#------------------------------------------------------------------------------
#$Date: 2019-11-20 12:20:29 +0200 (Wed, 20 Nov 2019) $
#$Revision: 231085 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/59/4345995.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_4345995
loop_
_publ_author_name
'Andrew J. Gaunt'
'Brian L. Scott'
'Mary P. Neu'
_publ_section_title
;
 U(IV) Chalcogenolates Synthesized via Oxidation of Uranium Metal by
 Dichalcogenides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7401
_journal_page_last               7407
_journal_paper_doi               10.1021/ic060560k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C39 H35 N3 S4 U'
_chemical_formula_weight         911.97
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.162(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6836(10)
_cell_length_b                   16.1000(14)
_cell_length_c                   19.6157(17)
_cell_measurement_temperature    141(2)
_cell_volume                     3684.2(6)
_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      141(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33105
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.664
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.951
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0453
_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)+(0.0393P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                5524
_reflns_number_total             7740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060560ksi20060614_012839.cif
_cod_data_source_block           apx136
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4345995
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 0.12622(2) 0.355233(14) 0.221574(12) 0.01810(9) Uani 1 1 d . . .
S1 S 0.35773(14) 0.35785(10) 0.24931(9) 0.0229(4) Uani 1 1 d . . .
S2 S 0.13374(14) 0.22056(11) 0.13848(8) 0.0240(4) Uani 1 1 d . . .
S3 S -0.01460(14) 0.41334(10) 0.11656(8) 0.0223(4) Uani 1 1 d . . .
S4 S 0.07871(15) 0.50164(10) 0.28795(9) 0.0241(4) Uani 1 1 d . . .
N1 N 0.1379(5) 0.2645(3) 0.3291(3) 0.0236(13) Uani 1 1 d . . .
N2 N 0.2299(5) 0.4483(3) 0.1361(3) 0.0238(13) Uani 1 1 d . . .
N3 N -0.0740(4) 0.3024(3) 0.2587(3) 0.0221(12) Uani 1 1 d . . .
C1 C 0.4058(5) 0.2955(4) 0.3199(3) 0.0260(16) Uani 1 1 d . . .
C2 C 0.4549(6) 0.3354(4) 0.3778(3) 0.0267(16) Uani 1 1 d . . .
H2 H 0.4616 0.3930 0.3785 0.032 Uiso 1 1 calc R . .
C3 C 0.4939(6) 0.2888(5) 0.4348(4) 0.0311(17) Uani 1 1 d . . .
H3 H 0.5263 0.3154 0.4733 0.037 Uiso 1 1 calc R . .
C4 C 0.4842(6) 0.2043(5) 0.4336(4) 0.0333(18) Uani 1 1 d . . .
H4 H 0.5097 0.1737 0.4717 0.040 Uiso 1 1 calc R . .
C5 C 0.4376(6) 0.1638(4) 0.3774(4) 0.0303(17) Uani 1 1 d . . .
H5 H 0.4317 0.1062 0.3772 0.036 Uiso 1 1 calc R . .
C6 C 0.3986(6) 0.2103(4) 0.3200(4) 0.0267(16) Uani 1 1 d . . .
H6 H 0.3676 0.1829 0.2816 0.032 Uiso 1 1 calc R . .
C7 C 0.2508(6) 0.1520(4) 0.1554(3) 0.0228(15) Uani 1 1 d . . .
C8 C 0.3606(6) 0.1733(4) 0.1353(4) 0.0336(18) Uani 1 1 d . . .
H8 H 0.3716 0.2226 0.1118 0.040 Uiso 1 1 calc R . .
C9 C 0.4518(7) 0.1212(5) 0.1504(4) 0.0377(19) Uani 1 1 d . . .
H9 H 0.5245 0.1367 0.1380 0.045 Uiso 1 1 calc R . .
C10 C 0.4382(7) 0.0467(5) 0.1833(4) 0.0369(19) Uani 1 1 d . . .
H10 H 0.5008 0.0125 0.1938 0.044 Uiso 1 1 calc R . .
C11 C 0.3290(7) 0.0235(4) 0.2006(4) 0.0343(18) Uani 1 1 d . . .
H11 H 0.3185 -0.0273 0.2219 0.041 Uiso 1 1 calc R . .
C12 C 0.2350(6) 0.0752(4) 0.1866(3) 0.0239(15) Uani 1 1 d . . .
H12 H 0.1622 0.0587 0.1980 0.029 Uiso 1 1 calc R . .
C13 C -0.1563(6) 0.3728(4) 0.1142(3) 0.0217(15) Uani 1 1 d . . .
C14 C -0.1841(6) 0.3003(5) 0.0784(3) 0.0306(17) Uani 1 1 d . . .
H14 H -0.1281 0.2723 0.0555 0.037 Uiso 1 1 calc R . .
C15 C -0.2941(7) 0.2701(5) 0.0769(4) 0.038(2) Uani 1 1 d . . .
H15 H -0.3116 0.2213 0.0532 0.045 Uiso 1 1 calc R . .
C16 C -0.3791(7) 0.3108(5) 0.1097(4) 0.040(2) Uani 1 1 d . . .
H16 H -0.4535 0.2900 0.1079 0.048 Uiso 1 1 calc R . .
C17 C -0.3527(6) 0.3827(5) 0.1451(4) 0.0360(19) Uani 1 1 d . . .
H17 H -0.4098 0.4100 0.1676 0.043 Uiso 1 1 calc R . .
C18 C -0.2409(6) 0.4156(5) 0.1480(3) 0.0286(17) Uani 1 1 d . . .
H18 H -0.2237 0.4645 0.1716 0.034 Uiso 1 1 calc R . .
C19 C 0.1456(6) 0.5211(4) 0.3669(4) 0.0274(16) Uani 1 1 d . . .
C20 C 0.0804(7) 0.5489(5) 0.4197(4) 0.043(2) Uani 1 1 d . . .
H20 H 0.0026 0.5592 0.4117 0.052 Uiso 1 1 calc R . .
C21 C 0.1332(8) 0.5614(6) 0.4859(4) 0.053(2) Uani 1 1 d . . .
H21 H 0.0895 0.5790 0.5214 0.063 Uiso 1 1 calc R . .
C22 C 0.2488(7) 0.5476(5) 0.4976(4) 0.043(2) Uani 1 1 d . . .
H22 H 0.2828 0.5544 0.5412 0.052 Uiso 1 1 calc R . .
C23 C 0.3130(7) 0.5242(5) 0.4457(4) 0.039(2) Uani 1 1 d . . .
H23 H 0.3914 0.5165 0.4538 0.047 Uiso 1 1 calc R . .
C24 C 0.2638(6) 0.5114(5) 0.3802(4) 0.0340(18) Uani 1 1 d . . .
H24 H 0.3099 0.4963 0.3450 0.041 Uiso 1 1 calc R . .
C25 C 0.1592(6) 0.3030(5) 0.3888(3) 0.0270(16) Uani 1 1 d . . .
H25 H 0.1860 0.3574 0.3886 0.032 Uiso 1 1 calc R . .
C26 C 0.1432(7) 0.2656(5) 0.4504(4) 0.0377(19) Uani 1 1 d . . .
H26 H 0.1577 0.2946 0.4910 0.045 Uiso 1 1 calc R . .
C27 C 0.1053(7) 0.1848(5) 0.4514(4) 0.041(2) Uani 1 1 d . . .
H27 H 0.0945 0.1582 0.4927 0.049 Uiso 1 1 calc R . .
C28 C 0.0837(6) 0.1436(5) 0.3903(4) 0.0362(18) Uani 1 1 d . . .
H28 H 0.0575 0.0890 0.3896 0.043 Uiso 1 1 calc R . .
C29 C 0.1018(6) 0.1849(5) 0.3309(4) 0.0332(18) Uani 1 1 d . . .
H29 H 0.0886 0.1568 0.2898 0.040 Uiso 1 1 calc R . .
C30 C 0.2827(7) 0.4128(5) 0.0851(4) 0.042(2) Uani 1 1 d . . .
H30 H 0.2940 0.3556 0.0862 0.051 Uiso 1 1 calc R . .
C31 C 0.3214(7) 0.4573(5) 0.0307(4) 0.043(2) Uani 1 1 d . . .
H31 H 0.3571 0.4298 -0.0040 0.052 Uiso 1 1 calc R . .
C32 C 0.3078(6) 0.5403(5) 0.0277(3) 0.0299(17) Uani 1 1 d . . .
H32 H 0.3335 0.5709 -0.0087 0.036 Uiso 1 1 calc R . .
C33 C 0.2549(7) 0.5780(5) 0.0797(4) 0.040(2) Uani 1 1 d . . .
H33 H 0.2439 0.6352 0.0791 0.048 Uiso 1 1 calc R . .
C34 C 0.2179(6) 0.5319(5) 0.1327(4) 0.0345(18) Uani 1 1 d . . .
H34 H 0.1831 0.5590 0.1679 0.041 Uiso 1 1 calc R . .
C35 C -0.1271(5) 0.2361(4) 0.2287(3) 0.0221(15) Uani 1 1 d . . .
H35 H -0.0915 0.2093 0.1936 0.027 Uiso 1 1 calc R . .
C36 C -0.2324(6) 0.2060(5) 0.2477(4) 0.0289(16) Uani 1 1 d . . .
H36 H -0.2663 0.1603 0.2258 0.035 Uiso 1 1 calc R . .
C37 C -0.2846(6) 0.2454(4) 0.2994(4) 0.0319(17) Uani 1 1 d . . .
H37 H -0.3555 0.2272 0.3129 0.038 Uiso 1 1 calc R . .
C38 C -0.2315(6) 0.3121(5) 0.3314(4) 0.0320(17) Uani 1 1 d . . .
H38 H -0.2656 0.3391 0.3669 0.038 Uiso 1 1 calc R . .
C39 C -0.1279(6) 0.3384(4) 0.3102(4) 0.0298(17) Uani 1 1 d . . .
H39 H -0.0927 0.3834 0.3324 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'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 '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
N1 U1 N2 148.70(17) . .
N1 U1 N3 66.13(17) . .
N2 U1 N3 144.99(16) . .
N1 U1 S2 92.10(13) . .
N2 U1 S2 92.36(13) . .
N3 U1 S2 88.08(13) . .
N1 U1 S3 144.96(13) . .
N2 U1 S3 66.31(12) . .
N3 U1 S3 79.14(12) . .
S2 U1 S3 81.89(5) . .
N1 U1 S1 80.66(12) . .
N2 U1 S1 68.14(12) . .
N3 U1 S1 146.78(12) . .
S2 U1 S1 93.86(5) . .
S3 U1 S1 133.98(5) . .
N1 U1 S4 95.83(13) . .
N2 U1 S4 85.72(12) . .
N3 U1 S4 86.60(13) . .
S2 U1 S4 167.74(5) . .
S3 U1 S4 86.27(5) . .
S1 U1 S4 96.63(5) . .
C1 S1 U1 114.4(2) . .
C7 S2 U1 115.7(2) . .
C13 S3 U1 114.5(2) . .
C19 S4 U1 119.0(2) . .
C25 N1 C29 117.4(6) . .
C25 N1 U1 117.1(4) . .
C29 N1 U1 124.1(5) . .
C30 N2 C34 116.1(6) . .
C30 N2 U1 119.3(5) . .
C34 N2 U1 123.6(4) . .
C39 N3 C35 116.3(6) . .
C39 N3 U1 121.8(5) . .
C35 N3 U1 121.9(4) . .
C6 C1 C2 118.6(6) . .
C6 C1 S1 123.4(5) . .
C2 C1 S1 118.1(5) . .
C1 C2 C3 120.2(7) . .
C4 C3 C2 119.8(7) . .
C3 C4 C5 121.2(7) . .
C4 C5 C6 119.3(7) . .
C1 C6 C5 121.0(7) . .
C12 C7 C8 119.0(6) . .
C12 C7 S2 120.9(5) . .
C8 C7 S2 120.1(5) . .
C9 C8 C7 120.0(7) . .
C8 C9 C10 121.6(7) . .
C9 C10 C11 118.7(7) . .
C10 C11 C12 121.1(7) . .
C11 C12 C7 119.6(6) . .
C14 C13 C18 120.1(6) . .
C14 C13 S3 120.8(5) . .
C18 C13 S3 119.1(5) . .
C15 C14 C13 120.0(7) . .
C14 C15 C16 121.3(8) . .
C17 C16 C15 119.2(7) . .
C16 C17 C18 121.3(7) . .
C13 C18 C17 118.2(7) . .
C20 C19 C24 118.1(7) . .
C20 C19 S4 119.1(6) . .
C24 C19 S4 122.7(6) . .
C19 C20 C21 119.9(8) . .
C22 C21 C20 120.1(8) . .
C23 C22 C21 120.0(8) . .
C22 C23 C24 121.2(8) . .
C23 C24 C19 120.5(7) . .
N1 C25 C26 122.7(7) . .
C25 C26 C27 119.1(7) . .
C26 C27 C28 119.1(7) . .
C29 C28 C27 118.5(7) . .
N1 C29 C28 123.2(7) . .
N2 C30 C31 122.8(7) . .
C32 C31 C30 120.4(8) . .
C31 C32 C33 117.8(7) . .
C32 C33 C34 120.2(7) . .
N2 C34 C33 122.8(7) . .
N3 C35 C36 123.3(6) . .
C37 C36 C35 118.3(7) . .
C36 C37 C38 119.4(7) . .
C39 C38 C37 119.2(7) . .
N3 C39 C38 123.4(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 2.563(5) .
U1 N2 2.598(5) .
U1 N3 2.629(5) .
U1 S2 2.7169(17) .
U1 S3 2.7298(16) .
U1 S1 2.7298(17) .
U1 S4 2.7639(17) .
S1 C1 1.776(7) .
S2 C7 1.775(7) .
S3 C13 1.778(7) .
S4 C19 1.725(7) .
N1 C25 1.336(8) .
N1 C29 1.349(9) .
N2 C30 1.332(9) .
N2 C34 1.355(9) .
N3 C39 1.350(9) .
N3 C35 1.353(8) .
C1 C6 1.374(9) .
C1 C2 1.401(9) .
C2 C3 1.402(9) .
C3 C4 1.366(10) .
C4 C5 1.368(10) .
C5 C6 1.406(9) .
C7 C12 1.396(9) .
C7 C8 1.405(9) .
C8 C9 1.375(10) .
C9 C10 1.377(10) .
C10 C11 1.388(10) .
C11 C12 1.394(10) .
C13 C14 1.391(9) .
C13 C18 1.402(9) .
C14 C15 1.373(10) .
C15 C16 1.380(11) .
C16 C17 1.375(11) .
C17 C18 1.408(9) .
C19 C20 1.393(10) .
C19 C24 1.400(10) .
C20 C21 1.421(11) .
C21 C22 1.375(11) .
C22 C23 1.351(11) .
C23 C24 1.393(10) .
C25 C26 1.372(10) .
C26 C27 1.375(11) .
C27 C28 1.381(11) .
C28 C29 1.369(10) .
C30 C31 1.383(10) .
C31 C32 1.346(10) .
C32 C33 1.365(10) .
C33 C34 1.366(10) .
C35 C36 1.391(9) .
C36 C37 1.369(10) .
C37 C38 1.375(10) .
C38 C39 1.368(10) .
