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#$Date: 2025-08-21 02:27:06 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301840 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/26/4342613.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_4342613
loop_
_publ_author_name
'Hervé, Alexandre'
'Bouzidi, Yamina'
'Berthet, Jean-Claude'
'Belkhiri, Lotfi'
'Thuéry, Pierre'
'Boucekkine, Abdou'
'Ephritikhine, Michel'
_publ_section_title
;
 U(III)-CN versus U(IV)-NC Coordination in Tris(silylamide) Complexes.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2474
_journal_paper_doi               10.1021/acs.inorgchem.5b00034
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C36 H86 K N5 O4 Si6 U'
_chemical_formula_weight         1098.77
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.710(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.4829(10)
_cell_length_b                   11.9358(7)
_cell_length_c                   24.8150(9)
_cell_measurement_reflns_used    101389
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.21
_cell_volume                     5465.6(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and seven ω scans with 2° steps (498 frames)'
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            101389
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.213
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.169
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         8338
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0438
_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)+(0.0600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                6050
_reflns_number_total             8338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00034_si_001.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4342613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
U1 U 0.5000 0.725489(17) 0.7500 0.03266(8) Uani 1 2 d S
K1 K 0.7500 0.7500 1.0000 0.0644(5) Uani 1 2 d S
Si1 Si 0.62957(6) 0.93002(11) 0.75736(5) 0.0456(3) Uani 1 1 d .
Si2 Si 0.59891(7) 0.77365(11) 0.65769(5) 0.0461(3) Uani 1 1 d .
Si3 Si 0.58031(8) 0.46372(12) 0.77981(8) 0.0644(4) Uani 1 1 d .
O1 O 0.8540(3) 0.8070(5) 0.95159(19) 0.0970(15) Uani 1 1 d .
O2 O 0.7150(4) 0.9716(7) 1.0055(4) 0.181(3) Uani 1 1 d DU
N1 N 0.5859(2) 0.7291(4) 0.84916(18) 0.0573(10) Uani 1 1 d .
N2 N 0.58231(17) 0.8158(3) 0.71953(13) 0.0370(7) Uani 1 1 d .
N3 N 0.5000 0.5371(4) 0.7500 0.0453(12) Uani 1 2 d S
C1 C 0.6286(3) 0.7315(5) 0.8938(2) 0.0582(13) Uani 1 1 d .
C2 C 0.7226(2) 0.8900(5) 0.8029(2) 0.0595(13) Uani 1 1 d .
H2A H 0.7193 0.8368 0.8311 0.089 Uiso 1 1 calc R
H2B H 0.7480 0.9555 0.8215 0.089 Uiso 1 1 calc R
H2C H 0.7482 0.8570 0.7797 0.089 Uiso 1 1 calc R
C3 C 0.5834(3) 0.9898(5) 0.8062(2) 0.0690(15) Uani 1 1 d .
H3A H 0.5630 1.0614 0.7920 0.103 Uiso 1 1 calc R
H3B H 0.6179 0.9987 0.8435 0.103 Uiso 1 1 calc R
H3C H 0.5455 0.9400 0.8080 0.103 Uiso 1 1 calc R
C4 C 0.6367(3) 1.0471(4) 0.7090(2) 0.0585(12) Uani 1 1 d .
H4A H 0.6619 1.0212 0.6839 0.088 Uiso 1 1 calc R
H4B H 0.6628 1.1085 0.7313 0.088 Uiso 1 1 calc R
H4C H 0.5889 1.0716 0.6870 0.088 Uiso 1 1 calc R
C5 C 0.5495(3) 0.8653(5) 0.5957(2) 0.0644(14) Uani 1 1 d .
H5A H 0.4983 0.8544 0.5866 0.097 Uiso 1 1 calc R
H5B H 0.5640 0.8459 0.5634 0.097 Uiso 1 1 calc R
H5C H 0.5612 0.9424 0.6055 0.097 Uiso 1 1 calc R
C6 C 0.5693(3) 0.6249(4) 0.6380(2) 0.0571(12) Uani 1 1 d .
H6A H 0.6006 0.5747 0.6652 0.086 Uiso 1 1 calc R
H6B H 0.5717 0.6087 0.6008 0.086 Uiso 1 1 calc R
H6C H 0.5204 0.6154 0.6381 0.086 Uiso 1 1 calc R
C7 C 0.6984(3) 0.7748(5) 0.6652(3) 0.0635(14) Uani 1 1 d .
H7A H 0.7174 0.8491 0.6746 0.095 Uiso 1 1 calc R
H7B H 0.7046 0.7521 0.6299 0.095 Uiso 1 1 calc R
H7C H 0.7239 0.7239 0.6948 0.095 Uiso 1 1 calc R
C8 C 0.5896(4) 0.4121(6) 0.8534(3) 0.105(3) Uani 1 1 d .
H8A H 0.5932 0.4749 0.8783 0.157 Uiso 1 1 calc R
H8B H 0.6324 0.3669 0.8672 0.157 Uiso 1 1 calc R
H8C H 0.5479 0.3680 0.8522 0.157 Uiso 1 1 calc R
C9 C 0.5883(4) 0.3394(5) 0.7361(4) 0.113(3) Uani 1 1 d .
H9A H 0.5514 0.2859 0.7356 0.170 Uiso 1 1 calc R
H9B H 0.6351 0.3056 0.7524 0.170 Uiso 1 1 calc R
H9C H 0.5826 0.3631 0.6979 0.170 Uiso 1 1 calc R
C10 C 0.6619(2) 0.5532(4) 0.7856(2) 0.0589(12) Uani 1 1 d .
H10A H 0.6878 0.5226 0.7619 0.088 Uiso 1 1 calc R
H10B H 0.6931 0.5545 0.8244 0.088 Uiso 1 1 calc R
H10C H 0.6466 0.6281 0.7734 0.088 Uiso 1 1 calc R
C11 C 0.8708(4) 0.7379(6) 0.9110(3) 0.086(2) Uani 1 1 d .
H11A H 0.8542 0.7726 0.8736 0.104 Uiso 1 1 calc R
H11B H 0.8475 0.6654 0.9087 0.104 Uiso 1 1 calc R
C12 C 0.9519(4) 0.7247(5) 0.9307(3) 0.0806(18) Uani 1 1 d .
H12A H 0.9697 0.7134 0.8988 0.097 Uiso 1 1 calc R
H12B H 0.9672 0.6624 0.9569 0.097 Uiso 1 1 calc R
C13 C 0.9776(4) 0.8355(6) 0.9600(3) 0.0818(17) Uani 1 1 d .
H13A H 1.0221 0.8261 0.9914 0.098 Uiso 1 1 calc R
H13B H 0.9855 0.8898 0.9335 0.098 Uiso 1 1 calc R
C14 C 0.9162(4) 0.8715(7) 0.9809(3) 0.099(2) Uani 1 1 d .
H14A H 0.9291 0.8590 1.0216 0.119 Uiso 1 1 calc R
H14B H 0.9062 0.9506 0.9735 0.119 Uiso 1 1 calc R
C15 C 0.6452(5) 1.0125(9) 0.9861(6) 0.181(3) Uani 1 1 d DU
H15A H 0.6248 1.0137 1.0170 0.217 Uiso 1 1 calc R
H15B H 0.6154 0.9641 0.9564 0.217 Uiso 1 1 calc R
C16 C 0.6455(6) 1.1261(9) 0.9638(5) 0.173(3) Uani 1 1 d DU
H16A H 0.6013 1.1397 0.9325 0.207 Uiso 1 1 calc R
H16B H 0.6489 1.1811 0.9933 0.207 Uiso 1 1 calc R
C17 C 0.7076(6) 1.1335(11) 0.9445(5) 0.181(3) Uani 1 1 d DU
H17A H 0.7262 1.2093 0.9467 0.217 Uiso 1 1 calc R
H17B H 0.6977 1.1046 0.9062 0.217 Uiso 1 1 calc R
C18 C 0.7569(5) 1.0584(11) 0.9883(6) 0.198(3) Uani 1 1 d DU
H18A H 0.7915 1.0235 0.9728 0.238 Uiso 1 1 calc R
H18B H 0.7837 1.1022 1.0212 0.238 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'
Si Si 0.0817 0.0704 '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'
K K 0.2009 0.2494 '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'
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
N3 U1 N2 118.56(9) . 2_656
N3 U1 N2 118.55(9) . .
N2 U1 N2 122.89(18) 2_656 .
N3 U1 N1 90.99(10) . .
N2 U1 N1 89.15(13) 2_656 .
N2 U1 N1 89.91(13) . .
N3 U1 N1 90.99(10) . 2_656
N2 U1 N1 89.91(13) 2_656 2_656
N2 U1 N1 89.14(13) . 2_656
N1 U1 N1 178.0(2) . 2_656
O2 K1 O2 179.998(3) 7_667 .
O2 K1 O1 89.3(2) 7_667 .
O2 K1 O1 90.7(2) . .
O2 K1 O1 90.7(2) 7_667 7_667
O2 K1 O1 89.3(2) . 7_667
O1 K1 O1 179.999(1) . 7_667
O2 K1 C1 91.4(2) 7_667 .
O2 K1 C1 88.6(2) . .
O1 K1 C1 96.95(14) . .
O1 K1 C1 83.05(15) 7_667 .
O2 K1 C1 88.6(2) 7_667 7_667
O2 K1 C1 91.4(2) . 7_667
O1 K1 C1 83.05(15) . 7_667
O1 K1 C1 96.95(14) 7_667 7_667
C1 K1 C1 179.999(1) . 7_667
N2 Si1 C2 111.7(2) . .
N2 Si1 C3 111.6(2) . .
C2 Si1 C3 106.3(2) . .
N2 Si1 C4 111.9(2) . .
C2 Si1 C4 108.8(2) . .
C3 Si1 C4 106.3(3) . .
N2 Si2 C5 111.2(2) . .
N2 Si2 C6 111.9(2) . .
C5 Si2 C6 107.6(2) . .
N2 Si2 C7 112.7(2) . .
C5 Si2 C7 108.4(3) . .
C6 Si2 C7 104.6(2) . .
N3 Si3 C9 112.6(3) . .
N3 Si3 C8 111.8(2) . .
C9 Si3 C8 107.6(4) . .
N3 Si3 C10 111.7(2) . .
C9 Si3 C10 105.5(3) . .
C8 Si3 C10 107.2(3) . .
C11 O1 C14 109.0(6) . .
C11 O1 K1 122.4(5) . .
C14 O1 K1 122.4(4) . .
C15 O2 C18 103.1(6) . .
C15 O2 K1 123.9(7) . .
C18 O2 K1 119.8(7) . .
Si2 N2 Si1 119.0(2) . .
Si3 N3 Si3 119.5(3) 2_656 .
N1 C1 K1 172.5(4) . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si1 C3 H3A 109.5 . .
Si1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si1 C4 H4A 109.5 . .
Si1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si2 C5 H5A 109.5 . .
Si2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si2 C6 H6A 109.5 . .
Si2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si2 C7 H7A 109.5 . .
Si2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si3 C8 H8A 109.5 . .
Si3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si3 C9 H9A 109.5 . .
Si3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
Si3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
Si3 C10 H10A 109.5 . .
Si3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O1 C11 C12 106.7(5) . .
O1 C11 H11A 110.4 . .
C12 C11 H11A 110.4 . .
O1 C11 H11B 110.4 . .
C12 C11 H11B 110.4 . .
H11A C11 H11B 108.6 . .
C11 C12 C13 102.4(6) . .
C11 C12 H12A 111.3 . .
C13 C12 H12A 111.3 . .
C11 C12 H12B 111.3 . .
C13 C12 H12B 111.3 . .
H12A C12 H12B 109.2 . .
C14 C13 C12 103.7(6) . .
C14 C13 H13A 111.0 . .
C12 C13 H13A 111.0 . .
C14 C13 H13B 111.0 . .
C12 C13 H13B 111.0 . .
H13A C13 H13B 109.0 . .
O1 C14 C13 108.0(6) . .
O1 C14 H14A 110.1 . .
C13 C14 H14A 110.1 . .
O1 C14 H14B 110.1 . .
C13 C14 H14B 110.1 . .
H14A C14 H14B 108.4 . .
O2 C15 C16 109.7(8) . .
O2 C15 H15A 109.7 . .
C16 C15 H15A 109.7 . .
O2 C15 H15B 109.7 . .
C16 C15 H15B 109.7 . .
H15A C15 H15B 108.2 . .
C17 C16 C15 106.7(10) . .
C17 C16 H16A 110.4 . .
C15 C16 H16A 110.4 . .
C17 C16 H16B 110.4 . .
C15 C16 H16B 110.4 . .
H16A C16 H16B 108.6 . .
C16 C17 C18 97.7(10) . .
C16 C17 H17A 112.2 . .
C18 C17 H17A 112.2 . .
C16 C17 H17B 112.2 . .
C18 C17 H17B 112.2 . .
H17A C17 H17B 109.8 . .
O2 C18 C17 110.4(8) . .
O2 C18 H18A 109.6 . .
C17 C18 H18A 109.6 . .
O2 C18 H18B 109.6 . .
C17 C18 H18B 109.6 . .
H18A C18 H18B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N3 2.248(5) .
U1 N2 2.254(3) 2_656
U1 N2 2.254(3) .
U1 N1 2.493(4) .
U1 N1 2.493(4) 2_656
K1 O2 2.746(8) 7_667
K1 O2 2.746(8) .
K1 O1 2.752(5) .
K1 O1 2.752(5) 7_667
K1 C1 2.930(5) .
K1 C1 2.930(5) 7_667
Si1 N2 1.742(4) .
Si1 C2 1.864(5) .
Si1 C3 1.867(5) .
Si1 C4 1.876(5) .
Si2 N2 1.741(3) .
Si2 C5 1.881(5) .
Si2 C6 1.882(5) .
Si2 C7 1.887(5) .
Si3 N3 1.738(3) .
Si3 C9 1.874(7) .
Si3 C8 1.880(6) .
Si3 C10 1.883(5) .
O1 C11 1.420(8) .
O1 C14 1.423(8) .
O2 C15 1.378(7) .
O2 C18 1.464(8) .
N1 C1 1.154(7) .
N3 Si3 1.738(3) 2_656
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.505(10) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.515(9) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.512(10) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.465(8) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C17 1.440(8) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 C18 1.495(8) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139142855
