#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008208.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_7008208
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 La N3'
_chemical_formula_weight         751.20
_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                102.588(3)
_cell_angle_beta                 93.636(3)
_cell_angle_gamma                108.458(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4495(4)
_cell_length_b                   8.8444(5)
_cell_length_c                   19.1107(10)
_cell_measurement_reflns_used    29806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.57
_cell_volume                     1308.53(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'one φ and five ω scans with 2° steps'
_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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       10
_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            29806
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    4.006
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0254
_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)+(0.0143P)²+0.8513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                4647
_reflns_number_total             4967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419088b.txt
_cod_data_source_block           5
_cod_database_code               7008208
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
La La 0.52261(2) 0.25945(2) 0.261183(9) 0.03521(7) Uani 1 1 d . . .
I1 I 0.77493(3) 0.14129(3) 0.164336(11) 0.04153(7) Uani 1 1 d . . .
I2 I 0.32947(3) 0.29918(3) 0.400828(12) 0.04623(8) Uani 1 1 d . . .
N1 N 0.2813(3) -0.0363(3) 0.22197(15) 0.0404(6) Uani 1 1 d . . .
N2 N 0.6326(4) 0.0784(4) 0.34190(15) 0.0438(6) Uani 1 1 d . . .
N3 N 0.8044(3) 0.4749(3) 0.34382(15) 0.0412(6) Uani 1 1 d . . .
C1 C 0.3966(4) 0.3467(4) 0.13662(17) 0.0372(7) Uani 1 1 d . . .
C2 C 0.2882(4) 0.3580(4) 0.18948(18) 0.0413(7) Uani 1 1 d . . .
H2 H 0.1774 0.2887 0.1856 0.050 Uiso 1 1 calc R . .
C3 C 0.3750(4) 0.4907(4) 0.24871(19) 0.0433(7) Uani 1 1 d . . .
H3 H 0.3312 0.5259 0.2902 0.052 Uiso 1 1 calc R . .
C4 C 0.5395(4) 0.5611(4) 0.23441(19) 0.0431(7) Uani 1 1 d . . .
H4 H 0.6244 0.6507 0.2647 0.052 Uiso 1 1 calc R . .
C5 C 0.5529(4) 0.4709(4) 0.16548(18) 0.0400(7) Uani 1 1 d . . .
H5 H 0.6491 0.4905 0.1429 0.048 Uiso 1 1 calc R . .
C6 C 0.3457(4) 0.2346(4) 0.05958(18) 0.0407(7) Uani 1 1 d . . .
C7 C 0.2790(5) 0.0519(4) 0.05981(19) 0.0499(9) Uani 1 1 d . . .
H7A H 0.3670 0.0233 0.0820 0.075 Uiso 1 1 calc R . .
H7B H 0.2428 -0.0143 0.0109 0.075 Uiso 1 1 calc R . .
H7C H 0.1856 0.0324 0.0867 0.075 Uiso 1 1 calc R . .
C8 C 0.2009(5) 0.2748(5) 0.02126(19) 0.0484(8) Uani 1 1 d . . .
H8A H 0.1091 0.2611 0.0492 0.073 Uiso 1 1 calc R . .
H8B H 0.1624 0.2016 -0.0262 0.073 Uiso 1 1 calc R . .
H8C H 0.2421 0.3865 0.0173 0.073 Uiso 1 1 calc R . .
C9 C 0.4931(5) 0.2642(5) 0.01607(18) 0.0472(8) Uani 1 1 d . . .
H9A H 0.5313 0.3770 0.0135 0.071 Uiso 1 1 calc R . .
H9B H 0.4572 0.1933 -0.0320 0.071 Uiso 1 1 calc R . .
H9C H 0.5836 0.2410 0.0394 0.071 Uiso 1 1 calc R . .
C10 C 0.1164(4) -0.0562(4) 0.21710(18) 0.0403(7) Uani 1 1 d . . .
H10 H 0.0841 0.0306 0.2406 0.048 Uiso 1 1 calc R . .
C11 C -0.0075(4) -0.2008(4) 0.17858(19) 0.0445(8) Uani 1 1 d . . .
H11 H -0.1208 -0.2108 0.1760 0.053 Uiso 1 1 calc R . .
C12 C 0.0413(5) -0.3302(4) 0.1439(2) 0.0471(8) Uani 1 1 d . . .
H12 H -0.0393 -0.4284 0.1174 0.056 Uiso 1 1 calc R . .
C13 C 0.2110(5) -0.3123(4) 0.14902(19) 0.0461(8) Uani 1 1 d . . .
H13 H 0.2464 -0.3980 0.1267 0.055 Uiso 1 1 calc R . .
C14 C 0.3262(4) -0.1632(4) 0.18828(19) 0.0435(8) Uani 1 1 d . . .
H14 H 0.4402 -0.1502 0.1915 0.052 Uiso 1 1 calc R . .
C15 C 0.5239(4) -0.0249(4) 0.37321(18) 0.0426(7) Uani 1 1 d . . .
H15 H 0.4111 -0.0333 0.3672 0.051 Uiso 1 1 calc R . .
C16 C 0.5714(4) -0.1198(5) 0.41408(19) 0.0454(8) Uani 1 1 d . . .
H16 H 0.4919 -0.1916 0.4339 0.055 Uiso 1 1 calc R . .
C17 C 0.7397(5) -0.1047(5) 0.42457(19) 0.0468(8) Uani 1 1 d . . .
H17 H 0.7760 -0.1645 0.4525 0.056 Uiso 1 1 calc R . .
C18 C 0.8528(4) 0.0007(4) 0.39285(19) 0.0439(8) Uani 1 1 d . . .
H18 H 0.9664 0.0118 0.3986 0.053 Uiso 1 1 calc R . .
C19 C 0.7949(4) 0.0897(4) 0.35230(18) 0.0426(7) Uani 1 1 d . . .
H19 H 0.8723 0.1606 0.3313 0.051 Uiso 1 1 calc R . .
C20 C 0.8245(4) 0.5184(4) 0.41698(18) 0.0424(7) Uani 1 1 d . . .
H20 H 0.7388 0.4661 0.4407 0.051 Uiso 1 1 calc R . .
C21 C 0.9681(4) 0.6380(5) 0.45765(19) 0.0458(8) Uani 1 1 d . . .
H21 H 0.9786 0.6652 0.5080 0.055 Uiso 1 1 calc R . .
C22 C 1.0965(4) 0.7171(5) 0.4230(2) 0.0475(8) Uani 1 1 d . . .
H22 H 1.1940 0.7982 0.4496 0.057 Uiso 1 1 calc R . .
C23 C 1.0769(4) 0.6730(4) 0.3485(2) 0.0449(8) Uani 1 1 d . . .
H23 H 1.1609 0.7240 0.3237 0.054 Uiso 1 1 calc R . .
C24 C 0.9303(4) 0.5517(4) 0.31118(19) 0.0434(7) Uani 1 1 d . . .
H24 H 0.9184 0.5218 0.2609 0.052 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'
La La -0.2871 2.4523 '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 La N1 151.88(8) . . ?
N3 La N2 75.67(8) . . ?
N1 La N2 76.41(8) . . ?
N3 La I1 84.21(6) . . ?
N1 La I1 93.37(6) . . ?
N2 La I1 78.24(6) . . ?
N3 La I2 88.34(6) . . ?
N1 La I2 82.47(6) . . ?
N2 La I2 77.56(6) . . ?
I1 La I2 155.748(9) . . ?
C10 N1 C14 118.0(3) . . ?
C10 N1 La 122.8(2) . . ?
C14 N1 La 116.8(2) . . ?
C19 N2 C15 117.0(3) . . ?
C19 N2 La 122.2(2) . . ?
C15 N2 La 120.8(2) . . ?
C24 N3 C20 117.6(3) . . ?
C24 N3 La 118.4(2) . . ?
C20 N3 La 123.9(2) . . ?
C5 C1 C2 106.7(3) . . ?
C5 C1 C6 126.9(3) . . ?
C2 C1 C6 126.0(3) . . ?
C3 C2 C1 108.9(3) . . ?
C2 C3 C4 108.0(3) . . ?
C3 C4 C5 107.5(3) . . ?
C1 C5 C4 108.8(3) . . ?
C9 C6 C1 111.4(3) . . ?
C9 C6 C7 109.1(3) . . ?
C1 C6 C7 111.7(3) . . ?
C9 C6 C8 108.6(3) . . ?
C1 C6 C8 108.0(3) . . ?
C7 C6 C8 107.9(3) . . ?
N1 C10 C11 122.7(3) . . ?
C10 C11 C12 118.4(3) . . ?
C13 C12 C11 119.6(3) . . ?
C14 C13 C12 118.0(3) . . ?
N1 C14 C13 123.2(3) . . ?
N2 C15 C16 123.5(3) . . ?
C17 C16 C15 118.4(3) . . ?
C18 C17 C16 118.9(3) . . ?
C17 C18 C19 119.1(3) . . ?
N2 C19 C18 123.1(3) . . ?
N3 C20 C21 122.1(3) . . ?
C20 C21 C22 119.5(3) . . ?
C23 C22 C21 118.6(3) . . ?
C22 C23 C24 118.8(3) . . ?
N3 C24 C23 123.3(3) . . ?
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
La N3 2.671(3) . ?
La N1 2.671(3) . ?
La C3 2.755(3) . ?
La N2 2.765(3) . ?
La C4 2.786(3) . ?
La C2 2.798(3) . ?
La C5 2.856(3) . ?
La C1 2.898(3) . ?
La I1 3.1830(3) . ?
La I2 3.2273(3) . ?
N1 C10 1.342(4) . ?
N1 C14 1.343(4) . ?
N2 C19 1.342(4) . ?
N2 C15 1.346(4) . ?
N3 C24 1.339(4) . ?
N3 C20 1.351(4) . ?
C1 C5 1.407(4) . ?
C1 C2 1.414(5) . ?
C1 C6 1.533(5) . ?
C2 C3 1.403(5) . ?
C3 C4 1.404(5) . ?
C4 C5 1.415(5) . ?
C6 C9 1.527(5) . ?
C6 C7 1.535(5) . ?
C6 C8 1.560(5) . ?
C10 C11 1.385(5) . ?
C11 C12 1.386(5) . ?
C12 C13 1.387(5) . ?
C13 C14 1.383(5) . ?
C15 C16 1.391(5) . ?
C16 C17 1.383(5) . ?
C17 C18 1.381(5) . ?
C18 C19 1.386(5) . ?
C20 C21 1.380(5) . ?
C21 C22 1.384(5) . ?
C22 C23 1.377(5) . ?
C23 C24 1.381(5) . ?
