#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308551.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_4308551
loop_
_publ_author_name
'Jean-Claude Berthet'
'Pierre Thuéry'
'Michel Ephritikhine'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      Bât. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       ephri@drecam.cea.fr
_publ_contact_author_fax         '33 (1) 69 08 66 40'
_publ_contact_author_name        'M. Ephritikhine'
_publ_contact_author_phone       '33 (1) 69 08 64 36'
_publ_section_title
;
New Efficient Synthesis of [UI4(MeCN)4]. X-ray Crystal Structures of
[UI2(MeCN)7][UI6], [UI4(py)3], and [U(dmf)9]I4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1142
_journal_page_last               1146
_journal_paper_doi               10.1021/ic048603p
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C15 H15 I4 N3 U'
_chemical_formula_weight         982.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.094(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3294(3)
_cell_length_b                   13.1236(5)
_cell_length_c                   15.4734(6)
_cell_measurement_reflns_used    14135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.06
_cell_volume                     2198.99(14)
_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 0.896
_diffrn_measured_fraction_theta_max 0.896
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14135
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    12.999
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    2.969
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0255
_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)+6.7946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                3558
_reflns_number_total             3741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048603psi20041007_101646_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4308551
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.741839(18) 0.122340(15) 0.802055(13) 0.02101(8) Uani 1 1 d . . .
I1 I 0.74853(4) -0.08953(3) 0.87364(2) 0.02736(10) Uani 1 1 d . . .
I2 I 0.88800(3) 0.19397(3) 0.99017(2) 0.02652(10) Uani 1 1 d . . .
I3 I 0.48945(3) 0.07745(3) 0.67459(2) 0.02946(10) Uani 1 1 d . . .
I4 I 0.73667(4) 0.33097(3) 0.72906(3) 0.03260(11) Uani 1 1 d . . .
N1 N 0.9716(5) 0.1274(4) 0.8024(3) 0.0244(10) Uani 1 1 d . . .
N2 N 0.7870(5) 0.0320(4) 0.6631(3) 0.0258(10) Uani 1 1 d . . .
N3 N 0.5828(5) 0.1852(4) 0.8805(3) 0.0270(10) Uani 1 1 d . . .
C1 C 1.0104(6) 0.1755(5) 0.7378(4) 0.0281(13) Uani 1 1 d . . .
H1A H 0.9536 0.2149 0.6953 0.034 Uiso 1 1 calc R . .
C2 C 1.1278(6) 0.1691(5) 0.7317(4) 0.0323(14) Uani 1 1 d . . .
H2A H 1.1498 0.2032 0.6861 0.039 Uiso 1 1 calc R . .
C3 C 1.2144(6) 0.1108(5) 0.7949(4) 0.0343(14) Uani 1 1 d . . .
H3A H 1.2954 0.1055 0.7930 0.041 Uiso 1 1 calc R . .
C4 C 1.1759(6) 0.0615(5) 0.8603(4) 0.0335(14) Uani 1 1 d . . .
H4A H 1.2316 0.0217 0.9032 0.040 Uiso 1 1 calc R . .
C5 C 1.0555(5) 0.0702(4) 0.8629(4) 0.0247(12) Uani 1 1 d . . .
H5A H 1.0316 0.0357 0.9075 0.030 Uiso 1 1 calc R . .
C6 C 0.7454(6) 0.0731(5) 0.5807(4) 0.0306(13) Uani 1 1 d . . .
H6A H 0.6932 0.1293 0.5727 0.037 Uiso 1 1 calc R . .
C7 C 0.7767(6) 0.0356(5) 0.5062(4) 0.0312(13) Uani 1 1 d . . .
H7A H 0.7468 0.0667 0.4500 0.037 Uiso 1 1 calc R . .
C8 C 0.8532(6) -0.0489(5) 0.5172(4) 0.0367(15) Uani 1 1 d . . .
H8A H 0.8749 -0.0759 0.4685 0.044 Uiso 1 1 calc R . .
C9 C 0.8958(6) -0.0915(5) 0.6012(4) 0.0349(14) Uani 1 1 d . . .
H9A H 0.9473 -0.1482 0.6101 0.042 Uiso 1 1 calc R . .
C10 C 0.8630(6) -0.0507(5) 0.6727(4) 0.0292(13) Uani 1 1 d . . .
H10A H 0.8935 -0.0804 0.7295 0.035 Uiso 1 1 calc R . .
C11 C 0.5136(6) 0.2697(5) 0.8575(4) 0.0318(13) Uani 1 1 d . . .
H11A H 0.5225 0.3084 0.8095 0.038 Uiso 1 1 calc R . .
C12 C 0.4311(6) 0.3019(5) 0.9005(5) 0.0350(14) Uani 1 1 d . . .
H12A H 0.3852 0.3609 0.8819 0.042 Uiso 1 1 calc R . .
C13 C 0.4166(6) 0.2457(5) 0.9721(4) 0.0329(14) Uani 1 1 d . . .
H13A H 0.3608 0.2658 1.0025 0.039 Uiso 1 1 calc R . .
C14 C 0.4872(6) 0.1583(5) 0.9975(4) 0.0311(13) Uani 1 1 d . . .
H14A H 0.4794 0.1188 1.0454 0.037 Uiso 1 1 calc R . .
C15 C 0.5689(6) 0.1308(5) 0.9513(4) 0.0303(13) Uani 1 1 d . . .
H15A H 0.6165 0.0725 0.9692 0.036 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'
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
N3 U N1 145.64(15) . . ?
N3 U N2 148.89(15) . . ?
N1 U N2 65.10(15) . . ?
N3 U I4 86.87(11) . . ?
N1 U I4 83.38(11) . . ?
N2 U I4 95.27(11) . . ?
N3 U I1 93.92(11) . . ?
N1 U I1 96.12(11) . . ?
N2 U I1 83.90(11) . . ?
I4 U I1 179.157(13) . . ?
N3 U I3 73.24(11) . . ?
N1 U I3 139.63(10) . . ?
N2 U I3 75.68(11) . . ?
I4 U I3 91.293(12) . . ?
I1 U I3 88.654(12) . . ?
N3 U I2 73.21(11) . . ?
N1 U I2 74.17(10) . . ?
N2 U I2 137.55(11) . . ?
I4 U I2 91.342(12) . . ?
I1 U I2 89.170(12) . . ?
I3 U I2 146.135(12) . . ?
C5 N1 C1 117.0(5) . . ?
C5 N1 U 119.2(4) . . ?
C1 N1 U 123.3(4) . . ?
C6 N2 C10 117.3(5) . . ?
C6 N2 U 119.9(4) . . ?
C10 N2 U 122.5(4) . . ?
C11 N3 C15 116.8(5) . . ?
C11 N3 U 124.9(4) . . ?
C15 N3 U 118.3(4) . . ?
N1 C1 C2 123.7(6) . . ?
C1 C2 C3 119.0(6) . . ?
C4 C3 C2 117.7(6) . . ?
C3 C4 C5 120.8(6) . . ?
N1 C5 C4 121.8(6) . . ?
N2 C6 C7 122.9(6) . . ?
C8 C7 C6 118.9(6) . . ?
C9 C8 C7 118.5(6) . . ?
C8 C9 C10 120.2(6) . . ?
N2 C10 C9 122.2(6) . . ?
N3 C11 C12 123.8(6) . . ?
C11 C12 C13 119.1(6) . . ?
C12 C13 C14 118.3(6) . . ?
C15 C14 C13 119.4(6) . . ?
N3 C15 C14 122.6(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
U N3 2.586(5) . ?
U N1 2.602(5) . ?
U N2 2.634(5) . ?
U I4 2.9558(4) . ?
U I1 2.9857(4) . ?
U I3 3.0163(4) . ?
U I2 3.0438(4) . ?
N1 C5 1.349(8) . ?
N1 C1 1.361(7) . ?
N2 C6 1.337(8) . ?
N2 C10 1.366(8) . ?
N3 C11 1.343(8) . ?
N3 C15 1.355(8) . ?
C1 C2 1.363(9) . ?
C2 C3 1.393(10) . ?
C3 C4 1.375(9) . ?
C4 C5 1.381(9) . ?
C6 C7 1.392(9) . ?
C7 C8 1.386(10) . ?
C8 C9 1.367(10) . ?
C9 C10 1.375(9) . ?
C11 C12 1.365(9) . ?
C12 C13 1.380(9) . ?
C13 C14 1.387(9) . ?
C14 C15 1.374(9) . ?
