#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:16:32 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179529 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/26/4342611.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_4342611
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            'C34 H86 F6 N4 O8 S2 Si8 U2'
_chemical_formula_weight         1557.97
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.187(5)
_cell_angle_beta                 104.462(5)
_cell_angle_gamma                114.001(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8587(10)
_cell_length_b                   11.9910(10)
_cell_length_c                   12.5171(9)
_cell_measurement_reflns_used    85800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.49
_cell_volume                     1554.7(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 φ and 13 ω scans with 2° steps (743 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  0.0450
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            85800
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.482
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.096
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0478
_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)+(0.0705P)²+5.7227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                5280
_reflns_number_total             5913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00034_si_001.cif
_cod_data_source_block           6
_cod_database_code               4342611
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.02384(3) 0.34992(2) 0.29390(2) 0.03184(12) Uani 1 1 d .
S1 S -0.17103(19) 0.50307(18) 0.38834(16) 0.0353(4) Uani 1 1 d .
Si1 Si -0.2235(2) 0.2044(2) 0.10933(18) 0.0378(5) Uani 1 1 d .
Si2 Si -0.2639(2) 0.0908(2) 0.3226(2) 0.0407(5) Uani 1 1 d .
Si3 Si 0.2056(2) 0.1930(2) 0.32902(19) 0.0423(5) Uani 1 1 d .
Si4 Si 0.2227(2) 0.3185(2) 0.12809(19) 0.0409(5) Uani 1 1 d .
O1 O -0.0726(5) 0.4887(5) 0.3482(5) 0.0391(12) Uani 1 1 d .
O2 O -0.1163(6) 0.5817(5) 0.4974(4) 0.0409(13) Uani 1 1 d .
O3 O -0.2855(6) 0.3942(5) 0.3765(5) 0.0481(14) Uani 1 1 d .
O4 O 0.1795(5) 0.5654(5) 0.3030(5) 0.0404(12) Uani 1 1 d .
N1 N -0.1693(6) 0.1949(6) 0.2521(5) 0.0345(14) Uani 1 1 d .
N2 N 0.1643(6) 0.2911(6) 0.2447(5) 0.0366(14) Uani 1 1 d .
F1 F -0.1188(6) 0.7069(5) 0.3022(5) 0.0610(15) Uani 1 1 d .
F2 F -0.3081(6) 0.6250(6) 0.3246(5) 0.0647(15) Uani 1 1 d .
F3 F -0.2666(7) 0.5429(6) 0.1916(4) 0.0707(17) Uani 1 1 d .
C1 C -0.0832(9) 0.3475(8) 0.1033(6) 0.0411(18) Uani 1 1 d .
H1A H -0.1034 0.4193 0.0917 0.049 Uiso 1 1 calc R
H1B H -0.0388 0.3355 0.0496 0.049 Uiso 1 1 calc R
C2 C -0.2459(11) 0.0627(9) 0.0212(8) 0.058(2) Uani 1 1 d .
H2A H -0.1663 0.0516 0.0422 0.087 Uiso 1 1 calc R
H2B H -0.2666 0.0722 -0.0578 0.087 Uiso 1 1 calc R
H2C H -0.3167 -0.0097 0.0331 0.087 Uiso 1 1 calc R
C3 C -0.3773(9) 0.2238(10) 0.0705(8) 0.056(2) Uani 1 1 d .
H3A H -0.4497 0.1458 0.0706 0.084 Uiso 1 1 calc R
H3B H -0.3913 0.2472 -0.0042 0.084 Uiso 1 1 calc R
H3C H -0.3711 0.2887 0.1248 0.084 Uiso 1 1 calc R
C4 C -0.1943(9) 0.1438(9) 0.4769(7) 0.049(2) Uani 1 1 d .
H4A H -0.1106 0.1406 0.5021 0.074 Uiso 1 1 calc R
H4B H -0.2531 0.0896 0.5153 0.074 Uiso 1 1 calc R
H4C H -0.1827 0.2288 0.4943 0.074 Uiso 1 1 calc R
C5 C -0.4326(9) 0.0768(9) 0.2903(9) 0.055(2) Uani 1 1 d .
H5A H -0.4302 0.1594 0.2994 0.083 Uiso 1 1 calc R
H5B H -0.4756 0.0281 0.3415 0.083 Uiso 1 1 calc R
H5C H -0.4804 0.0355 0.2132 0.083 Uiso 1 1 calc R
C6 C -0.2751(10) -0.0682(8) 0.2889(9) 0.055(2) Uani 1 1 d .
H6A H -0.3301 -0.1045 0.2122 0.083 Uiso 1 1 calc R
H6B H -0.3125 -0.1205 0.3408 0.083 Uiso 1 1 calc R
H6C H -0.1887 -0.0626 0.2961 0.083 Uiso 1 1 calc R
C7 C 0.3736(9) 0.2705(12) 0.4256(8) 0.065(3) Uani 1 1 d .
H7A H 0.4354 0.2919 0.3819 0.097 Uiso 1 1 calc R
H7B H 0.3885 0.2143 0.4762 0.097 Uiso 1 1 calc R
H7C H 0.3850 0.3459 0.4692 0.097 Uiso 1 1 calc R
C8 C 0.0952(9) 0.1453(8) 0.4193(7) 0.0441(19) Uani 1 1 d .
H8A H 0.1075 0.2185 0.4670 0.066 Uiso 1 1 calc R
H8B H 0.1147 0.0881 0.4663 0.066 Uiso 1 1 calc R
H8C H 0.0055 0.1042 0.3721 0.066 Uiso 1 1 calc R
C9 C 0.1765(14) 0.0437(10) 0.2491(9) 0.070(3) Uani 1 1 d .
H9A H 0.0854 0.0004 0.2057 0.104 Uiso 1 1 calc R
H9B H 0.1984 -0.0081 0.3014 0.104 Uiso 1 1 calc R
H9C H 0.2304 0.0608 0.1983 0.104 Uiso 1 1 calc R
C10 C 0.3881(10) 0.3208(12) 0.1553(10) 0.067(3) Uani 1 1 d .
H10A H 0.4466 0.3792 0.2233 0.101 Uiso 1 1 calc R
H10B H 0.4216 0.3466 0.0918 0.101 Uiso 1 1 calc R
H10C H 0.3817 0.2379 0.1648 0.101 Uiso 1 1 calc R
C11 C 0.1113(10) 0.1971(9) 0.0035(8) 0.056(2) Uani 1 1 d .
H11A H 0.0969 0.1150 0.0232 0.085 Uiso 1 1 calc R
H11B H 0.1503 0.2102 -0.0581 0.085 Uiso 1 1 calc R
H11C H 0.0287 0.2026 -0.0196 0.085 Uiso 1 1 calc R
C12 C 0.2470(10) 0.4727(9) 0.0855(8) 0.053(2) Uani 1 1 d .
H12A H 0.1682 0.4840 0.0778 0.079 Uiso 1 1 calc R
H12B H 0.2669 0.4767 0.0139 0.079 Uiso 1 1 calc R
H12C H 0.3188 0.5382 0.1426 0.079 Uiso 1 1 calc R
C13 C -0.2183(10) 0.6013(9) 0.2958(7) 0.049(2) Uani 1 1 d .
C14 C 0.1500(9) 0.6615(8) 0.2520(8) 0.045(2) Uani 1 1 d .
H14A H 0.1139 0.6983 0.2988 0.054 Uiso 1 1 calc R
H14B H 0.0872 0.6275 0.1768 0.054 Uiso 1 1 calc R
C15 C 0.2757(10) 0.7550(9) 0.2446(9) 0.055(2) Uani 1 1 d .
H15A H 0.2924 0.7338 0.1747 0.066 Uiso 1 1 calc R
H15B H 0.2773 0.8382 0.2468 0.066 Uiso 1 1 calc R
C16 C 0.3729(10) 0.7509(9) 0.3437(10) 0.064(3) Uani 1 1 d .
H16A H 0.3840 0.8067 0.4097 0.077 Uiso 1 1 calc R
H16B H 0.4574 0.7752 0.3290 0.077 Uiso 1 1 calc R
C17 C 0.3174(8) 0.6162(8) 0.3620(8) 0.049(2) Uani 1 1 d .
H17A H 0.3585 0.5707 0.3309 0.058 Uiso 1 1 calc R
H17B H 0.3313 0.6110 0.4426 0.058 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'
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'
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 '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 110.9(2) . .
N1 U1 C1 73.2(3) . .
N2 U1 C1 92.5(3) . .
N1 U1 O4 155.1(2) . .
N2 U1 O4 87.3(2) . .
C1 U1 O4 89.6(2) . .
N1 U1 O2 110.8(2) . 2_566
N2 U1 O2 104.6(2) . 2_566
C1 U1 O2 159.0(2) . 2_566
O4 U1 O2 79.13(18) . 2_566
N1 U1 O1 88.2(2) . .
N2 U1 O1 159.9(2) . .
C1 U1 O1 87.0(2) . .
O4 U1 O1 72.62(18) . .
O2 U1 O1 72.71(18) 2_566 .
O3 S1 O1 116.4(4) . .
O3 S1 O2 115.4(4) . .
O1 S1 O2 111.7(4) . .
O3 S1 C13 106.0(4) . .
O1 S1 C13 102.9(4) . .
O2 S1 C13 102.3(4) . .
N1 Si1 C1 98.4(3) . .
N1 Si1 C2 109.6(4) . .
C1 Si1 C2 113.9(4) . .
N1 Si1 C3 113.8(4) . .
C1 Si1 C3 111.5(4) . .
C2 Si1 C3 109.3(5) . .
N1 Si2 C4 110.2(4) . .
N1 Si2 C5 113.8(4) . .
C4 Si2 C5 104.8(5) . .
N1 Si2 C6 111.0(4) . .
C4 Si2 C6 109.2(5) . .
C5 Si2 C6 107.5(5) . .
N2 Si3 C7 112.9(4) . .
N2 Si3 C8 107.7(4) . .
C7 Si3 C8 106.5(4) . .
N2 Si3 C9 113.6(4) . .
C7 Si3 C9 111.1(6) . .
C8 Si3 C9 104.2(5) . .
N2 Si4 C12 114.0(4) . .
N2 Si4 C11 111.3(4) . .
C12 Si4 C11 107.6(5) . .
N2 Si4 C10 112.2(4) . .
C12 Si4 C10 103.5(5) . .
C11 Si4 C10 107.8(5) . .
S1 O1 U1 149.1(3) . .
S1 O2 U1 160.6(3) . 2_566
C14 O4 C17 109.5(6) . .
C14 O4 U1 126.1(5) . .
C17 O4 U1 124.4(5) . .
Si2 N1 Si1 124.0(4) . .
Si2 N1 U1 137.2(3) . .
Si1 N1 U1 98.6(3) . .
Si3 N2 Si4 117.4(4) . .
Si3 N2 U1 113.5(3) . .
Si4 N2 U1 128.8(4) . .
Si1 C1 U1 89.4(3) . .
Si1 C1 H1A 113.7 . .
U1 C1 H1A 113.7 . .
Si1 C1 H1B 113.7 . .
U1 C1 H1B 113.7 . .
H1A C1 H1B 111.0 . .
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 . .
Si2 C4 H4A 109.5 . .
Si2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si2 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 . .
Si3 C7 H7A 109.5 . .
Si3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si3 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 . .
Si4 C10 H10A 109.5 . .
Si4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Si4 C11 H11A 109.5 . .
Si4 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
Si4 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
Si4 C12 H12A 109.5 . .
Si4 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
Si4 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
F1 C13 F3 109.2(8) . .
F1 C13 F2 108.6(7) . .
F3 C13 F2 108.8(8) . .
F1 C13 S1 111.1(6) . .
F3 C13 S1 109.3(6) . .
F2 C13 S1 109.8(6) . .
O4 C14 C15 104.7(7) . .
O4 C14 H14A 110.8 . .
C15 C14 H14A 110.8 . .
O4 C14 H14B 110.8 . .
C15 C14 H14B 110.8 . .
H14A C14 H14B 108.9 . .
C16 C15 C14 104.9(8) . .
C16 C15 H15A 110.8 . .
C14 C15 H15A 110.8 . .
C16 C15 H15B 110.8 . .
C14 C15 H15B 110.8 . .
H15A C15 H15B 108.9 . .
C15 C16 C17 104.4(8) . .
C15 C16 H16A 110.9 . .
C17 C16 H16A 110.9 . .
C15 C16 H16B 110.9 . .
C17 C16 H16B 110.9 . .
H16A C16 H16B 108.9 . .
O4 C17 C16 105.2(7) . .
O4 C17 H17A 110.7 . .
C16 C17 H17A 110.7 . .
O4 C17 H17B 110.7 . .
C16 C17 H17B 110.7 . .
H17A C17 H17B 108.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 2.200(6) .
U1 N2 2.256(6) .
U1 C1 2.400(8) .
U1 O4 2.468(5) .
U1 O2 2.525(5) 2_566
U1 O1 2.528(5) .
S1 O3 1.418(6) .
S1 O1 1.447(5) .
S1 O2 1.461(5) .
S1 C13 1.833(9) .
Si1 N1 1.767(6) .
Si1 C1 1.862(9) .
Si1 C2 1.876(9) .
Si1 C3 1.877(9) .
Si2 N1 1.742(7) .
Si2 C4 1.870(9) .
Si2 C5 1.874(9) .
Si2 C6 1.881(9) .
Si3 N2 1.744(7) .
Si3 C7 1.871(10) .
Si3 C8 1.871(9) .
Si3 C9 1.874(10) .
Si4 N2 1.753(6) .
Si4 C12 1.872(9) .
Si4 C11 1.879(10) .
Si4 C10 1.894(10) .
O2 U1 2.525(5) 2_566
O4 C14 1.460(10) .
O4 C17 1.463(10) .
F1 C13 1.316(12) .
F2 C13 1.332(11) .
F3 C13 1.324(10) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C14 C15 1.485(12) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.485(15) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C17 1.527(13) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
