#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/14/4311422.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_4311422
loop_
_publ_author_name
'Lydia Karmazin'
'Marinella Mazzanti'
'Jean-Philippe Bezombes'
'Christelle Gateau'
'Jacques Pécaut'
_publ_section_title
;
 Comparative Structural Studies of Iodide Complexes of Uranium(III) and
 Lanthanide(III) with Hexadentate Tetrapodal Neutral N-Donor Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5147
_journal_page_last               5158
_journal_paper_doi               10.1021/ic049538m
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C27 H31.5 I3 N10.5 U'
_chemical_formula_weight         1121.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   33.1530(12)
_cell_length_b                   33.1530(12)
_cell_length_c                   15.9643(8)
_cell_measurement_temperature    193(2)
_cell_volume                     15195.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14538
_diffrn_reflns_theta_full        28.85
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    7.584
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9324
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.975
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0522P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                3661
_reflns_number_total             4442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049538msi20040408_103455_12.cif
_cod_data_source_block           struc_U(tpzcn),11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_original_formula_sum        'C27 H31.50 I3 N10.50 U'
_cod_database_code               4311422
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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 0.849580(17) 0.560096(17) 0.16525(2) 0.02027(12) Uani 1 1 d . . .
I1 I 0.78321(4) 0.50612(4) 0.01474(6) 0.0414(3) Uani 1 1 d . . .
I2 I 0.89628(4) 0.64980(4) 0.04959(5) 0.0330(2) Uani 1 1 d . . .
I3 I 0.62012(4) 0.51927(4) 0.28441(6) 0.0389(3) Uani 1 1 d . . .
N1 N 0.8594(4) 0.5893(4) 0.3242(6) 0.023(2) Uani 1 1 d . . .
N2 N 0.8549(4) 0.5027(4) 0.2720(6) 0.023(2) Uani 1 1 d . . .
N3 N 0.9360(4) 0.6157(4) 0.2195(7) 0.023(2) Uani 1 1 d . . .
N4 N 0.8033(4) 0.5987(4) 0.2085(6) 0.025(2) Uani 1 1 d . . .
N5 N 0.8951(4) 0.5206(4) 0.1105(7) 0.029(3) Uani 1 1 d . . .
N6 N 0.7692(4) 0.4935(4) 0.2313(7) 0.028(3) Uani 1 1 d . . .
N7 N 1.0235(4) 0.6897(4) 0.2665(7) 0.032(3) Uani 1 1 d . . .
N8 N 0.7431(4) 0.6309(5) 0.2534(8) 0.035(3) Uani 1 1 d . . .
N9 N 0.9481(4) 0.4805(4) 0.0615(7) 0.033(3) Uani 1 1 d . . .
N10 N 0.6889(5) 0.4134(6) 0.2835(16) 0.082(7) Uani 1 1 d . . .
C1 C 0.8952(5) 0.6390(5) 0.3183(8) 0.024(3) Uani 1 1 d . . .
H1A H 0.9016 0.6530 0.3750 0.029 Uiso 1 1 calc R . .
H1B H 0.8832 0.6554 0.2834 0.029 Uiso 1 1 calc R . .
C2 C 0.9399(5) 0.6458(4) 0.2809(8) 0.022(3) Uani 1 1 d . . .
C3 C 0.9824(5) 0.6814(5) 0.3051(8) 0.031(3) Uani 1 1 d . . .
H3 H 0.9840 0.7010 0.3497 0.037 Uiso 1 1 calc R . .
C4 C 1.0173(5) 0.6592(5) 0.2076(8) 0.028(3) Uani 1 1 d . . .
H4 H 1.0441 0.6622 0.1803 0.034 Uiso 1 1 calc R . .
C5 C 0.9740(5) 0.6230(5) 0.1833(8) 0.029(3) Uani 1 1 d . . .
H5 H 0.9723 0.6031 0.1390 0.034 Uiso 1 1 calc R . .
C6 C 0.8164(4) 0.5867(5) 0.3543(8) 0.024(3) Uani 1 1 d . . .
H6A H 0.8235 0.6067 0.4045 0.028 Uiso 1 1 calc R . .
H6B H 0.7942 0.5542 0.3713 0.028 Uiso 1 1 calc R . .
C7 C 0.7934(5) 0.6019(5) 0.2893(8) 0.026(3) Uani 1 1 d . . .
C8 C 0.7639(5) 0.6179(5) 0.3105(9) 0.033(3) Uani 1 1 d . . .
H8 H 0.7580 0.6199 0.3682 0.039 Uiso 1 1 calc R . .
C9 C 0.7526(5) 0.6292(5) 0.1746(8) 0.031(3) Uani 1 1 d . . .
H9 H 0.7389 0.6389 0.1327 0.037 Uiso 1 1 calc R . .
C10 C 0.7834(5) 0.6129(5) 0.1511(8) 0.030(3) Uani 1 1 d . . .
H10 H 0.7900 0.6120 0.0934 0.036 Uiso 1 1 calc R . .
C11 C 0.8998(5) 0.5027(5) 0.2587(8) 0.028(3) Uani 1 1 d . . .
H11A H 0.8980 0.4754 0.2875 0.033 Uiso 1 1 calc R . .
H11B H 0.9256 0.5311 0.2840 0.033 Uiso 1 1 calc R . .
C12 C 0.9101(5) 0.5010(5) 0.1670(8) 0.025(3) Uani 1 1 d . . .
C13 C 0.9366(5) 0.4815(5) 0.1419(9) 0.030(3) Uani 1 1 d . . .
H13 H 0.9471 0.4683 0.1833 0.035 Uiso 1 1 calc R . .
C14 C 0.9322(5) 0.4987(6) 0.0077(9) 0.035(4) Uani 1 1 d . . .
H14 H 0.9388 0.4978 -0.0499 0.042 Uiso 1 1 calc R . .
C15 C 0.9064(6) 0.5189(5) 0.0289(8) 0.034(4) Uani 1 1 d . . .
H15 H 0.8963 0.5319 -0.0136 0.041 Uiso 1 1 calc R . .
C16 C 0.8151(5) 0.4558(5) 0.2470(9) 0.033(3) Uani 1 1 d . . .
H16A H 0.8143 0.4315 0.2840 0.039 Uiso 1 1 calc R . .
H16B H 0.8196 0.4487 0.1887 0.039 Uiso 1 1 calc R . .
C17 C 0.7692(5) 0.4555(5) 0.2537(9) 0.032(3) Uani 1 1 d . . .
C18 C 0.7289(6) 0.4151(6) 0.2795(15) 0.058(5) Uani 1 1 d . . .
H18 H 0.7309 0.3884 0.2944 0.070 Uiso 1 1 calc R . .
C19 C 0.6890(6) 0.4522(7) 0.2664(16) 0.069(6) Uani 1 1 d . . .
H19 H 0.6616 0.4539 0.2756 0.082 Uiso 1 1 calc R . .
C20 C 0.7285(5) 0.4906(5) 0.2352(11) 0.040(4) Uani 1 1 d . . .
H20 H 0.7258 0.5162 0.2157 0.049 Uiso 1 1 calc R . .
C21 C 0.8751(5) 0.5634(4) 0.3822(7) 0.020(3) Uani 1 1 d . . .
H21 H 0.9087 0.5750 0.3695 0.024 Uiso 1 1 calc R . .
C22 C 0.8492(6) 0.5118(5) 0.3647(7) 0.030(3) Uani 1 1 d . . .
H22 H 0.8154 0.5001 0.3747 0.036 Uiso 1 1 calc R . .
C23 C 0.8644(6) 0.4863(6) 0.4249(8) 0.033(3) Uani 1 1 d . . .
H23A H 0.8978 0.4970 0.4157 0.039 Uiso 1 1 calc R . .
H23B H 0.8465 0.4524 0.4128 0.039 Uiso 1 1 calc R . .
C24 C 0.8570(6) 0.4945(5) 0.5163(9) 0.036(4) Uani 1 1 d . . .
H24A H 0.8238 0.4841 0.5265 0.043 Uiso 1 1 calc R . .
H24B H 0.8662 0.4766 0.5537 0.043 Uiso 1 1 calc R . .
C25 C 0.8866(6) 0.5458(6) 0.5335(8) 0.038(4) Uani 1 1 d . . .
H25A H 0.9198 0.5558 0.5241 0.045 Uiso 1 1 calc R . .
H25B H 0.8828 0.5523 0.5926 0.045 Uiso 1 1 calc R . .
C26 C 0.8722(6) 0.5733(6) 0.4755(8) 0.030(3) Uani 1 1 d . . .
H26A H 0.8926 0.6070 0.4862 0.036 Uiso 1 1 calc R . .
H26B H 0.8398 0.5651 0.4889 0.036 Uiso 1 1 calc R . .
C101 C 0.752(4) 0.383(2) 0.538(9) 0.17(6) Uani 0.50 1 d P . .
N101 N 0.744(5) 0.376(3) 0.595(5) 0.20(5) Uani 0.50 1 d P . .
C102 C 0.747(3) 0.384(2) 0.459(4) 0.13(3) Uani 0.50 1 d P . .
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
N4 U N5 176.1(4) . . ?
N4 U N2 117.8(3) . . ?
N5 U N2 65.5(4) . . ?
N4 U N3 106.0(3) . . ?
N5 U N3 76.3(4) . . ?
N2 U N3 81.5(3) . . ?
N4 U N1 63.5(3) . . ?
N5 U N1 120.4(3) . . ?
N2 U N1 66.9(3) . . ?
N3 U N1 63.1(3) . . ?
N4 U N6 72.9(4) . . ?
N5 U N6 107.8(4) . . ?
N2 U N6 63.1(4) . . ?
N3 U N6 136.4(3) . . ?
N1 U N6 79.4(3) . . ?
N4 U I1 93.9(2) . . ?
N5 U I1 82.7(3) . . ?
N2 U I1 111.4(2) . . ?
N3 U I1 148.0(2) . . ?
N1 U I1 148.7(2) . . ?
N6 U I1 73.0(2) . . ?
N4 U I2 79.6(2) . . ?
N5 U I2 98.2(3) . . ?
N2 U I2 151.6(2) . . ?
N3 U I2 71.8(2) . . ?
N1 U I2 107.4(2) . . ?
N6 U I2 145.0(2) . . ?
I1 U I2 87.90(3) . . ?
C6 N1 C1 107.6(10) . . ?
C6 N1 C21 111.5(9) . . ?
C1 N1 C21 110.9(10) . . ?
C6 N1 U 110.6(7) . . ?
C1 N1 U 103.2(7) . . ?
C21 N1 U 112.8(7) . . ?
C11 N2 C16 108.7(10) . . ?
C11 N2 C22 110.9(10) . . ?
C16 N2 C22 109.0(11) . . ?
C11 N2 U 109.5(8) . . ?
C16 N2 U 103.5(7) . . ?
C22 N2 U 114.9(7) . . ?
C5 N3 C2 117.3(12) . . ?
C5 N3 U 126.6(9) . . ?
C2 N3 U 114.7(8) . . ?
C10 N4 C7 116.4(12) . . ?
C10 N4 U 121.1(8) . . ?
C7 N4 U 122.1(9) . . ?
C12 N5 C15 116.3(12) . . ?
C12 N5 U 117.9(8) . . ?
C15 N5 U 125.7(10) . . ?
C20 N6 C17 114.4(13) . . ?
C20 N6 U 130.1(11) . . ?
C17 N6 U 114.9(9) . . ?
C4 N7 C3 113.7(12) . . ?
C9 N8 C8 117.9(12) . . ?
C14 N9 C13 115.5(12) . . ?
C18 N10 C19 116.4(17) . . ?
N1 C1 C2 111.9(10) . . ?
N3 C2 C3 121.0(12) . . ?
N3 C2 C1 116.9(11) . . ?
C3 C2 C1 122.1(12) . . ?
C2 C3 N7 122.2(12) . . ?
N7 C4 C5 123.9(13) . . ?
N3 C5 C4 121.8(13) . . ?
N1 C6 C7 113.0(10) . . ?
N4 C7 C8 121.1(13) . . ?
N4 C7 C6 116.6(12) . . ?
C8 C7 C6 122.3(12) . . ?
N8 C8 C7 122.7(13) . . ?
N8 C9 C10 120.3(13) . . ?
N4 C10 C9 121.5(12) . . ?
N2 C11 C12 112.3(11) . . ?
N5 C12 C13 120.5(12) . . ?
N5 C12 C11 119.1(11) . . ?
C13 C12 C11 120.3(12) . . ?
N9 C13 C12 122.8(13) . . ?
N9 C14 C15 124.2(13) . . ?
N5 C15 C14 120.6(13) . . ?
N2 C16 C17 110.4(11) . . ?
N6 C17 C18 122.9(15) . . ?
N6 C17 C16 117.0(13) . . ?
C18 C17 C16 120.0(14) . . ?
N10 C18 C17 121.3(18) . . ?
N10 C19 C20 121.0(18) . . ?
N6 C20 C19 123.5(17) . . ?
C22 C21 N1 111.4(10) . . ?
C22 C21 C26 111.0(11) . . ?
N1 C21 C26 113.2(10) . . ?
C21 C22 C23 110.7(12) . . ?
C21 C22 N2 110.2(10) . . ?
C23 C22 N2 112.8(11) . . ?
C22 C23 C24 112.1(12) . . ?
C25 C24 C23 107.7(12) . . ?
C24 C25 C26 110.0(12) . . ?
C25 C26 C21 112.7(12) . . ?
N101 C101 C102 159(10) . . ?
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 N4 2.537(11) . ?
U N5 2.593(12) . ?
U N2 2.627(10) . ?
U N3 2.659(11) . ?
U N1 2.677(10) . ?
U N6 2.685(12) . ?
U I1 3.1432(11) . ?
U I2 3.1695(10) . ?
N1 C6 1.466(16) . ?
N1 C1 1.477(17) . ?
N1 C21 1.521(16) . ?
N2 C11 1.502(18) . ?
N2 C16 1.505(18) . ?
N2 C22 1.541(15) . ?
N3 C5 1.296(17) . ?
N3 C2 1.358(16) . ?
N4 C10 1.344(17) . ?
N4 C7 1.348(16) . ?
N5 C12 1.345(18) . ?
N5 C15 1.365(18) . ?
N6 C20 1.306(19) . ?
N6 C17 1.309(18) . ?
N7 C4 1.319(18) . ?
N7 C3 1.389(18) . ?
N8 C9 1.306(19) . ?
N8 C8 1.338(18) . ?
N9 C14 1.30(2) . ?
N9 C13 1.345(18) . ?
N10 C18 1.30(2) . ?
N10 C19 1.31(3) . ?
C1 C2 1.506(18) . ?
C2 C3 1.366(19) . ?
C4 C5 1.389(19) . ?
C6 C7 1.514(19) . ?
C7 C8 1.37(2) . ?
C9 C10 1.42(2) . ?
C11 C12 1.511(18) . ?
C12 C13 1.386(19) . ?
C14 C15 1.37(2) . ?
C16 C17 1.52(2) . ?
C17 C18 1.40(2) . ?
C19 C20 1.38(3) . ?
C21 C22 1.508(19) . ?
C21 C26 1.539(16) . ?
C22 C23 1.525(19) . ?
C23 C24 1.527(18) . ?
C24 C25 1.51(2) . ?
C25 C26 1.53(2) . ?
C101 N101 0.93(13) . ?
C101 C102 1.29(13) . ?
