#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/38/7103807.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_7103807
loop_
_publ_author_name
'Enriquez, Alejandro E.'
'Matonic, John H.'
'Scott, Brian L.'
'Neu, Mary P.'
_publ_section_title
;
 Preparation and structures of homoleptic Pu(III) and U(III) acetonitrile
 salts
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   15
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1892
_journal_page_last               1893
_journal_paper_doi               10.1039/b303558a
_journal_year                    2003
_chemical_formula_sum            'C18 H27 I3 N9 O0 U'
_chemical_formula_weight         988.22
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            3
_cell_length_a                   10.974(4)
_cell_length_b                   10.974(4)
_cell_length_c                   24.475(11)
_cell_measurement_temperature    203(2)
_cell_volume                     2552.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       '/f and /w 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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            6253
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    7.508
_exptl_absorpt_correction_T_max  0.3151
_exptl_absorpt_correction_T_min  0.1532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1347
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.273
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.052
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0737
_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)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                1141
_reflns_number_total             1329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303558a.txt
_cod_data_source_block           ccd615
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7103807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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'
'-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'
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
U1 U 0.6667 0.3333 0.3333 0.0475(3) Uani 1 6 d S . .
I2 I 0.6667 0.3333 0.09592(3) 0.0489(3) Uani 1 3 d S . .
I3 I 1.0000 0.0000 0.55212(17) 0.0632(8) Uani 0.33 3 d SP . .
I4 I 1.0000 0.0000 0.5000 0.104(3) Uani 0.33 6 d SP . .
N1 N 0.8312(14) 0.3342(14) 0.4095(6) 0.058(3) Uani 0.50 1 d P . .
N2 N 0.6673(16) 0.0921(16) 0.3334(6) 0.070(4) Uani 0.50 1 d P . .
N3 N 0.6649(14) 0.1671(16) 0.4097(6) 0.062(4) Uani 0.50 1 d P . .
C1 C 0.8990(16) 0.3346(15) 0.4456(7) 0.052(4) Uani 0.50 1 d P . .
C2 C 0.996(2) 0.342(2) 0.4892(7) 0.049(5) Uani 0.50 1 d P . .
C3 C 0.663(3) -0.007(2) 0.3337(9) 0.092(8) Uani 0.50 1 d P . .
C4 C 0.6667 -0.1667 0.3333 0.190(13) Uani 1 2 d S . .
C5 C 0.6671(15) 0.1018(15) 0.4460(7) 0.050(4) Uani 0.50 1 d P . .
C6 C 0.658(2) 0.007(2) 0.4883(7) 0.050(5) 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'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 '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
N1 U1 N1 74.0(5) . 3_665 ?
N1 U1 N1 74.0(5) . 2_655 ?
N1 U1 N1 74.0(5) 3_665 2_655 ?
N1 U1 N1 179.998(2) . 16_655 ?
N1 U1 N1 106.0(5) 3_665 16_655 ?
N1 U1 N1 106.0(5) 2_655 16_655 ?
N1 U1 N1 106.0(5) . 18_545 ?
N1 U1 N1 179.999(1) 3_665 18_545 ?
N1 U1 N1 106.0(5) 2_655 18_545 ?
N1 U1 N1 74.0(5) 16_655 18_545 ?
N1 U1 N1 106.0(5) . 17 ?
N1 U1 N1 106.0(5) 3_665 17 ?
N1 U1 N1 179.999(2) 2_655 17 ?
N1 U1 N1 74.0(5) 16_655 17 ?
N1 U1 N1 74.0(5) 18_545 17 ?
N1 U1 N3 41.2(5) . . ?
N1 U1 N3 40.2(4) 3_665 . ?
N1 U1 N3 88.2(4) 2_655 . ?
N1 U1 N3 138.8(5) 16_655 . ?
N1 U1 N3 139.8(4) 18_545 . ?
N1 U1 N3 91.8(4) 17 . ?
N1 U1 N3 40.2(4) . 2_655 ?
N1 U1 N3 88.2(4) 3_665 2_655 ?
N1 U1 N3 41.2(5) 2_655 2_655 ?
N1 U1 N3 139.8(4) 16_655 2_655 ?
N1 U1 N3 91.8(4) 18_545 2_655 ?
N1 U1 N3 138.8(5) 17 2_655 ?
N3 U1 N3 74.2(5) . 2_655 ?
N1 U1 N3 88.2(4) . 3_665 ?
N1 U1 N3 41.2(5) 3_665 3_665 ?
N1 U1 N3 40.2(4) 2_655 3_665 ?
N1 U1 N3 91.8(4) 16_655 3_665 ?
N1 U1 N3 138.8(5) 18_545 3_665 ?
N1 U1 N3 139.8(4) 17 3_665 ?
N3 U1 N3 74.2(5) . 3_665 ?
N3 U1 N3 74.2(5) 2_655 3_665 ?
N1 U1 N3 138.8(5) . 16_655 ?
N1 U1 N3 139.8(4) 3_665 16_655 ?
N1 U1 N3 91.8(4) 2_655 16_655 ?
N1 U1 N3 41.2(5) 16_655 16_655 ?
N1 U1 N3 40.2(4) 18_545 16_655 ?
N1 U1 N3 88.2(4) 17 16_655 ?
N3 U1 N3 179.998(2) . 16_655 ?
N3 U1 N3 105.8(5) 2_655 16_655 ?
N3 U1 N3 105.8(5) 3_665 16_655 ?
N1 U1 N3 139.8(4) . 17 ?
N1 U1 N3 91.8(4) 3_665 17 ?
N1 U1 N3 138.8(5) 2_655 17 ?
N1 U1 N3 40.2(4) 16_655 17 ?
N1 U1 N3 88.2(4) 18_545 17 ?
N1 U1 N3 41.2(5) 17 17 ?
N3 U1 N3 105.8(5) . 17 ?
N3 U1 N3 179.999(1) 2_655 17 ?
N3 U1 N3 105.8(5) 3_665 17 ?
N3 U1 N3 74.2(5) 16_655 17 ?
N1 U1 N3 91.8(4) . 18_545 ?
N1 U1 N3 138.8(5) 3_665 18_545 ?
N1 U1 N3 139.8(4) 2_655 18_545 ?
N1 U1 N3 88.2(4) 16_655 18_545 ?
N1 U1 N3 41.2(5) 18_545 18_545 ?
N1 U1 N3 40.2(4) 17 18_545 ?
N3 U1 N3 105.8(5) . 18_545 ?
N3 U1 N3 105.8(5) 2_655 18_545 ?
N3 U1 N3 180.0(10) 3_665 18_545 ?
N3 U1 N3 74.2(5) 16_655 18_545 ?
N3 U1 N3 74.2(5) 17 18_545 ?
N1 U1 N2 110.3(4) . 16_655 ?
N1 U1 N2 110.5(4) 3_665 16_655 ?
N1 U1 N2 46.0(4) 2_655 16_655 ?
N1 U1 N2 69.7(4) 16_655 16_655 ?
N1 U1 N2 69.5(4) 18_545 16_655 ?
N1 U1 N2 134.0(4) 17 16_655 ?
N3 U1 N2 134.2(4) . 16_655 ?
N3 U1 N2 70.1(4) 2_655 16_655 ?
N3 U1 N2 69.2(4) 3_665 16_655 ?
N3 U1 N2 45.8(4) 16_655 16_655 ?
N3 U1 N2 109.9(4) 17 16_655 ?
N3 U1 N2 110.8(4) 18_545 16_655 ?
N1 U1 N2 69.7(4) . . ?
N1 U1 N2 69.5(4) 3_665 . ?
N1 U1 N2 134.0(4) 2_655 . ?
N1 U1 N2 110.3(4) 16_655 . ?
N1 U1 N2 110.5(4) 18_545 . ?
N1 U1 N2 46.0(4) 17 . ?
N3 U1 N2 45.8(4) . . ?
N3 U1 N2 109.9(4) 2_655 . ?
N3 U1 N2 110.8(4) 3_665 . ?
N3 U1 N2 134.2(4) 16_655 . ?
N3 U1 N2 70.1(4) 17 . ?
N3 U1 N2 69.2(4) 18_545 . ?
N2 U1 N2 179.999(3) 16_655 . ?
N1 U1 N2 110.5(4) . 17 ?
N1 U1 N2 46.0(4) 3_665 17 ?
N1 U1 N2 110.3(4) 2_655 17 ?
N1 U1 N2 69.5(4) 16_655 17 ?
N1 U1 N2 134.0(4) 18_545 17 ?
N1 U1 N2 69.7(4) 17 17 ?
N3 U1 N2 69.2(4) . 17 ?
N3 U1 N2 134.2(4) 2_655 17 ?
N3 U1 N2 70.1(4) 3_665 17 ?
N3 U1 N2 110.8(4) 16_655 17 ?
N3 U1 N2 45.8(4) 17 17 ?
N3 U1 N2 109.9(4) 18_545 17 ?
N2 U1 N2 120.001(3) 16_655 17 ?
N2 U1 N2 59.999(4) . 17 ?
N1 U1 N2 69.5(4) . 2_655 ?
N1 U1 N2 134.0(4) 3_665 2_655 ?
N1 U1 N2 69.7(4) 2_655 2_655 ?
N1 U1 N2 110.5(4) 16_655 2_655 ?
N1 U1 N2 46.0(4) 18_545 2_655 ?
N1 U1 N2 110.3(4) 17 2_655 ?
N3 U1 N2 110.8(4) . 2_655 ?
N3 U1 N2 45.8(4) 2_655 2_655 ?
N3 U1 N2 109.9(4) 3_665 2_655 ?
N3 U1 N2 69.2(4) 16_655 2_655 ?
N3 U1 N2 134.2(4) 17 2_655 ?
N3 U1 N2 70.1(4) 18_545 2_655 ?
N2 U1 N2 60.000(3) 16_655 2_655 ?
N2 U1 N2 120.000(4) . 2_655 ?
N2 U1 N2 179.998(1) 17 2_655 ?
N1 U1 N2 134.0(4) . 3_665 ?
N1 U1 N2 69.7(4) 3_665 3_665 ?
N1 U1 N2 69.5(4) 2_655 3_665 ?
N1 U1 N2 46.0(4) 16_655 3_665 ?
N1 U1 N2 110.3(4) 18_545 3_665 ?
N1 U1 N2 110.5(4) 17 3_665 ?
N3 U1 N2 109.9(4) . 3_665 ?
N3 U1 N2 110.8(4) 2_655 3_665 ?
N3 U1 N2 45.8(4) 3_665 3_665 ?
N3 U1 N2 70.1(4) 16_655 3_665 ?
N3 U1 N2 69.2(4) 17 3_665 ?
N3 U1 N2 134.2(4) 18_545 3_665 ?
N2 U1 N2 60.001(4) 16_655 3_665 ?
N2 U1 N2 120.000(4) . 3_665 ?
N2 U1 N2 60.001(3) 17 3_665 ?
N2 U1 N2 120.000(3) 2_655 3_665 ?
N1 U1 N2 46.0(4) . 18_545 ?
N1 U1 N2 110.3(4) 3_665 18_545 ?
N1 U1 N2 110.5(4) 2_655 18_545 ?
N1 U1 N2 134.0(4) 16_655 18_545 ?
N1 U1 N2 69.7(4) 18_545 18_545 ?
N1 U1 N2 69.5(4) 17 18_545 ?
N3 U1 N2 70.1(4) . 18_545 ?
N3 U1 N2 69.2(4) 2_655 18_545 ?
N3 U1 N2 134.2(4) 3_665 18_545 ?
N3 U1 N2 109.9(4) 16_655 18_545 ?
N3 U1 N2 110.8(4) 17 18_545 ?
N3 U1 N2 45.8(4) 18_545 18_545 ?
N2 U1 N2 120.000(4) 16_655 18_545 ?
N2 U1 N2 60.000(4) . 18_545 ?
N2 U1 N2 119.998(2) 17 18_545 ?
N2 U1 N2 60.001(3) 2_655 18_545 ?
N2 U1 N2 180.0(7) 3_665 18_545 ?
I4 I3 I3 0.0 . 10_756 ?
I3 I4 I3 180.000(2) 10_756 . ?
C1 N1 N3 108.2(13) . 2_655 ?
C1 N1 N3 108.6(13) . . ?
N3 N1 N3 120.7(11) 2_655 . ?
C1 N1 U1 176.0(12) . . ?
N3 N1 U1 70.3(7) 2_655 . ?
N3 N1 U1 69.7(6) . . ?
C3 N2 U1 177.4(18) . . ?
C5 N3 N1 109.8(13) . 3_665 ?
C5 N3 N1 107.8(13) . . ?
N1 N3 N1 119.3(11) 3_665 . ?
C5 N3 U1 174.9(13) . . ?
N1 N3 U1 69.5(6) 3_665 . ?
N1 N3 U1 69.0(7) . . ?
N1 C1 C2 175.4(18) . . ?
N1 C1 C6 173.1(15) . 11_666 ?
C2 C1 C6 9.5(12) . 11_666 ?
C6 C2 C1 144(5) 11_666 . ?
C6 C2 C5 24(4) 11_666 11_666 ?
C1 C2 C5 148.2(15) . 11_666 ?
N2 C3 C4 176(2) . . ?
C3 C4 C3 179.998(4) . 16_645 ?
N3 C5 C6 173.5(17) . . ?
N3 C5 C2 173.2(15) . 12_546 ?
C6 C5 C2 9.3(13) . 12_546 ?
C2 C6 C5 146(5) 12_546 . ?
C2 C6 C1 26(4) 12_546 12_546 ?
C5 C6 C1 149.1(16) . 12_546 ?
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
U1 N1 2.592(14) . ?
U1 N1 2.592(14) 3_665 ?
U1 N1 2.592(14) 2_655 ?
U1 N1 2.592(14) 16_655 ?
U1 N1 2.592(14) 18_545 ?
U1 N1 2.592(14) 17 ?
U1 N3 2.604(15) . ?
U1 N3 2.604(15) 2_655 ?
U1 N3 2.604(15) 3_665 ?
U1 N3 2.604(15) 16_655 ?
U1 N3 2.604(15) 17 ?
U1 N3 2.604(15) 18_545 ?
U1 N2 2.651(16) 16_655 ?
U1 N2 2.651(16) . ?
U1 N2 2.651(16) 17 ?
U1 N2 2.651(16) 2_655 ?
U1 N2 2.651(16) 3_665 ?
U1 N2 2.651(16) 18_545 ?
I3 I4 1.276(4) . ?
I3 I3 2.551(8) 10_756 ?
I4 I3 1.276(4) 10_756 ?
N1 C1 1.15(2) . ?
N1 N3 1.79(2) 2_655 ?
N1 N3 1.83(2) . ?
N2 C3 1.06(2) . ?
N3 C5 1.15(2) . ?
N3 N1 1.79(2) 3_665 ?
C1 C2 1.48(2) . ?
C1 C6 1.96(3) 11_666 ?
C2 C6 0.559(14) 11_666 ?
C2 C5 1.93(3) 11_666 ?
C3 C4 1.78(2) . ?
C4 C3 1.78(2) 16_645 ?
C5 C6 1.44(2) . ?
C5 C2 1.93(3) 12_546 ?
C6 C2 0.559(14) 12_546 ?
C6 C1 1.96(3) 12_546 ?
