#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:43:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179259 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/79/4317909.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_4317909
loop_
_publ_author_name
'Marinella Mazzanti'
'Raphaël Wietzke'
'Jacques Pécaut'
'Jean-Marc Latour'
'Pascale Maldivi'
'Michael Remy'
_publ_section_title
;
 Structural and Density Functional Studies of Uranium(III) and
 Lanthanum(III) Complexes with a Neutral Tripodal N-Donor Ligand
 Suggesting the Presence of a U-N Back-Bonding Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2389
_journal_page_last               2399
_journal_paper_doi               10.1021/ic010839v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C19 H21 I3 N9 U'
_chemical_formula_weight         994.18
_chemical_name_systematic
;
?
;
_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                111.41(3)
_cell_angle_beta                 92.07(3)
_cell_angle_gamma                109.17(3)
_cell_formula_units_Z            2
_cell_length_a                   9.950(2)
_cell_length_b                   12.190(2)
_cell_length_c                   14.440(3)
_cell_measurement_temperature    143(2)
_cell_volume                     1515.7(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.858
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9538
_diffrn_reflns_theta_full        28.65
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    8.431
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    2.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.4
_refine_diff_density_max         3.084
_refine_diff_density_min         -4.701
_refine_diff_density_rms         0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0572
_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)+(0.1086P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                5294
_reflns_number_total             6711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010839v_2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1515.7(5)
_cod_database_code               4317909
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 0.34536(3) 0.11666(3) -0.22252(3) 0.01918(12) Uani 1 1 d . . .
I1 I 0.41836(7) 0.24947(6) 0.02203(5) 0.02609(17) Uani 1 1 d . . .
I2 I 0.32649(7) 0.18402(8) -0.42042(5) 0.03338(19) Uani 1 1 d . . .
I3 I 0.60062(7) 0.01582(8) -0.22315(6) 0.03329(19) Uani 1 1 d . . .
N1 N 0.2141(8) -0.0569(8) -0.1454(6) 0.0233(17) Uani 1 1 d . . .
N2 N 0.2387(8) -0.1000(8) -0.3887(6) 0.0249(18) Uani 1 1 d . . .
N3 N 0.2019(9) 0.2749(8) -0.1785(7) 0.0263(18) Uani 1 1 d . . .
N4 N 0.0519(8) 0.0058(7) -0.2685(6) 0.0209(16) Uani 1 1 d . . .
N5 N 0.0643(10) -0.2065(8) -0.0433(7) 0.0290(19) Uani 1 1 d . . .
N6 N 0.1252(11) -0.2770(10) -0.5923(7) 0.039(2) Uani 1 1 d . . .
N7 N 0.0241(12) 0.4220(10) -0.1213(8) 0.042(2) Uani 1 1 d . . .
C1 C 0.0020(10) -0.0021(10) -0.1732(8) 0.025(2) Uani 1 1 d . . .
H1A H -0.1019 -0.0463 -0.1868 0.030 Uiso 1 1 calc R . .
H1B H 0.0243 0.0827 -0.1223 0.030 Uiso 1 1 calc R . .
C2 C 0.0752(10) -0.0715(9) -0.1334(8) 0.0221(19) Uani 1 1 d . . .
C3 C -0.0013(11) -0.1493(10) -0.0835(8) 0.028(2) Uani 1 1 d . . .
H3 H -0.0975 -0.1604 -0.0789 0.033 Uiso 1 1 calc R . .
C4 C 0.2044(11) -0.1869(10) -0.0523(8) 0.029(2) Uani 1 1 d . . .
H4 H 0.2538 -0.2224 -0.0230 0.035 Uiso 1 1 calc R . .
C5 C 0.2779(11) -0.1139(9) -0.1050(8) 0.027(2) Uani 1 1 d . . .
H5 H 0.3730 -0.1055 -0.1116 0.033 Uiso 1 1 calc R . .
C6 C -0.0072(10) -0.1266(9) -0.3508(7) 0.025(2) Uani 1 1 d . . .
H6A H -0.0982 -0.1390 -0.3875 0.030 Uiso 1 1 calc R . .
H6B H -0.0272 -0.1870 -0.3194 0.030 Uiso 1 1 calc R . .
C7 C 0.0931(10) -0.1553(9) -0.4260(7) 0.0216(19) Uani 1 1 d . . .
C8 C 0.0387(12) -0.2426(10) -0.5250(8) 0.030(2) Uani 1 1 d . . .
H8 H -0.0610 -0.2793 -0.5464 0.036 Uiso 1 1 calc R . .
C9 C 0.2655(12) -0.2247(13) -0.5580(10) 0.044(3) Uani 1 1 d . . .
H9 H 0.3280 -0.2459 -0.6016 0.053 Uiso 1 1 calc R . .
C10 C 0.3238(12) -0.1374(12) -0.4571(8) 0.036(3) Uani 1 1 d . . .
H10 H 0.4235 -0.1041 -0.4362 0.043 Uiso 1 1 calc R . .
C11 C -0.0050(10) 0.0910(10) -0.2986(8) 0.025(2) Uani 1 1 d . . .
H11A H -0.1095 0.0599 -0.3058 0.030 Uiso 1 1 calc R . .
H11B H 0.0197 0.0886 -0.3635 0.030 Uiso 1 1 calc R . .
C12 C 0.0585(11) 0.2281(9) -0.2198(7) 0.022(2) Uani 1 1 d . . .
C13 C -0.0286(12) 0.3004(11) -0.1887(9) 0.032(2) Uani 1 1 d . . .
H13 H -0.1268 0.2628 -0.2158 0.038 Uiso 1 1 calc R . .
C14 C 0.1688(14) 0.4717(12) -0.0825(10) 0.042(3) Uani 1 1 d . . .
H14 H 0.2112 0.5560 -0.0375 0.050 Uiso 1 1 calc R . .
C15 C 0.2545(13) 0.3965(10) -0.1098(9) 0.035(3) Uani 1 1 d . . .
H15 H 0.3513 0.4321 -0.0794 0.043 Uiso 1 1 calc R . .
N11 N 0.5611(11) 0.3280(10) -0.1857(7) 0.039(2) Uani 1 1 d . . .
C21 C 0.6590(12) 0.4173(10) -0.1846(9) 0.033(2) Uani 1 1 d . . .
C22 C 0.7799(14) 0.5250(13) -0.1901(12) 0.051(4) Uani 1 1 d . . .
N12 N -0.078(3) -0.621(2) -0.674(2) 0.066(8) Uani 0.50 1 d P . .
C23 C -0.172(4) -0.603(3) -0.677(3) 0.066(10) Uani 0.50 1 d P . .
C24 C -0.296(5) -0.576(4) -0.692(3) 0.108(17) Uani 0.50 1 d P . .
H24A H -0.3583 -0.5927 -0.6457 0.163 Uiso 0.50 1 calc PR . .
H24B H -0.3472 -0.6274 -0.7602 0.163 Uiso 0.50 1 calc PR . .
H24C H -0.2678 -0.4879 -0.6810 0.163 Uiso 0.50 1 calc PR . .
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
N11 U N3 81.0(3) . . ?
N11 U N2 131.2(3) . . ?
N3 U N2 118.9(3) . . ?
N11 U N4 143.2(3) . . ?
N3 U N4 64.1(2) . . ?
N2 U N4 64.4(2) . . ?
N11 U N1 144.1(3) . . ?
N3 U N1 104.9(2) . . ?
N2 U N1 77.5(3) . . ?
N4 U N1 62.3(2) . . ?
N11 U I3 81.6(2) . . ?
N3 U I3 160.23(18) . . ?
N2 U I3 79.96(18) . . ?
N4 U I3 134.60(17) . . ?
N1 U I3 84.00(17) . . ?
N11 U I1 76.8(2) . . ?
N3 U I1 77.09(19) . . ?
N2 U I1 147.18(19) . . ?
N4 U I1 104.81(17) . . ?
N1 U I1 70.39(18) . . ?
I3 U I1 89.82(4) . . ?
N11 U I2 72.7(2) . . ?
N3 U I2 75.27(18) . . ?
N2 U I2 71.01(19) . . ?
N4 U I2 86.63(17) . . ?
N1 U I2 143.15(17) . . ?
I3 U I2 108.28(3) . . ?
I1 U I2 141.44(3) . . ?
C5 N1 C2 117.0(8) . . ?
C5 N1 U 126.5(6) . . ?
C2 N1 U 115.7(6) . . ?
C7 N2 C10 114.6(9) . . ?
C7 N2 U 120.4(6) . . ?
C10 N2 U 121.7(7) . . ?
C15 N3 C12 115.6(9) . . ?
C15 N3 U 125.5(7) . . ?
C12 N3 U 118.6(6) . . ?
C1 N4 C11 110.2(7) . . ?
C1 N4 C6 107.7(7) . . ?
C11 N4 C6 109.6(7) . . ?
C1 N4 U 106.2(5) . . ?
C11 N4 U 107.8(5) . . ?
C6 N4 U 115.3(5) . . ?
C3 N5 C4 116.9(9) . . ?
C9 N6 C8 116.4(10) . . ?
C13 N7 C14 116.1(10) . . ?
N4 C1 C2 110.9(8) . . ?
N1 C2 C3 121.4(9) . . ?
N1 C2 C1 118.4(8) . . ?
C3 C2 C1 120.2(8) . . ?
N5 C3 C2 121.0(9) . . ?
N5 C4 C5 121.9(9) . . ?
N1 C5 C4 121.7(9) . . ?
N4 C6 C7 114.6(8) . . ?
N2 C7 C8 121.7(9) . . ?
N2 C7 C6 116.8(8) . . ?
C8 C7 C6 121.3(9) . . ?
N6 C8 C7 122.8(10) . . ?
N6 C9 C10 122.0(10) . . ?
N2 C10 C9 122.5(10) . . ?
N4 C11 C12 111.4(8) . . ?
N3 C12 C13 121.6(9) . . ?
N3 C12 C11 117.2(8) . . ?
C13 C12 C11 121.2(9) . . ?
N7 C13 C12 122.8(10) . . ?
N7 C14 C15 120.9(11) . . ?
N3 C15 C14 122.9(11) . . ?
C21 N11 U 169.9(9) . . ?
N11 C21 C22 176.5(13) . . ?
N12 C23 C24 172(5) . . ?
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 N11 2.610(10) . ?
U N3 2.672(8) . ?
U N2 2.685(8) . ?
U N4 2.721(8) . ?
U N1 2.726(8) . ?
U I3 3.1632(10) . ?
U I1 3.2383(14) . ?
U I2 3.2637(10) . ?
N1 C5 1.336(13) . ?
N1 C2 1.360(12) . ?
N2 C7 1.372(12) . ?
N2 C10 1.373(13) . ?
N3 C15 1.355(14) . ?
N3 C12 1.368(13) . ?
N4 C1 1.504(12) . ?
N4 C11 1.511(12) . ?
N4 C6 1.513(12) . ?
N5 C3 1.347(14) . ?
N5 C4 1.355(13) . ?
N6 C9 1.317(15) . ?
N6 C8 1.364(14) . ?
N7 C13 1.349(15) . ?
N7 C14 1.369(16) . ?
C1 C2 1.518(13) . ?
C2 C3 1.437(13) . ?
C4 C5 1.421(14) . ?
C6 C7 1.525(13) . ?
C7 C8 1.387(14) . ?
C9 C10 1.412(17) . ?
C11 C12 1.534(14) . ?
C12 C13 1.403(14) . ?
C14 C15 1.412(16) . ?
N11 C21 1.193(14) . ?
C21 C22 1.491(16) . ?
N12 C23 1.03(4) . ?
C23 C24 1.41(5) . ?
