#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:43:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179259 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/79/4317908.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_4317908
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 La N9'
_chemical_formula_weight         895.06
_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                111.7590(10)
_cell_angle_beta                 92.4440(10)
_cell_angle_gamma                108.9560(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8436(6)
_cell_length_b                   12.2206(8)
_cell_length_c                   14.3700(10)
_cell_measurement_temperature    193(2)
_cell_volume                     1492.01(17)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9731
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    4.557
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.480
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0452
_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)+(0.0898P)²+2.7474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                5957
_reflns_number_total             6867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010839v_1.cif
_cod_data_source_block           complex1
_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_database_code               4317908
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 0.34792(3) 0.11736(3) -0.21870(2) 0.02382(10) Uani 1 1 d . . .
I1 I 0.42578(4) 0.25411(4) 0.02762(3) 0.03480(12) Uani 1 1 d . . .
I2 I 0.32963(5) 0.18183(6) -0.41765(4) 0.04850(15) Uani 1 1 d . . .
I3 I 0.60241(5) 0.01436(5) -0.21951(4) 0.04506(14) Uani 1 1 d . . .
N1 N 0.2116(5) -0.0542(5) -0.1422(4) 0.0267(9) Uani 1 1 d . . .
N2 N 0.2363(6) -0.1002(6) -0.3873(4) 0.0384(12) Uani 1 1 d . . .
N3 N 0.1996(6) 0.2749(5) -0.1747(4) 0.0345(11) Uani 1 1 d . . .
N4 N 0.0519(5) 0.0075(4) -0.2670(3) 0.0236(9) Uani 1 1 d . . .
N5 N 0.0567(6) -0.2064(5) -0.0477(4) 0.0362(11) Uani 1 1 d . . .
N6 N 0.1188(7) -0.2767(7) -0.5895(4) 0.0497(16) Uani 1 1 d . . .
N7 N 0.0203(8) 0.4179(7) -0.1193(5) 0.0529(16) Uani 1 1 d . . .
C1 C 0.0030(6) 0.0020(6) -0.1715(4) 0.0282(11) Uani 1 1 d . . .
H1A H -0.1026 -0.0389 -0.1845 0.034 Uiso 1 1 calc R . .
H1B H 0.0296 0.0873 -0.1197 0.034 Uiso 1 1 calc R . .
C2 C 0.0721(6) -0.0702(5) -0.1336(4) 0.0250(10) Uani 1 1 d . . .
C3 C -0.0038(7) -0.1461(6) -0.0867(5) 0.0303(12) Uani 1 1 d . . .
H3 H -0.1006 -0.1552 -0.0824 0.036 Uiso 1 1 calc R . .
C4 C 0.1959(8) -0.1871(6) -0.0548(5) 0.0361(13) Uani 1 1 d . . .
H4 H 0.2439 -0.2247 -0.0263 0.043 Uiso 1 1 calc R . .
C5 C 0.2732(7) -0.1130(6) -0.1030(5) 0.0320(12) Uani 1 1 d . . .
H5 H 0.3696 -0.1047 -0.1078 0.038 Uiso 1 1 calc R . .
C6 C -0.0080(6) -0.1224(6) -0.3486(4) 0.0285(11) Uani 1 1 d . . .
H6A H -0.0996 -0.1342 -0.3861 0.034 Uiso 1 1 calc R . .
H6B H -0.0291 -0.1826 -0.3173 0.034 Uiso 1 1 calc R . .
C7 C 0.0922(6) -0.1519(6) -0.4229(4) 0.0276(11) Uani 1 1 d . . .
C8 C 0.0337(8) -0.2386(6) -0.5234(5) 0.0359(13) Uani 1 1 d . . .
H8 H -0.0670 -0.2712 -0.5455 0.043 Uiso 1 1 calc R . .
C9 C 0.2599(9) -0.2253(8) -0.5540(6) 0.0518(19) Uani 1 1 d . . .
H9 H 0.3229 -0.2470 -0.5977 0.062 Uiso 1 1 calc R . .
C10 C 0.3193(8) -0.1391(8) -0.4528(6) 0.051(2) Uani 1 1 d . . .
H10 H 0.4199 -0.1082 -0.4306 0.061 Uiso 1 1 calc R . .
C11 C -0.0055(6) 0.0906(6) -0.2965(4) 0.0275(11) Uani 1 1 d . . .
H11A H -0.1113 0.0590 -0.3047 0.033 Uiso 1 1 calc R . .
H11B H 0.0197 0.0890 -0.3614 0.033 Uiso 1 1 calc R . .
C12 C 0.0568(7) 0.2247(6) -0.2171(4) 0.0299(12) Uani 1 1 d . . .
C13 C -0.0306(8) 0.2980(7) -0.1873(5) 0.0390(14) Uani 1 1 d . . .
H13 H -0.1294 0.2608 -0.2166 0.047 Uiso 1 1 calc R . .
C14 C 0.1635(10) 0.4664(7) -0.0804(6) 0.053(2) Uani 1 1 d . . .
H14 H 0.2047 0.5506 -0.0340 0.064 Uiso 1 1 calc R . .
C15 C 0.2529(8) 0.3969(6) -0.1061(6) 0.0442(16) Uani 1 1 d . . .
H15 H 0.3512 0.4347 -0.0758 0.053 Uiso 1 1 calc R . .
N11 N 0.5705(7) 0.3323(6) -0.1801(5) 0.0467(14) Uani 1 1 d . . .
C21 C 0.6600(7) 0.4159(6) -0.1833(5) 0.0373(14) Uani 1 1 d . . .
C22 C 0.7766(9) 0.5221(7) -0.1879(7) 0.0523(19) Uani 1 1 d . . .
N12 N -0.039(3) -0.6216(17) -0.6694(15) 0.154(7) Uani 1 1 d . . .
C23 C -0.132(3) -0.5920(15) -0.6828(13) 0.116(6) Uani 1 1 d . . .
C24 C -0.238(4) -0.550(3) -0.700(2) 0.226(15) Uani 1 1 d . . .
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
N11 La N3 81.57(19) . . ?
N11 La N2 131.50(19) . . ?
N3 La N2 117.90(16) . . ?
N11 La N4 142.96(18) . . ?
N3 La N4 63.49(15) . . ?
N2 La N4 63.72(15) . . ?
N11 La N1 144.65(17) . . ?
N3 La N1 103.63(15) . . ?
N2 La N1 77.46(17) . . ?
N4 La N1 61.76(14) . . ?
N11 La I3 82.15(15) . . ?
N3 La I3 161.24(12) . . ?
N2 La I3 80.13(11) . . ?
N4 La I3 134.21(10) . . ?
N1 La I3 84.59(10) . . ?
N11 La I1 76.22(14) . . ?
N3 La I1 77.18(11) . . ?
N2 La I1 147.82(13) . . ?
N4 La I1 105.62(10) . . ?
N1 La I1 71.14(10) . . ?
I3 La I1 89.944(14) . . ?
N11 La I2 72.66(14) . . ?
N3 La I2 75.82(11) . . ?
N2 La I2 70.67(13) . . ?
N4 La I2 86.51(10) . . ?
N1 La I2 142.68(10) . . ?
I3 La I2 107.952(15) . . ?
I1 La I2 141.170(17) . . ?
C5 N1 C2 116.9(5) . . ?
C5 N1 La 126.5(4) . . ?
C2 N1 La 116.2(3) . . ?
C10 N2 C7 116.0(6) . . ?
C10 N2 La 121.5(5) . . ?
C7 N2 La 119.7(4) . . ?
C12 N3 C15 117.2(6) . . ?
C12 N3 La 117.2(4) . . ?
C15 N3 La 125.3(4) . . ?
C6 N4 C11 109.3(4) . . ?
C6 N4 C1 108.2(4) . . ?
C11 N4 C1 109.4(4) . . ?
C6 N4 La 115.8(3) . . ?
C11 N4 La 108.4(3) . . ?
C1 N4 La 105.6(3) . . ?
C4 N5 C3 115.5(5) . . ?
C9 N6 C8 116.0(6) . . ?
C13 N7 C14 115.4(6) . . ?
N4 C1 C2 110.7(4) . . ?
N1 C2 C3 121.1(5) . . ?
N1 C2 C1 117.8(5) . . ?
C3 C2 C1 121.0(5) . . ?
N5 C3 C2 122.5(6) . . ?
N5 C4 C5 122.8(6) . . ?
N1 C5 C4 121.1(6) . . ?
N4 C6 C7 114.3(5) . . ?
N2 C7 C8 121.7(6) . . ?
N2 C7 C6 118.1(5) . . ?
C8 C7 C6 120.0(5) . . ?
N6 C8 C7 121.9(6) . . ?
N6 C9 C10 122.4(6) . . ?
N2 C10 C9 121.9(7) . . ?
N4 C11 C12 111.0(5) . . ?
N3 C12 C13 119.8(6) . . ?
N3 C12 C11 118.8(5) . . ?
C13 C12 C11 121.4(6) . . ?
N7 C13 C12 123.5(7) . . ?
N7 C14 C15 122.9(7) . . ?
N3 C15 C14 121.1(7) . . ?
C21 N11 La 166.9(6) . . ?
N11 C21 C22 179.1(8) . . ?
N12 C23 C24 176(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 N11 2.662(6) . ?
La N3 2.691(5) . ?
La N2 2.692(6) . ?
La N4 2.715(4) . ?
La N1 2.723(5) . ?
La I3 3.1465(5) . ?
La I1 3.2342(5) . ?
La I2 3.2472(5) . ?
N1 C5 1.324(8) . ?
N1 C2 1.341(7) . ?
N2 C10 1.329(8) . ?
N2 C7 1.337(8) . ?
N3 C12 1.347(8) . ?
N3 C15 1.352(9) . ?
N4 C6 1.482(7) . ?
N4 C11 1.485(7) . ?
N4 C1 1.491(7) . ?
N5 C4 1.328(9) . ?
N5 C3 1.333(8) . ?
N6 C9 1.312(10) . ?
N6 C8 1.346(9) . ?
N7 C13 1.331(10) . ?
N7 C14 1.340(11) . ?
C1 C2 1.500(8) . ?
C2 C3 1.389(8) . ?
C4 C5 1.394(9) . ?
C6 C7 1.509(8) . ?
C7 C8 1.392(8) . ?
C9 C10 1.399(10) . ?
C11 C12 1.506(8) . ?
C12 C13 1.404(9) . ?
C14 C15 1.383(10) . ?
N11 C21 1.130(9) . ?
C21 C22 1.452(10) . ?
N12 C23 1.13(3) . ?
C23 C24 1.35(3) . ?
