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#$Date: 2016-03-22 12:45:29 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178962 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/91/4119170.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_4119170
loop_
_publ_author_name
'Andrew J. Lewis'
'Patrick J. Carroll'
'Eric J. Schelter'
_publ_section_title
;
 Reductive Cleavage of Nitrite to Form Terminal Uranium Mono-Oxo Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              511
_journal_page_last               518
_journal_paper_doi               10.1021/ja311057y
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C18 H54 Br N3 O Si6 U'
_chemical_formula_weight         815.12
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.5005(9)
_cell_length_b                   18.5005(9)
_cell_length_c                   16.9729(7)
_cell_measurement_temperature    143(1)
_cell_volume                     5031.0(4)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62664
_diffrn_reflns_theta_full        27.68
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    6.260
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.630
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2530
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0245
_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)+(0.0194P)²+24.0844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                2385
_reflns_number_total             2530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311057y_si_002_5.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'R 3 c '
_cod_database_code               4119170
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'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+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'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+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'
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 0.0000 0.0000 0.00080(3) 0.03918(9) Uani 1 3 d S . .
Br1 Br 0.0000 0.0000 0.16171(11) 0.0556(4) Uani 1 3 d S A 1
O1 O 0.0000 0.0000 -0.1111(10) 0.098(4) Uani 0.90 3 d SP A 1
Br1' Br 0.0000 0.0000 -0.170(2) 0.102(7) Uani 0.10 3 d SP A 2
N1 N 0.03423(19) -0.09755(19) -0.01074(17) 0.0244(6) Uani 1 1 d . A .
Si1 Si -0.01095(7) -0.18580(7) 0.05097(8) 0.0287(2) Uani 1 1 d . A .
Si2 Si 0.10558(8) -0.08924(8) -0.08367(8) 0.0292(3) Uani 1 1 d . A .
C1 C 0.0564(3) -0.1714(3) 0.1384(3) 0.0442(11) Uani 1 1 d . . .
H1A H 0.1076 -0.1676 0.1213 0.066 Uiso 1 1 calc R A .
H1B H 0.0277 -0.2182 0.1733 0.066 Uiso 1 1 calc R . .
H1C H 0.0684 -0.1211 0.1655 0.066 Uiso 1 1 calc R . .
C2 C -0.1162(3) -0.2082(4) 0.0855(4) 0.0408(12) Uani 1 1 d . . .
H2A H -0.1204 -0.1588 0.0806 0.061 Uiso 1 1 calc R A .
H2B H -0.1236 -0.2255 0.1396 0.061 Uiso 1 1 calc R . .
H2C H -0.1586 -0.2519 0.0539 0.061 Uiso 1 1 calc R . .
C3 C -0.0285(3) -0.2823(3) -0.0009(3) 0.0387(10) Uani 1 1 d . . .
H3A H -0.0636 -0.2922 -0.0459 0.058 Uiso 1 1 calc R A .
H3B H -0.0549 -0.3290 0.0344 0.058 Uiso 1 1 calc R . .
H3C H 0.0242 -0.2754 -0.0178 0.058 Uiso 1 1 calc R . .
C4 C 0.0559(3) -0.1626(3) -0.1673(3) 0.0425(10) Uani 1 1 d . . .
H4A H 0.0300 -0.2190 -0.1483 0.064 Uiso 1 1 calc R A .
H4B H 0.0976 -0.1539 -0.2057 0.064 Uiso 1 1 calc R . .
H4C H 0.0145 -0.1528 -0.1910 0.064 Uiso 1 1 calc R . .
C5 C 0.1601(5) 0.0175(3) -0.1289(3) 0.076(2) Uani 1 1 d . . .
H5A H 0.1194 0.0309 -0.1482 0.114 Uiso 1 1 calc R A .
H5B H 0.1944 0.0185 -0.1718 0.114 Uiso 1 1 calc R . .
H5C H 0.1944 0.0577 -0.0900 0.114 Uiso 1 1 calc R . .
C6 C 0.1890(3) -0.1057(4) -0.0416(3) 0.0556(14) Uani 1 1 d . . .
H6A H 0.2172 -0.0659 -0.0003 0.083 Uiso 1 1 calc R A .
H6B H 0.2282 -0.0984 -0.0822 0.083 Uiso 1 1 calc R . .
H6C H 0.1646 -0.1612 -0.0207 0.083 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'
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'
Br Br -0.2901 2.4595 '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
O1 U1 N1 84.89(8) . 2
O1 U1 N1 84.89(8) . .
N1 U1 N1 119.22(2) 2 .
O1 U1 N1 84.89(8) . 3
N1 U1 N1 119.22(2) 2 3
N1 U1 N1 119.22(2) . 3
O1 U1 Br1 180.0 . .
N1 U1 Br1 95.11(8) 2 .
N1 U1 Br1 95.11(8) . .
N1 U1 Br1 95.11(8) 3 .
O1 U1 Br1' 0.0 . .
N1 U1 Br1' 84.89(8) 2 .
N1 U1 Br1' 84.89(8) . .
N1 U1 Br1' 84.89(8) 3 .
Br1 U1 Br1' 180.0 . .
O1 U1 Si2 65.36(2) . 3
N1 U1 Si2 129.69(8) 2 3
N1 U1 Si2 98.44(8) . 3
N1 U1 Si2 26.27(8) 3 3
Br1 U1 Si2 114.64(2) . 3
Br1' U1 Si2 65.36(2) . 3
O1 U1 Si2 65.36(2) . 2
N1 U1 Si2 26.27(8) 2 2
N1 U1 Si2 129.69(8) . 2
N1 U1 Si2 98.44(8) 3 2
Br1 U1 Si2 114.64(2) . 2
Br1' U1 Si2 65.36(2) . 2
Si2 U1 Si2 103.84(3) 3 2
O1 U1 Si2 65.36(2) . .
N1 U1 Si2 98.44(8) 2 .
N1 U1 Si2 26.27(8) . .
N1 U1 Si2 129.69(8) 3 .
Br1 U1 Si2 114.64(2) . .
Br1' U1 Si2 65.36(2) . .
Si2 U1 Si2 103.84(3) 3 .
Si2 U1 Si2 103.84(3) 2 .
O1 U1 Si1 104.30(2) . 2
N1 U1 Si1 26.04(8) 2 2
N1 U1 Si1 103.34(8) . 2
N1 U1 Si1 137.19(8) 3 2
Br1 U1 Si1 75.70(2) . 2
Br1' U1 Si1 104.30(2) . 2
Si2 U1 Si1 154.99(3) 3 2
Si2 U1 Si1 52.30(3) 2 2
Si2 U1 Si1 90.82(3) . 2
O1 U1 Si1 104.30(2) . .
N1 U1 Si1 137.19(8) 2 .
N1 U1 Si1 26.04(8) . .
N1 U1 Si1 103.34(8) 3 .
Br1 U1 Si1 75.70(2) . .
Br1' U1 Si1 104.30(2) . .
Si2 U1 Si1 90.82(3) 3 .
Si2 U1 Si1 154.99(3) 2 .
Si2 U1 Si1 52.30(3) . .
Si1 U1 Si1 114.109(18) 2 .
O1 U1 Si1 104.30(2) . 3
N1 U1 Si1 103.34(8) 2 3
N1 U1 Si1 137.19(8) . 3
N1 U1 Si1 26.04(8) 3 3
Br1 U1 Si1 75.70(2) . 3
Br1' U1 Si1 104.30(2) . 3
Si2 U1 Si1 52.30(3) 3 3
Si2 U1 Si1 90.82(3) 2 3
Si2 U1 Si1 154.99(3) . 3
Si1 U1 Si1 114.109(18) 2 3
Si1 U1 Si1 114.109(18) . 3
Si2 N1 Si1 119.17(18) . .
Si2 N1 U1 120.14(16) . .
Si1 N1 U1 120.67(16) . .
N1 Si1 C3 112.42(17) . .
N1 Si1 C1 111.53(19) . .
C3 Si1 C1 107.1(2) . .
N1 Si1 C2 110.5(2) . .
C3 Si1 C2 105.8(2) . .
C1 Si1 C2 109.2(3) . .
N1 Si1 U1 33.29(10) . .
C3 Si1 U1 137.09(14) . .
C1 Si1 U1 110.59(17) . .
C2 Si1 U1 80.45(19) . .
N1 Si2 C4 113.46(18) . .
N1 Si2 C6 111.3(2) . .
C4 Si2 C6 108.8(2) . .
N1 Si2 C5 111.4(2) . .
C4 Si2 C5 105.4(3) . .
C6 Si2 C5 106.0(3) . .
N1 Si2 U1 33.60(10) . .
C4 Si2 U1 118.48(16) . .
C6 Si2 U1 129.51(18) . .
C5 Si2 U1 78.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.899(17) .
U1 N1 2.200(3) 2
U1 N1 2.200(3) .
U1 N1 2.200(3) 3
U1 Br1 2.7311(19) .
U1 Br1' 2.90(4) .
U1 Si2 3.4383(15) 3
U1 Si2 3.4383(15) 2
U1 Si2 3.4383(15) .
U1 Si1 3.4475(11) 2
U1 Si1 3.4475(11) .
U1 Si1 3.4475(11) 3
N1 Si2 1.759(3) .
N1 Si1 1.760(3) .
Si1 C3 1.868(4) .
Si1 C1 1.869(4) .
Si1 C2 1.870(5) .
Si2 C4 1.858(5) .
Si2 C6 1.859(5) .
Si2 C5 1.875(5) .
