#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008206.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_7008206
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 Ce I2 N3'
_chemical_formula_weight         752.41
_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                102.444(4)
_cell_angle_beta                 93.809(5)
_cell_angle_gamma                108.371(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4213(4)
_cell_length_b                   8.8376(7)
_cell_length_c                   19.0845(15)
_cell_measurement_reflns_used    9001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.21
_cell_volume                     1302.39(16)
_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 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_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            9001
_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    4.133
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.374
_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    1.919
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0342
_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)+1.5087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                3820
_reflns_number_total             4559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419088b.txt
_cod_data_source_block           3
_cod_database_code               7008206
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
Ce Ce 0.52270(4) 0.25973(4) 0.261703(18) 0.03434(10) Uani 1 1 d . . .
I1 I 0.77288(5) 0.14127(5) 0.16520(2) 0.04062(12) Uani 1 1 d . . .
I2 I 0.32973(5) 0.29904(5) 0.40025(2) 0.04566(12) Uani 1 1 d . . .
N1 N 0.2839(6) -0.0330(6) 0.2221(3) 0.0386(11) Uani 1 1 d . . .
N2 N 0.6316(6) 0.0798(6) 0.3416(3) 0.0409(11) Uani 1 1 d . . .
N3 N 0.8029(6) 0.4729(6) 0.3432(3) 0.0395(11) Uani 1 1 d . . .
C1 C 0.3953(7) 0.3449(7) 0.1370(3) 0.0364(12) Uani 1 1 d . . .
C2 C 0.2890(8) 0.3575(8) 0.1910(3) 0.0415(13) Uani 1 1 d . . .
H2 H 0.1781 0.2883 0.1875 0.050 Uiso 1 1 calc R . .
C3 C 0.3749(8) 0.4881(8) 0.2499(3) 0.0422(14) Uani 1 1 d . . .
H3 H 0.3303 0.5209 0.2914 0.051 Uiso 1 1 calc R . .
C4 C 0.5442(7) 0.5649(7) 0.2364(3) 0.0360(12) Uani 1 1 d . . .
H4 H 0.6285 0.6560 0.2662 0.043 Uiso 1 1 calc R . .
C5 C 0.5536(7) 0.4696(7) 0.1668(3) 0.0390(13) Uani 1 1 d . . .
H5 H 0.6501 0.4869 0.1442 0.047 Uiso 1 1 calc R . .
C6 C 0.3454(8) 0.2348(8) 0.0603(3) 0.0427(14) Uani 1 1 d . . .
C7 C 0.2774(9) 0.0507(7) 0.0590(4) 0.0469(15) Uani 1 1 d . . .
H7A H 0.3651 0.0206 0.0809 0.070 Uiso 1 1 calc R . .
H7B H 0.2413 -0.0134 0.0097 0.070 Uiso 1 1 calc R . .
H7C H 0.1832 0.0302 0.0856 0.070 Uiso 1 1 calc R . .
C8 C 0.2028(8) 0.2751(8) 0.0213(4) 0.0482(15) Uani 1 1 d . . .
H8A H 0.1102 0.2622 0.0489 0.072 Uiso 1 1 calc R . .
H8B H 0.1647 0.2015 -0.0261 0.072 Uiso 1 1 calc R . .
H8C H 0.2449 0.3866 0.0170 0.072 Uiso 1 1 calc R . .
C9 C 0.4941(8) 0.2642(8) 0.0161(3) 0.0463(15) Uani 1 1 d . . .
H9A H 0.5384 0.3788 0.0167 0.069 Uiso 1 1 calc R . .
H9B H 0.4552 0.2000 -0.0331 0.069 Uiso 1 1 calc R . .
H9C H 0.5813 0.2320 0.0371 0.069 Uiso 1 1 calc R . .
C10 C 0.1173(8) -0.0549(8) 0.2171(3) 0.0413(13) Uani 1 1 d . . .
H10 H 0.0839 0.0321 0.2396 0.050 Uiso 1 1 calc R . .
C11 C -0.0059(8) -0.2008(7) 0.1801(3) 0.0423(14) Uani 1 1 d . . .
H11 H -0.1198 -0.2124 0.1786 0.051 Uiso 1 1 calc R . .
C12 C 0.0429(8) -0.3284(8) 0.1456(4) 0.0449(14) Uani 1 1 d . . .
H12 H -0.0382 -0.4268 0.1195 0.054 Uiso 1 1 calc R . .
C13 C 0.2131(8) -0.3107(8) 0.1497(4) 0.0450(14) Uani 1 1 d . . .
H13 H 0.2486 -0.3961 0.1272 0.054 Uiso 1 1 calc R . .
C14 C 0.3285(8) -0.1602(7) 0.1889(3) 0.0406(13) Uani 1 1 d . . .
H14 H 0.4430 -0.1470 0.1922 0.049 Uiso 1 1 calc R . .
C15 C 0.5244(8) -0.0237(8) 0.3732(3) 0.0423(14) Uani 1 1 d . . .
H15 H 0.4112 -0.0321 0.3671 0.051 Uiso 1 1 calc R . .
C16 C 0.5695(8) -0.1178(8) 0.4138(3) 0.0436(14) Uani 1 1 d . . .
H16 H 0.4894 -0.1888 0.4338 0.052 Uiso 1 1 calc R . .
C17 C 0.7395(8) -0.1038(7) 0.4243(4) 0.0439(14) Uani 1 1 d . . .
H17 H 0.7752 -0.1652 0.4517 0.053 Uiso 1 1 calc R . .
C18 C 0.8545(8) 0.0029(8) 0.3931(4) 0.0436(14) Uani 1 1 d . . .
H18 H 0.9685 0.0144 0.3988 0.052 Uiso 1 1 calc R . .
C19 C 0.7941(8) 0.0921(7) 0.3530(3) 0.0415(13) Uani 1 1 d . . .
H19 H 0.8715 0.1651 0.3328 0.050 Uiso 1 1 calc R . .
C20 C 0.8219(8) 0.5172(8) 0.4163(3) 0.0415(13) Uani 1 1 d . . .
H20 H 0.7347 0.4665 0.4398 0.050 Uiso 1 1 calc R . .
C21 C 0.9684(8) 0.6370(8) 0.4577(3) 0.0438(14) Uani 1 1 d . . .
H21 H 0.9796 0.6632 0.5081 0.053 Uiso 1 1 calc R . .
C22 C 1.0949(8) 0.7150(8) 0.4234(4) 0.0476(15) Uani 1 1 d . . .
H22 H 1.1926 0.7960 0.4500 0.057 Uiso 1 1 calc R . .
C23 C 1.0757(8) 0.6716(7) 0.3478(4) 0.0452(15) Uani 1 1 d . . .
H23 H 1.1599 0.7228 0.3230 0.054 Uiso 1 1 calc R . .
C24 C 0.9284(8) 0.5507(8) 0.3107(4) 0.0443(14) Uani 1 1 d . . .
H24 H 0.9157 0.5217 0.2603 0.053 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'
Ce Ce -0.2486 2.6331 '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
N3 Ce N1 152.18(15) . . ?
N3 Ce N2 75.91(15) . . ?
N1 Ce N2 76.42(15) . . ?
N3 Ce I1 84.29(11) . . ?
N1 Ce I1 92.87(11) . . ?
N2 Ce I1 78.25(11) . . ?
N3 Ce I2 88.62(11) . . ?
N1 Ce I2 82.77(11) . . ?
N2 Ce I2 77.69(11) . . ?
I1 Ce I2 155.911(16) . . ?
C14 N1 C10 117.3(5) . . ?
C14 N1 Ce 117.3(4) . . ?
C10 N1 Ce 123.4(4) . . ?
C19 N2 C15 116.1(5) . . ?
C19 N2 Ce 122.3(4) . . ?
C15 N2 Ce 121.6(4) . . ?
C24 N3 C20 117.7(5) . . ?
C24 N3 Ce 118.7(4) . . ?
C20 N3 Ce 123.5(4) . . ?
C2 C1 C5 105.5(5) . . ?
C2 C1 C6 127.3(5) . . ?
C5 C1 C6 126.9(5) . . ?
C3 C2 C1 110.0(6) . . ?
C2 C3 C4 109.3(5) . . ?
C5 C4 C3 104.6(5) . . ?
C1 C5 C4 110.6(5) . . ?
C1 C6 C7 112.5(5) . . ?
C1 C6 C9 112.0(5) . . ?
C7 C6 C9 108.5(5) . . ?
C1 C6 C8 108.5(5) . . ?
C7 C6 C8 107.5(5) . . ?
C9 C6 C8 107.7(5) . . ?
N1 C10 C11 122.9(6) . . ?
C12 C11 C10 118.7(6) . . ?
C11 C12 C13 120.0(6) . . ?
C12 C13 C14 117.4(6) . . ?
N1 C14 C13 123.6(6) . . ?
N2 C15 C16 124.8(6) . . ?
C15 C16 C17 117.9(6) . . ?
C18 C17 C16 119.1(6) . . ?
C17 C18 C19 118.0(6) . . ?
N2 C19 C18 124.2(6) . . ?
N3 C20 C21 122.1(6) . . ?
C22 C21 C20 119.2(6) . . ?
C21 C22 C23 119.2(6) . . ?
C24 C23 C22 118.2(6) . . ?
N3 C24 C23 123.6(6) . . ?
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
Ce N3 2.643(5) . ?
Ce N1 2.643(5) . ?
Ce C3 2.723(6) . ?
Ce N2 2.733(5) . ?
Ce C2 2.767(6) . ?
Ce C4 2.794(6) . ?
Ce C5 2.827(6) . ?
Ce C1 2.884(6) . ?
Ce I1 3.1625(5) . ?
Ce I2 3.2069(5) . ?
N1 C14 1.340(8) . ?
N1 C10 1.348(8) . ?
N2 C19 1.337(8) . ?
N2 C15 1.345(8) . ?
N3 C24 1.337(8) . ?
N3 C20 1.349(8) . ?
C1 C2 1.418(9) . ?
C1 C5 1.421(8) . ?
C1 C6 1.521(8) . ?
C2 C3 1.387(9) . ?
C3 C4 1.439(8) . ?
C4 C5 1.433(8) . ?
C6 C7 1.539(8) . ?
C6 C9 1.542(9) . ?
C6 C8 1.545(9) . ?
C10 C11 1.380(8) . ?
C11 C12 1.372(9) . ?
C12 C13 1.387(9) . ?
C13 C14 1.390(9) . ?
C15 C16 1.368(9) . ?
C16 C17 1.394(9) . ?
C17 C18 1.388(9) . ?
C18 C19 1.388(9) . ?
C20 C21 1.398(8) . ?
C21 C22 1.365(9) . ?
C22 C23 1.395(9) . ?
C23 C24 1.379(9) . ?
