#------------------------------------------------------------------------------
#$Date: 2016-03-22 14:03:27 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178984 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/07/4120741.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_4120741
loop_
_publ_author_name
'Andrew J. Lewis'
'Patrick J. Carroll'
'Eric J. Schelter'
_publ_section_title
;
 Stable Uranium(VI) Methyl and Acetylide Complexes and the Elucidation of
 an Inverse Trans Influence Ligand Series
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13185
_journal_page_last               13192
_journal_paper_doi               10.1021/ja406610r
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C19 H57 N3 Si6 U'
_chemical_formula_weight         734.25
_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                   18.476(4)
_cell_length_b                   18.476(4)
_cell_length_c                   16.940(4)
_cell_measurement_temperature    143(1)
_cell_volume                     5007.9(19)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35192
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    5.088
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.113
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.361
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.386
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2502
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.386
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0210
_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)+(0.0483P)²+4.8960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                2407
_reflns_number_total             2502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406610r_si_002_3.cif
_cod_data_source_block           4405
_cod_original_cell_volume        5008.1(19)
_cod_original_sg_symbol_H-M      'R 3 c '
_cod_database_code               4120741
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
U1 U 0.6667 0.3333 0.30688(8) 0.02417(10) Uani 1 3 d S
Si1 Si 0.75566(9) 0.52652(13) 0.21084(10) 0.0257(3) Uani 1 1 d .
Si2 Si 0.85351(6) 0.51122(5) 0.34570(7) 0.02657(19) Uani 1 1 d .
N1 N 0.76599(17) 0.46749(17) 0.28491(16) 0.0232(5) Uani 1 1 d .
C1 C 0.6667 0.3333 0.4515(9) 0.038(3) Uani 1 3 d S
H1a H 0.6101 0.3058 0.4704 0.057 Uiso 0.33 1 calc PR
H1b H 0.6957 0.3899 0.4704 0.057 Uiso 0.33 1 calc PR
H1c H 0.6942 0.3043 0.4704 0.057 Uiso 0.33 1 calc PR
C2 C 0.6519(3) 0.4628(3) 0.1598(2) 0.0432(10) Uani 1 1 d .
H2a H 0.6464 0.4109 0.1423 0.065 Uiso 1 1 calc R
H2b H 0.6489 0.4933 0.1152 0.065 Uiso 1 1 calc R
H2c H 0.6076 0.4518 0.1960 0.065 Uiso 1 1 calc R
C3 C 0.7622(3) 0.6239(3) 0.2493(3) 0.0429(9) Uani 1 1 d .
H3a H 0.7208 0.6100 0.2896 0.064 Uiso 1 1 calc R
H3b H 0.7523 0.6525 0.2070 0.064 Uiso 1 1 calc R
H3c H 0.8167 0.6594 0.2710 0.064 Uiso 1 1 calc R
C4 C 0.8339(3) 0.5575(2) 0.1294(2) 0.0367(8) Uani 1 1 d .
H4a H 0.8891 0.5912 0.1504 0.055 Uiso 1 1 calc R
H4b H 0.8234 0.5890 0.0905 0.055 Uiso 1 1 calc R
H4c H 0.8292 0.5083 0.1053 0.055 Uiso 1 1 calc R
C5 C 0.8412(3) 0.5672(3) 0.4319(3) 0.0453(10) Uani 1 1 d .
H5a H 0.8365 0.6138 0.4135 0.068 Uiso 1 1 calc R
H5b H 0.8890 0.5869 0.4658 0.068 Uiso 1 1 calc R
H5c H 0.7917 0.5296 0.4607 0.068 Uiso 1 1 calc R
C6 C 0.9512(2) 0.5892(3) 0.2934(2) 0.0380(9) Uani 1 1 d .
H6a H 0.9588 0.5640 0.2469 0.057 Uiso 1 1 calc R
H6b H 0.9983 0.6066 0.3279 0.057 Uiso 1 1 calc R
H6c H 0.9465 0.6368 0.2787 0.057 Uiso 1 1 calc R
C7 C 0.8735(6) 0.4273(4) 0.3841(5) 0.0408(16) Uani 1 1 d .
H7a H 0.8213 0.3763 0.3906 0.061 Uiso 1 1 calc R
H7b H 0.9016 0.4442 0.4341 0.061 Uiso 1 1 calc R
H7c H 0.9078 0.4185 0.3473 0.061 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'
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 N1 117.34(4) 3_665 .
N1 U1 N1 117.34(4) 3_665 2_655
N1 U1 N1 117.34(4) . 2_655
N1 U1 C1 99.48(8) 3_665 .
N1 U1 C1 99.48(8) . .
N1 U1 C1 99.48(8) 2_655 .
N1 U1 Si2 26.54(7) 3_665 3_665
N1 U1 Si2 137.62(7) . 3_665
N1 U1 Si2 104.51(7) 2_655 3_665
C1 U1 Si2 78.96(3) . 3_665
N1 U1 Si2 104.51(7) 3_665 .
N1 U1 Si2 26.54(7) . .
N1 U1 Si2 137.62(7) 2_655 .
C1 U1 Si2 78.96(3) . .
Si2 U1 Si2 116.43(2) 3_665 .
N1 U1 Si2 137.62(7) 3_665 2_655
N1 U1 Si2 104.51(7) . 2_655
N1 U1 Si2 26.54(7) 2_655 2_655
C1 U1 Si2 78.96(3) . 2_655
Si2 U1 Si2 116.43(2) 3_665 2_655
Si2 U1 Si2 116.43(2) . 2_655
N1 Si1 C3 112.4(2) . .
N1 Si1 C4 114.57(16) . .
C3 Si1 C4 107.2(2) . .
N1 Si1 C2 109.65(19) . .
C3 Si1 C2 108.6(2) . .
C4 Si1 C2 104.0(2) . .
N1 Si2 C5 112.19(17) . .
N1 Si2 C6 113.06(16) . .
C5 Si2 C6 106.3(2) . .
N1 Si2 C7 110.0(3) . .
C5 Si2 C7 108.3(3) . .
C6 Si2 C7 106.6(3) . .
N1 Si2 U1 35.49(9) . .
C5 Si2 U1 109.68(15) . .
C6 Si2 U1 139.92(13) . .
C7 Si2 U1 78.2(3) . .
Si1 N1 Si2 120.37(17) . .
Si1 N1 U1 121.65(15) . .
Si2 N1 U1 117.97(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 2.259(3) 3_665
U1 N1 2.259(3) .
U1 N1 2.259(3) 2_655
U1 C1 2.450(15) .
U1 Si2 3.4361(12) 3_665
U1 Si2 3.4361(12) .
U1 Si2 3.4361(12) 2_655
Si1 N1 1.734(3) .
Si1 C3 1.860(5) .
Si1 C4 1.869(4) .
Si1 C2 1.884(4) .
Si2 N1 1.738(3) .
Si2 C5 1.868(4) .
Si2 C6 1.875(4) .
Si2 C7 1.881(6) .
