R . .
H32C H -0.1790 0.0684 0.7700 0.118 Uiso 1 1 calc R . .
C33 C -0.202(2) 0.126(2) 0.7218(6) 0.077(8) Uani 1 1 d U . .
H33A H -0.1703 0.1446 0.7064 0.116 Uiso 1 1 calc R . .
H33B H -0.2086 0.1829 0.7324 0.116 Uiso 1 1 calc R . .
H33C H -0.2660 0.0993 0.7183 0.116 Uiso 1 1 calc R . .
C34 C 0.1941(15) -0.0957(16) 0.7300(4) 0.044(5) Uani 1 1 d . . .
H34 H 0.2512 -0.0598 0.7332 0.052 Uiso 1 1 calc R . .
C35 C 0.0861(18) -0.2389(19) 0.7380(4) 0.056(6) Uani 1 1 d . . .
H35A H 0.0532 -0.2118 0.7236 0.083 Uiso 1 1 calc R . .
H35B H 0.0419 -0.2389 0.7521 0.083 Uiso 1 1 calc R . .
H35C H 0.1064 -0.3053 0.7345 0.083 Uiso 1 1 calc R . .
C36 C 0.2366(18) -0.2033(18) 0.7655(4) 0.050(6) Uani 1 1 d . . .
H36A H 0.2897 -0.1568 0.7670 0.075 Uiso 1 1 calc R . .
H36B H 0.2631 -0.2684 0.7631 0.075 Uiso 1 1 calc R . .
H36C H 0.1974 -0.2021 0.7805 0.075 Uiso 1 1 calc R . .
C37 C 0.078(2) -0.164(2) 0.6712(5) 0.072(9) Uani 1 1 d . . .
H37 H 0.0162 -0.1535 0.6780 0.086 Uiso 1 1 calc R . .
C38 C 0.205(2) -0.282(3) 0.6589(6) 0.085(9) Uani 1 1 d U . .
H38A H 0.2369 -0.2213 0.6539 0.128 Uiso 1 1 calc R . .
H38B H 0.1983 -0.3240 0.6446 0.128 Uiso 1 1 calc R . .
H38C H 0.2449 -0.3140 0.6714 0.128 Uiso 1 1 calc R . .
C39 C 0.051(3) -0.339(3) 0.6769(7) 0.093(10) Uani 1 1 d U . .
H39A H -0.0094 -0.3099 0.6829 0.140 Uiso 1 1 calc R . .
H39B H 0.0815 -0.3755 0.6903 0.140 Uiso 1 1 calc R . .
H39C H 0.0363 -0.3828 0.6632 0.140 Uiso 1 1 calc R . .
C40 C -0.018(2) 0.2706(19) 0.6802(5) 0.064(8) Uani 1 1 d . . .
H40 H -0.0597 0.2456 0.6678 0.077 Uiso 1 1 calc R . .
C41 C 0.018(3) 0.392(3) 0.7112(6) 0.093(10) Uani 1 1 d U . .
H41A H 0.0696 0.3451 0.7148 0.139 Uiso 1 1 calc R . .
H41B H -0.0196 0.4041 0.7261 0.139 Uiso 1 1 calc R . .
H41C H 0.0468 0.4522 0.7053 0.139 Uiso 1 1 calc R . .
C42 C -0.133(2) 0.408(3) 0.6834(6) 0.087(9) Uani 1 1 d U . .
H42A H -0.1668 0.3691 0.6711 0.131 Uiso 1 1 calc R . .
H42B H -0.1121 0.4690 0.6762 0.131 Uiso 1 1 calc R . .
H42C H -0.1758 0.4201 0.6974 0.131 Uiso 1 1 calc R . .
C43 C 0.1807(18) 0.2032(17) 0.7363(3) 0.048(6) Uani 1 1 d . . .
H43 H 0.2042 0.2580 0.7277 0.057 Uiso 1 1 calc R . .
C44 C 0.132(2) 0.136(2) 0.7758(5) 0.060(6) Uani 1 1 d U . .
H44A H 0.1353 0.0745 0.7669 0.090 Uiso 1 1 calc R . .
H44B H 0.0654 0.1463 0.7817 0.090 Uiso 1 1 calc R . .
H44C H 0.1760 0.1348 0.7898 0.090 Uiso 1 1 calc R . .
C45 C 0.154(2) 0.311(2) 0.7725(5) 0.062(6) Uani 1 1 d U . .
H45A H 0.1718 0.3611 0.7606 0.093 Uiso 1 1 calc R . .
H45B H 0.1993 0.3120 0.7863 0.093 Uiso 1 1 calc R . .
H45C H 0.0883 0.3231 0.7785 0.093 Uiso 1 1 calc R . .
C46 C 0.353(3) -0.028(3) 0.6723(7) 0.097(11) Uani 1 1 d U . .
H46 H 0.3343 -0.0572 0.6572 0.116 Uiso 1 1 calc R . .
C47 C 0.523(3) 0.023(3) 0.6993(7) 0.104(11) Uani 1 1 d U . .
H47A H 0.5889 0.0014 0.6962 0.156 Uiso 1 1 calc R . .
H47B H 0.5025 0.0026 0.7158 0.156 Uiso 1 1 calc R . .
H47C H 0.5196 0.0938 0.6982 0.156 Uiso 1 1 calc R . .
C48 C 0.511(3) -0.075(3) 0.6605(7) 0.101(11) Uani 1 1 d U . .
H48A H 0.5808 -0.0748 0.6636 0.152 Uiso 1 1 calc R . .
H48B H 0.4980 -0.0429 0.6447 0.152 Uiso 1 1 calc R . .
H48C H 0.4871 -0.1412 0.6599 0.152 Uiso 1 1 calc R . .
C49 C 0.1764(18) 0.0500(18) 0.6219(4) 0.050(6) Uani 1 1 d . . .
H49 H 0.1720 -0.0183 0.6234 0.061 Uiso 1 1 calc R . .
C50 C 0.177(2) 0.192(2) 0.5958(4) 0.065(8) Uani 1 1 d . . .
H50A H 0.1894 0.2243 0.6115 0.097 Uiso 1 1 calc R . .
H50B H 0.1162 0.2168 0.5888 0.097 Uiso 1 1 calc R . .
H50C H 0.2301 0.2058 0.5844 0.097 Uiso 1 1 calc R . .
C51 C 0.1468(18) 0.0251(17) 0.5777(5) 0.054(6) Uani 1 1 d . . .
H51A H 0.1402 -0.0429 0.5825 0.081 Uiso 1 1 calc R . .
H51B H 0.1994 0.0315 0.5657 0.081 Uiso 1 1 calc R . .
H51C H 0.0862 0.0474 0.5703 0.081 Uiso 1 1 calc R . .
C52 C 0.2528(18) 0.2791(17) 0.6681(4) 0.050(6) Uani 1 1 d . . .
H52 H 0.1967 0.2942 0.6588 0.060 Uiso 1 1 calc R . .
C53 C 0.328(2) 0.4278(19) 0.6519(5) 0.071(8) Uani 1 1 d . . .
H53A H 0.2672 0.4282 0.6428 0.106 Uiso 1 1 calc R . .
H53B H 0.3825 0.4300 0.6404 0.106 Uiso 1 1 calc R . .
H53C H 0.3307 0.4843 0.6628 0.106 Uiso 1 1 calc R . .
C54 C 0.420(2) 0.323(2) 0.6827(6) 0.080(8) Uani 1 1 d U . .
H54A H 0.4139 0.2612 0.6915 0.119 Uiso 1 1 calc R . .
H54B H 0.4247 0.3758 0.6945 0.119 Uiso 1 1 calc R . .
H54C H 0.4780 0.3216 0.6724 0.119 Uiso 1 1 calc R . .
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'
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'
O O 0.0106 0.0060 '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
O6 U1 O8 138.9(5) . . ?
O6 U1 O2 71.1(5) . . ?
O8 U1 O2 143.2(6) . . ?
O6 U1 O1 137.0(4) . . ?
O8 U1 O1 73.2(5) . . ?
O2 U1 O1 70.5(5) . . ?
O6 U1 O4 138.0(5) . . ?
O8 U1 O4 69.3(6) . . ?
O2 U1 O4 102.7(5) . . ?
O1 U1 O4 69.9(5) . . ?
O6 U1 O5 79.5(5) . . ?
O8 U1 O5 90.8(6) . . ?
O2 U1 O5 72.2(5) . . ?
O1 U1 O5 71.0(5) . . ?
O4 U1 O5 139.8(5) . . ?
O6 U1 O7 79.3(5) . . ?
O8 U1 O7 81.0(5) . . ?
O2 U1 O7 133.6(5) . . ?
O1 U1 O7 143.0(5) . . ?
O4 U1 O7 76.5(5) . . ?
O5 U1 O7 136.3(5) . . ?
O6 U1 O9 72.2(5) . . ?
O8 U1 O9 67.2(6) . . ?
O2 U1 O9 129.8(5) . . ?
O1 U1 O9 121.4(5) . . ?
O4 U1 O9 127.5(6) . . ?
O5 U1 O9 68.3(5) . . ?
O7 U1 O9 69.0(5) . . ?
O6 U1 O3 73.0(5) . . ?
O8 U1 O3 131.4(6) . . ?
O2 U1 O3 67.8(5) . . ?
O1 U1 O3 108.8(5) . . ?
O4 U1 O3 66.6(5) . . ?
O5 U1 O3 136.9(5) . . ?
O7 U1 O3 69.8(4) . . ?
O9 U1 O3 129.7(5) . . ?
O14 U2 O17 90.6(6) . . ?
O14 U2 O12 133.3(5) . . ?
O17 U2 O12 136.0(5) . . ?
O14 U2 O10 76.4(6) . . ?
O17 U2 O10 70.0(5) . . ?
O12 U2 O10 111.5(5) . . ?
O14 U2 O13 146.2(6) . . ?
O17 U2 O13 73.8(5) . . ?
O12 U2 O13 66.6(5) . . ?
O10 U2 O13 70.2(5) . . ?
O14 U2 O16 135.1(6) . . ?
O17 U2 O16 79.5(5) . . ?
O12 U2 O16 71.0(5) . . ?
O10 U2 O16 136.7(5) . . ?
O13 U2 O16 72.3(5) . . ?
O14 U2 O11 71.0(6) . . ?
O17 U2 O11 137.3(5) . . ?
O12 U2 O11 70.3(5) . . ?
O10 U2 O11 68.4(5) . . ?
O13 U2 O11 100.3(5) . . ?
O16 U2 O11 140.1(5) . . ?
O14 U2 O15 76.7(6) . . ?
O17 U2 O15 138.0(5) . . ?
O12 U2 O15 69.5(5) . . ?
O10 U2 O15 140.8(6) . . ?
O13 U2 O15 134.2(5) . . ?
O16 U2 O15 82.0(6) . . ?
O11 U2 O15 76.1(6) . . ?
O14 U2 O18 66.2(6) . . ?
O17 U2 O18 68.1(5) . . ?
O12 U2 O18 126.3(5) . . ?
O10 U2 O18 122.2(5) . . ?
O13 U2 O18 129.7(5) . . ?
O16 U2 O18 69.5(4) . . ?
O11 U2 O18 130.0(5) . . ?
O15 U2 O18 70.2(5) . . ?
C1 O1 U1 137.1(13) . . ?
C4 O2 U1 137.9(13) . . ?
C7 O3 U1 125.3(12) . . ?
C10 O4 U1 131.1(14) . . ?
C13 O5 U1 134.8(12) . . ?
C16 O6 U1 140.2(12) . . ?
C19 O7 U1 135.9(12) . . ?
C22 O8 U1 156.1(17) . . ?
C25 O9 U1 137.5(14) . . ?
C28 O10 U2 145.3(14) . . ?
C31 O11 U2 138.2(15) . . ?
C34 O12 U2 135.8(13) . . ?
C37 O13 U2 122.3(15) . . ?
C40 O14 U2 141.5(16) . . ?
C43 O15 U2 137.7(14) . . ?
C46 O16 U2 134(2) . . ?
C49 O17 U2 132.2(14) . . ?
C52 O18 U2 127.5(15) . . ?
C1 N1 C2 122.7(18) . . ?
C1 N1 C3 116.4(17) . . ?
C2 N1 C3 120.4(17) . . ?
C4 N2 C5 120(2) . . ?
C4 N2 C6 121.9(19) . . ?
C5 N2 C6 117.3(18) . . ?
C7 N3 C8 119.6(18) . . ?
C7 N3 C9 121.7(19) . . ?
C8 N3 C9 118.7(18) . . ?
C10 N4 C11 123(2) . . ?
C10 N4 C12 125(2) . . ?
C11 N4 C12 111.8(19) . . ?
C13 N5 C14 120.3(18) . . ?
C13 N5 C15 121.9(18) . . ?
C14 N5 C15 117.6(17) . . ?
C16 N6 C17 120.8(17) . . ?
C16 N6 C18 124.0(18) . . ?
C17 N6 C18 115.2(18) . . ?
C19 N7 C21 121.8(17) . . ?
C19 N7 C20 120.3(18) . . ?
C21 N7 C20 117.2(17) . . ?
C22 N8 C23 119(2) . . ?
C22 N8 C24 122(2) . . ?
C23 N8 C24 119(2) . . ?
C25 N9 C26 123(2) . . ?
C25 N9 C27 118(2) . . ?
C26 N9 C27 119(2) . . ?
C28 N10 C29 119(2) . . ?
C28 N10 C30 118(2) . . ?
C29 N10 C30 124(2) . . ?
C31 N11 C32 125(2) . . ?
C31 N11 C33 117.8(19) . . ?
C32 N11 C33 117(2) . . ?
C34 N12 C36 121.8(19) . . ?
C34 N12 C35 118.6(17) . . ?
C36 N12 C35 119.5(17) . . ?
C38 N13 C37 124(3) . . ?
C38 N13 C39 122(3) . . ?
C37 N13 C39 114(3) . . ?
C40 N14 C41 120(2) . . ?
C40 N14 C42 119(2) . . ?
C41 N14 C42 121(2) . . ?
C43 N15 C44 126(2) . . ?
C43 N15 C45 121(2) . . ?
C44 N15 C45 112.8(19) . . ?
C47 N16 C48 114(3) . . ?
C47 N16 C46 146(3) . . ?
C48 N16 C46 100(3) . . ?
C49 N17 C51 124(2) . . ?
C49 N17 C50 119.3(19) . . ?
C51 N17 C50 116.5(18) . . ?
C52 N18 C54 124(2) . . ?
C52 N18 C53 117(2) . . ?
C54 N18 C53 118(2) . . ?
O1 C1 N1 125.6(19) . . ?
O2 C4 N2 122(2) . . ?
O3 C7 N3 121.1(18) . . ?
N4 C10 O4 124(2) . . ?
N5 C13 O5 120.6(18) . . ?
O6 C16 N6 127(2) . . ?
O7 C19 N7 125.6(19) . . ?
O8 C22 N8 127(2) . . ?
O9 C25 N9 121(2) . . ?
O10 C28 N10 123(2) . . ?
O11 C31 N11 125(2) . . ?
O12 C34 N12 123(2) . . ?
O13 C37 N13 117(3) . . ?
O14 C40 N14 122(2) . . ?
O15 C43 N15 121(2) . . ?
O16 C46 N16 111(3) . . ?
O17 C49 N17 128(2) . . ?
O18 C52 N18 118(2) . . ?
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 O6 2.352(12) . ?
U1 O8 2.354(15) . ?
U1 O2 2.373(11) . ?
U1 O1 2.377(13) . ?
U1 O4 2.381(14) . ?
U1 O5 2.386(14) . ?
U1 O7 2.393(14) . ?
U1 O9 2.418(15) . ?
U1 O3 2.473(12) . ?
U2 O14 2.333(17) . ?
U2 O17 2.376(11) . ?
U2 O12 2.383(12) . ?
U2 O10 2.385(14) . ?
U2 O13 2.392(13) . ?
U2 O16 2.397(14) . ?
U2 O11 2.400(13) . ?
U2 O15 2.406(14) . ?
U2 O18 2.486(13) . ?
O1 C1 1.24(2) . ?
O2 C4 1.27(3) . ?
O3 C7 1.27(2) . ?
O4 C10 1.28(3) . ?
O5 C13 1.31(2) . ?
O6 C16 1.22(2) . ?
O7 C19 1.25(2) . ?
O8 C22 1.21(3) . ?
O9 C25 1.24(3) . ?
O10 C28 1.25(3) . ?
O11 C31 1.19(2) . ?
O12 C34 1.27(2) . ?
O13 C37 1.35(4) . ?
O14 C40 1.29(3) . ?
O15 C43 1.21(3) . ?
O16 C46 1.14(4) . ?
O17 C49 1.27(3) . ?
O18 C52 1.23(3) . ?
N1 C1 1.34(3) . ?
N1 C2 1.43(3) . ?
N1 C3 1.49(3) . ?
N2 C4 1.30(3) . ?
N2 C5 1.44(3) . ?
N2 C6 1.45(3) . ?
N3 C7 1.33(3) . ?
N3 C8 1.45(3) . ?
N3 C9 1.49(3) . ?
N4 C10 1.25(3) . ?
N4 C11 1.46(3) . ?
N4 C12 1.49(3) . ?
N5 C13 1.28(3) . ?
N5 C14 1.46(2) . ?
N5 C15 1.52(3) . ?
N6 C16 1.27(2) . ?
N6 C17 1.45(3) . ?
N6 C18 1.47(3) . ?
N7 C19 1.29(3) . ?
N7 C21 1.44(3) . ?
N7 C20 1.50(2) . ?
N8 C22 1.33(3) . ?
N8 C23 1.43(4) . ?
N8 C24 1.45(3) . ?
N9 C25 1.32(3) . ?
N9 C26 1.41(3) . ?
N9 C27 1.47(4) . ?
N10 C28 1.32(3) . ?
N10 C29 1.44(3) . ?
N10 C30 1.50(3) . ?
N11 C31 1.36(3) . ?
N11 C32 1.41(3) . ?
N11 C33 1.50(3) . ?
N12 C34 1.36(3) . ?
N12 C36 1.45(3) . ?
N12 C35 1.51(3) . ?
N13 C38 1.32(4) . ?
N13 C37 1.43(4) . ?
N13 C39 1.45(4) . ?
N14 C40 1.33(3) . ?
N14 C41 1.42(4) . ?
N14 C42 1.48(4) . ?
N15 C43 1.30(3) . ?
N15 C44 1.37(3) . ?
N15 C45 1.50(3) . ?
N16 C47 1.41(4) . ?
N16 C48 1.52(4) . ?
N16 C46 1.52(4) . ?
N17 C49 1.27(3) . ?
N17 C51 1.46(3) . ?
N17 C50 1.48(3) . ?
N18 C52 1.36(3) . ?
N18 C54 1.44(4) . ?
N18 C53 1.47(3) . ?
