#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:19:23 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179055 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/17/4301730.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_4301730
loop_
_publ_author_name
'Liam P. Spencer'
'Ping Yang'
'Brian L. Scott'
'Enrique R. Batista'
'James M. Boncella'
_publ_section_title
;
Uranium(VI) Bis(imido) Chalcogenate Complexes: Synthesis and Density
Functional Theory Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2693
_journal_page_last               2700
_journal_paper_doi               10.1021/ic802212m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C20 H30 I2 N4 U'
_chemical_formula_weight         818.31
_chemical_name_systematic
; 

 ? 

;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.146(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.973(10)
_cell_length_b                   9.654(6)
_cell_length_c                   17.214(10)
_cell_measurement_temperature    120(1)
_cell_volume                     2631(3)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16799
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.528
_exptl_absorpt_correction_T_max  0.5486
_exptl_absorpt_correction_T_min  0.4276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.611
_refine_diff_density_min         -3.471
_refine_diff_density_rms         0.324
_refine_ls_extinction_coef       0.00138(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                3562
_reflns_number_total             5301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802212m_si_001_4.cif
_cod_data_source_block           apx520
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301730
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
U1 U 0.25063(3) 0.78005(5) 0.37845(3) 0.0314(2) Uani 1 1 d . . .
I1 I 0.35734(6) 1.01323(9) 0.48508(5) 0.0411(3) Uani 1 1 d . . .
I2 I 0.10420(7) 0.74686(10) 0.43647(7) 0.0442(3) Uani 1 1 d . . .
N1 N 0.3597(7) 0.7448(10) 0.3120(7) 0.028(2) Uani 1 1 d . . .
N2 N 0.2107(7) 0.6177(11) 0.2592(6) 0.035(3) Uani 1 1 d . . .
N3 N 0.1960(7) 0.9071(13) 0.2989(6) 0.042(3) Uani 1 1 d . A .
N4 N 0.3021(7) 0.6358(11) 0.4442(7) 0.035(3) Uani 1 1 d . . .
C1 C 0.1361(10) 0.5575(14) 0.2342(8) 0.041(3) Uani 1 1 d . . .
H1 H 0.1043 0.5665 0.2681 0.050 Uiso 1 1 calc R . .
C2 C 0.1009(9) 0.4811(14) 0.1609(9) 0.041(3) Uani 1 1 d . . .
H2 H 0.0461 0.4471 0.1445 0.050 Uiso 1 1 calc R . .
C3 C 0.1505(8) 0.4575(14) 0.1131(8) 0.035(3) Uani 1 1 d . . .
C4 C 0.1163(9) 0.3763(16) 0.0362(7) 0.043(4) Uani 1 1 d . . .
H4A H 0.1613 0.3266 0.0272 0.065 Uiso 1 1 calc R . .
H4B H 0.0900 0.4374 -0.0100 0.065 Uiso 1 1 calc R . .
H4C H 0.0752 0.3118 0.0409 0.065 Uiso 1 1 calc R . .
C5 C 0.2282(8) 0.5210(13) 0.1400(8) 0.035(3) Uani 1 1 d . . .
H5 H 0.2615 0.5125 0.1076 0.041 Uiso 1 1 calc R . .
C6 C 0.2589(8) 0.5962(13) 0.2123(8) 0.034(3) Uani 1 1 d . . .
C7 C 0.3420(8) 0.6614(13) 0.2450(8) 0.032(3) Uani 1 1 d . . .
C8 C 0.4025(8) 0.6396(13) 0.2087(8) 0.038(3) Uani 1 1 d . . .
H8 H 0.3894 0.5820 0.1624 0.045 Uiso 1 1 calc R . .
C9 C 0.4804(9) 0.7007(15) 0.2394(9) 0.040(3) Uani 1 1 d . . .
C10 C 0.5461(9) 0.6748(17) 0.2027(9) 0.050(4) Uani 1 1 d . . .
H10A H 0.5821 0.6004 0.2322 0.075 Uiso 1 1 calc R . .
H10B H 0.5792 0.7570 0.2072 0.075 Uiso 1 1 calc R . .
H10C H 0.5194 0.6500 0.1451 0.075 Uiso 1 1 calc R . .
C11 C 0.4973(9) 0.7824(14) 0.3096(10) 0.044(4) Uani 1 1 d . . .
H11 H 0.5499 0.8235 0.3346 0.053 Uiso 1 1 calc R . .
C12 C 0.4351(8) 0.8015(13) 0.3415(8) 0.034(3) Uani 1 1 d . . .
H12 H 0.4470 0.8590 0.3876 0.041 Uiso 1 1 calc R . .
C13 C 0.1464(10) 1.0115(15) 0.2397(9) 0.052(4) Uani 1 1 d D . .
C14 C 0.211(2) 1.114(3) 0.232(3) 0.090(5) Uani 0.50 1 d PD A 1
H14A H 0.2445 1.0708 0.2050 0.135 Uiso 0.50 1 calc PR A 1
H14B H 0.2461 1.1444 0.2867 0.135 Uiso 0.50 1 calc PR A 1
H14C H 0.1818 1.1925 0.2001 0.135 Uiso 0.50 1 calc PR A 1
C14' C 0.209(2) 1.073(4) 0.202(2) 0.090(5) Uani 0.50 1 d PD A 2
H14D H 0.2291 1.0010 0.1757 0.135 Uiso 0.50 1 calc PR A 2
H14E H 0.2556 1.1148 0.2453 0.135 Uiso 0.50 1 calc PR A 2
H14F H 0.1804 1.1424 0.1614 0.135 Uiso 0.50 1 calc PR A 2
C15 C 0.1087(13) 1.112(2) 0.2832(12) 0.090(5) Uani 1 1 d D A .
H15A H 0.0857 1.0627 0.3184 0.135 Uiso 1 1 calc R . .
H15B H 0.0647 1.1642 0.2425 0.135 Uiso 1 1 calc R . .
H15C H 0.1518 1.1747 0.3164 0.135 Uiso 1 1 calc R . .
C16 C 0.0656(19) 0.938(5) 0.188(3) 0.090(5) Uani 0.50 1 d PD A 1
H16A H 0.0783 0.8678 0.1544 0.135 Uiso 0.50 1 calc PR A 1
H16B H 0.0271 1.0041 0.1516 0.135 Uiso 0.50 1 calc PR A 1
H16C H 0.0403 0.8966 0.2235 0.135 Uiso 0.50 1 calc PR A 1
C16' C 0.083(2) 0.930(4) 0.167(2) 0.090(5) Uani 0.50 1 d PD A 2
H16D H 0.1129 0.8694 0.1432 0.135 Uiso 0.50 1 calc PR A 2
H16E H 0.0489 0.9930 0.1256 0.135 Uiso 0.50 1 calc PR A 2
H16F H 0.0471 0.8754 0.1878 0.135 Uiso 0.50 1 calc PR A 2
C17 C 0.3363(10) 0.5031(13) 0.4895(9) 0.043(4) Uani 1 1 d . . .
C18 C 0.3927(15) 0.5480(19) 0.5762(11) 0.099(8) Uani 1 1 d . . .
H18A H 0.4278 0.4719 0.6043 0.149 Uiso 1 1 calc R . .
H18B H 0.3583 0.5766 0.6071 0.149 Uiso 1 1 calc R . .
H18C H 0.4275 0.6239 0.5722 0.149 Uiso 1 1 calc R . .
C19 C 0.3859(11) 0.4334(16) 0.4472(12) 0.071(5) Uani 1 1 d . . .
H19A H 0.3496 0.4072 0.3922 0.107 Uiso 1 1 calc R . .
H19B H 0.4119 0.3522 0.4780 0.107 Uiso 1 1 calc R . .
H19C H 0.4289 0.4951 0.4437 0.107 Uiso 1 1 calc R . .
C20 C 0.2610(11) 0.4182(16) 0.4894(13) 0.082(6) Uani 1 1 d . . .
H20A H 0.2290 0.3887 0.4337 0.123 Uiso 1 1 calc R . .
H20B H 0.2259 0.4736 0.5101 0.123 Uiso 1 1 calc R . .
H20C H 0.2805 0.3384 0.5245 0.123 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
N4 U1 N3 171.2(5) . . ?
N4 U1 N2 87.6(4) . . ?
N3 U1 N2 83.7(4) . . ?
N4 U1 N1 85.0(4) . . ?
N3 U1 N1 90.4(4) . . ?
N2 U1 N1 64.2(3) . . ?
N4 U1 I2 88.9(3) . . ?
N3 U1 I2 93.7(4) . . ?
N2 U1 I2 101.3(3) . . ?
N1 U1 I2 164.4(2) . . ?
N4 U1 I1 98.3(3) . . ?
N3 U1 I1 89.2(4) . . ?
N2 U1 I1 153.0(3) . . ?
N1 U1 I1 89.9(2) . . ?
I2 U1 I1 105.11(4) . . ?
C12 N1 C7 117.7(11) . . ?
C12 N1 U1 122.7(8) . . ?
C7 N1 U1 119.6(8) . . ?
C1 N2 C6 117.0(11) . . ?
C1 N2 U1 119.6(9) . . ?
C6 N2 U1 123.2(8) . . ?
C13 N3 U1 174.2(10) . . ?
C17 N4 U1 171.8(9) . . ?
N2 C1 C2 125.1(13) . . ?
C3 C2 C1 117.9(13) . . ?
C5 C3 C2 116.1(12) . . ?
C5 C3 C4 124.1(12) . . ?
C2 C3 C4 119.7(12) . . ?
C6 C5 C3 123.0(13) . . ?
N2 C6 C5 120.5(12) . . ?
N2 C6 C7 114.3(11) . . ?
C5 C6 C7 125.2(12) . . ?
N1 C7 C8 119.9(12) . . ?
N1 C7 C6 118.3(11) . . ?
C8 C7 C6 121.8(11) . . ?
C9 C8 C7 121.8(12) . . ?
C8 C9 C11 116.7(13) . . ?
C8 C9 C10 122.1(13) . . ?
C11 C9 C10 121.1(13) . . ?
C12 C11 C9 118.8(13) . . ?
N1 C12 C11 125.1(12) . . ?
N3 C13 C15 109.9(12) . . ?
N3 C13 C14 105(2) . . ?
C15 C13 C14 93.8(19) . . ?
N3 C13 C16 105(2) . . ?
C15 C13 C16 98(2) . . ?
C14 C13 C16 141(3) . . ?
N3 C13 C16' 106(2) . . ?
C15 C13 C16' 116(2) . . ?
C14 C13 C16' 126(2) . . ?
C16 C13 C16' 20(2) . . ?
N3 C13 C14' 104(2) . . ?
C15 C13 C14' 115.9(19) . . ?
C14 C13 C14' 24(2) . . ?
C16 C13 C14' 123(3) . . ?
C16' C13 C14' 104.1(15) . . ?
C19 C17 C18 110.4(16) . . ?
C19 C17 N4 108.5(12) . . ?
C18 C17 N4 104.8(11) . . ?
C19 C17 C20 112.8(13) . . ?
C18 C17 C20 112.8(16) . . ?
N4 C17 C20 107.0(12) . . ?
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 N4 1.809(11) . ?
U1 N3 1.823(11) . ?
U1 N2 2.476(10) . ?
U1 N1 2.526(11) . ?
U1 I2 3.0114(18) . ?
U1 I1 3.0525(15) . ?
N1 C12 1.313(16) . ?
N1 C7 1.350(15) . ?
N2 C1 1.317(17) . ?
N2 C6 1.356(16) . ?
N3 C13 1.465(17) . ?
N4 C17 1.503(16) . ?
C1 C2 1.396(18) . ?
C2 C3 1.391(18) . ?
C3 C5 1.374(17) . ?
C3 C4 1.467(17) . ?
C5 C6 1.372(17) . ?
C6 C7 1.459(18) . ?
C7 C8 1.397(18) . ?
C8 C9 1.369(18) . ?
C9 C11 1.383(19) . ?
C9 C10 1.487(19) . ?
C11 C12 1.367(18) . ?
C13 C15 1.504(15) . ?
C13 C14 1.512(19) . ?
C13 C16 1.516(19) . ?
C13 C16' 1.541(18) . ?
C13 C14' 1.548(18) . ?
C17 C19 1.46(2) . ?
C17 C18 1.52(2) . ?
C17 C20 1.52(2) . ?
