#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008209.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_7008209
loop_
_publ_author_name
'Mehdoui, Thouraya'
'Berthet, Jean-Claude'
'Thuery, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 The distinct affinity of cyclopentadienyl ligands towards trivalent
 uranium over lanthanide ions. Evidence for cooperative ligation and
 back-bonding in the actinide complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1263
_journal_page_last               1272
_journal_paper_doi               10.1039/b419088b
_journal_year                    2005
_chemical_formula_sum            'C24 H28 I2 N3 U'
_chemical_formula_weight         850.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.423(9)
_cell_angle_beta                 93.827(8)
_cell_angle_gamma                108.547(9)
_cell_formula_units_Z            2
_cell_length_a                   8.4321(13)
_cell_length_b                   8.8209(14)
_cell_length_c                   19.053(3)
_cell_measurement_reflns_used    8656
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.21
_cell_volume                     1298.0(4)
_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 0.915
_diffrn_measured_fraction_theta_max 0.915
_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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8656
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    8.646
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.056
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+6.8378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                3264
_reflns_number_total             4511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419088b.txt
_cod_data_source_block           6
_cod_database_code               7008209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.52331(6) 0.26041(6) 0.26178(3) 0.03356(16) Uani 1 1 d . . .
I1 I 0.77174(11) 0.14250(11) 0.16568(5) 0.0411(2) Uani 1 1 d . . .
I2 I 0.33104(12) 0.29929(12) 0.39968(5) 0.0455(3) Uani 1 1 d . . .
N1 N 0.2859(13) -0.0286(13) 0.2238(6) 0.037(3) Uani 1 1 d . . .
N2 N 0.6313(13) 0.0827(13) 0.3426(6) 0.039(3) Uani 1 1 d . . .
N3 N 0.8025(14) 0.4751(14) 0.3439(6) 0.037(3) Uani 1 1 d . . .
C1 C 0.3975(15) 0.3418(16) 0.1361(8) 0.036(3) Uani 1 1 d . . .
C2 C 0.2886(18) 0.3534(17) 0.1902(8) 0.042(3) Uani 1 1 d . . .
H2 H 0.1781 0.2825 0.1866 0.050 Uiso 1 1 calc R . .
C3 C 0.3747(19) 0.4894(18) 0.2502(9) 0.049(4) Uani 1 1 d . . .
H3 H 0.3283 0.5225 0.2913 0.058 Uiso 1 1 calc R . .
C4 C 0.5507(13) 0.5711(14) 0.2374(6) 0.021(2) Uani 1 1 d . . .
H4 H 0.6360 0.6626 0.2668 0.026 Uiso 1 1 calc R . .
C5 C 0.5532(17) 0.4688(17) 0.1662(8) 0.042(4) Uani 1 1 d . . .
H5 H 0.6486 0.4860 0.1429 0.050 Uiso 1 1 calc R . .
C6 C 0.3445(19) 0.2302(16) 0.0593(8) 0.044(4) Uani 1 1 d . . .
C7 C 0.275(2) 0.0515(17) 0.0590(9) 0.056(4) Uani 1 1 d . . .
H7A H 0.3628 0.0182 0.0782 0.083 Uiso 1 1 calc R . .
H7B H 0.2303 -0.0134 0.0101 0.083 Uiso 1 1 calc R . .
H7C H 0.1857 0.0349 0.0885 0.083 Uiso 1 1 calc R . .
C8 C 0.203(2) 0.274(2) 0.0222(9) 0.054(4) Uani 1 1 d . . .
H8A H 0.1102 0.2579 0.0497 0.080 Uiso 1 1 calc R . .
H8B H 0.1647 0.2034 -0.0261 0.080 Uiso 1 1 calc R . .
H8C H 0.2453 0.3869 0.0198 0.080 Uiso 1 1 calc R . .
C9 C 0.490(2) 0.2608(18) 0.0172(8) 0.051(4) Uani 1 1 d . . .
H9A H 0.5247 0.3728 0.0129 0.077 Uiso 1 1 calc R . .
H9B H 0.4562 0.1867 -0.0304 0.077 Uiso 1 1 calc R . .
H9C H 0.5826 0.2426 0.0420 0.077 Uiso 1 1 calc R . .
C10 C 0.1194(17) -0.0518(17) 0.2183(8) 0.040(3) Uani 1 1 d . . .
H10 H 0.0850 0.0342 0.2412 0.048 Uiso 1 1 calc R . .
C11 C -0.0044(17) -0.2007(19) 0.1792(8) 0.043(4) Uani 1 1 d . . .
H11 H -0.1182 -0.2113 0.1757 0.052 Uiso 1 1 calc R . .
C12 C 0.0433(18) -0.3300(18) 0.1465(8) 0.044(4) Uani 1 1 d . . .
H12 H -0.0376 -0.4304 0.1218 0.053 Uiso 1 1 calc R . .
C13 C 0.2155(18) -0.3090(16) 0.1507(8) 0.041(3) Uani 1 1 d . . .
H13 H 0.2526 -0.3935 0.1282 0.049 Uiso 1 1 calc R . .
C14 C 0.3280(19) -0.1578(17) 0.1894(8) 0.043(3) Uani 1 1 d . . .
H14 H 0.4426 -0.1436 0.1921 0.051 Uiso 1 1 calc R . .
C15 C 0.5209(17) -0.0203(19) 0.3723(8) 0.045(4) Uani 1 1 d . . .
H15 H 0.4080 -0.0281 0.3661 0.054 Uiso 1 1 calc R . .
C16 C 0.570(2) -0.1192(17) 0.4132(9) 0.049(4) Uani 1 1 d . . .
H16 H 0.4910 -0.1942 0.4319 0.059 Uiso 1 1 calc R . .
C17 C 0.7394(19) -0.1007(17) 0.4244(8) 0.047(4) Uani 1 1 d . . .
H17 H 0.7757 -0.1591 0.4534 0.056 Uiso 1 1 calc R . .
C18 C 0.8562(16) 0.0045(15) 0.3928(7) 0.034(3) Uani 1 1 d . . .
H18 H 0.9699 0.0147 0.3983 0.041 Uiso 1 1 calc R . .
C19 C 0.7958(15) 0.0934(16) 0.3525(8) 0.035(3) Uani 1 1 d . . .
H19 H 0.8724 0.1644 0.3311 0.042 Uiso 1 1 calc R . .
C20 C 0.8212(16) 0.5146(17) 0.4156(8) 0.039(3) Uani 1 1 d . . .
H20 H 0.7337 0.4597 0.4380 0.047 Uiso 1 1 calc R . .
C21 C 0.9621(17) 0.632(2) 0.4589(9) 0.049(4) Uani 1 1 d . . .
H21 H 0.9702 0.6552 0.5093 0.059 Uiso 1 1 calc R . .
C22 C 1.0976(18) 0.718(2) 0.4239(9) 0.053(4) Uani 1 1 d . . .
H22 H 1.1942 0.8018 0.4502 0.063 Uiso 1 1 calc R . .
C23 C 1.0744(18) 0.6680(18) 0.3491(8) 0.043(3) Uani 1 1 d . . .
H23 H 1.1597 0.7168 0.3242 0.052 Uiso 1 1 calc R . .
C24 C 0.9311(17) 0.5499(16) 0.3110(9) 0.043(3) Uani 1 1 d . . .
H24 H 0.9209 0.5195 0.2606 0.051 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'
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
N1 U N3 152.1(3) . . ?
N1 U N2 76.6(3) . . ?
N3 U N2 75.7(3) . . ?
N1 U I1 93.4(2) . . ?
N3 U I1 84.6(2) . . ?
N2 U I1 78.7(2) . . ?
N1 U I2 82.1(2) . . ?
N3 U I2 88.4(2) . . ?
N2 U I2 77.3(2) . . ?
I1 U I2 155.97(3) . . ?
C10 N1 C14 116.0(12) . . ?
C10 N1 U 124.1(8) . . ?
C14 N1 U 117.5(8) . . ?
C15 N2 C19 118.4(12) . . ?
C15 N2 U 119.8(8) . . ?
C19 N2 U 121.8(9) . . ?
C20 N3 C24 118.5(12) . . ?
C20 N3 U 123.2(9) . . ?
C24 N3 U 118.3(9) . . ?
C5 C1 C2 105.2(13) . . ?
C5 C1 C6 128.4(12) . . ?
C2 C1 C6 125.8(12) . . ?
C3 C2 C1 109.8(13) . . ?
C2 C3 C4 109.7(13) . . ?
C5 C4 C3 101.4(11) . . ?
C1 C5 C4 113.8(12) . . ?
C9 C6 C7 110.5(13) . . ?
C9 C6 C1 110.4(11) . . ?
C7 C6 C1 112.1(12) . . ?
C9 C6 C8 108.8(12) . . ?
C7 C6 C8 107.5(13) . . ?
C1 C6 C8 107.5(12) . . ?
N1 C10 C11 122.6(13) . . ?
C12 C11 C10 119.6(13) . . ?
C11 C12 C13 119.1(13) . . ?
C14 C13 C12 117.2(14) . . ?
N1 C14 C13 125.5(14) . . ?
N2 C15 C16 121.8(12) . . ?
C17 C16 C15 118.1(13) . . ?
C16 C17 C18 120.7(13) . . ?
C19 C18 C17 117.0(12) . . ?
N2 C19 C18 123.8(12) . . ?
N3 C20 C21 123.9(13) . . ?
C20 C21 C22 118.0(14) . . ?
C23 C22 C21 115.8(13) . . ?
C24 C23 C22 121.8(14) . . ?
N3 C24 C23 121.9(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U N1 2.607(10) . ?
U N3 2.641(11) . ?
U N2 2.724(11) . ?
U C3 2.732(14) . ?
U C2 2.757(14) . ?
U C4 2.818(11) . ?
U C5 2.822(12) . ?
U C1 2.873(14) . ?
U I1 3.1466(11) . ?
U I2 3.1912(11) . ?
N1 C10 1.347(16) . ?
N1 C14 1.349(17) . ?
N2 C15 1.328(17) . ?
N2 C19 1.357(16) . ?
N3 C20 1.319(17) . ?
N3 C24 1.350(17) . ?
C1 C5 1.412(18) . ?
C1 C2 1.434(18) . ?
C1 C6 1.53(2) . ?
C2 C3 1.42(2) . ?
C3 C4 1.492(18) . ?
C4 C5 1.465(19) . ?
C6 C9 1.50(2) . ?
C6 C7 1.496(19) . ?
C6 C8 1.54(2) . ?
C10 C11 1.404(19) . ?
C11 C12 1.37(2) . ?
C12 C13 1.40(2) . ?
C13 C14 1.380(19) . ?
C15 C16 1.42(2) . ?
C16 C17 1.38(2) . ?
C17 C18 1.390(18) . ?
C18 C19 1.387(17) . ?
C20 C21 1.37(2) . ?
C21 C22 1.45(2) . ?
C22 C23 1.38(2) . ?
C23 C24 1.352(19) . ?
