#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:37:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179509 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/06/4340674.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_4340674
loop_
_publ_author_name
'Mullane, Kimberly C.'
'Lewis, Andrew J.'
'Yin, Haolin'
'Carroll, Patrick J.'
'Schelter, Eric J.'
_publ_section_title
;
 Anomalous one-electron processes in the chemistry of uranium nitrogen
 multiple bonds.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9129
_journal_page_last               9139
_journal_paper_doi               10.1021/ic501149u
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C37 H69 N4 Si6 U'
_chemical_formula_weight         976.53
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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                   14.5991(10)
_cell_length_b                   14.5991(10)
_cell_length_c                   46.380(4)
_cell_measurement_temperature    143(1)
_cell_volume                     8560.8(11)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            25970
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    2.993
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2970
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.560
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.635
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         4369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.635
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0278
_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)+(0.0782P)²+152.7262P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                3309
_reflns_number_total             4369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501149u_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

 Adding full bibliography for 4340671--4340680.cif.
;
_cod_original_sg_symbol_H-M      'R -3     '
_cod_database_code               4340674
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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+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, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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+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'
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 0.083878(4) 0.02622(8) Uani 1 3 d S
Si1 Si 0.41404(8) 0.27946(8) 0.07954(2) 0.0350(2) Uani 1 1 d .
Si2 Si 0.45213(9) 0.14571(10) 0.03823(2) 0.0430(3) Uani 1 1 d .
N1 N 0.6667 0.3333 0.12611(10) 0.0297(10) Uani 1 3 d S
N2 N 0.5031(2) 0.2466(2) 0.06410(6) 0.0324(6) Uani 1 1 d .
C1 C 0.6667 0.3333 0.15797(12) 0.0285(11) Uani 1 3 d S
C2 C 0.5869(3) 0.2206(3) 0.16873(7) 0.0289(6) Uani 1 1 d .
C3 C 0.6112(3) 0.1713(3) 0.19055(9) 0.0377(8) Uani 1 1 d .
H3 H 0.6769 0.2067 0.1995 0.050 Uiso 1 1 calc R
C4 C 0.5381(3) 0.0695(3) 0.19902(10) 0.0468(10) Uani 1 1 d .
H4 H 0.5553 0.0368 0.2136 0.062 Uiso 1 1 calc R
C5 C 0.4402(3) 0.0161(3) 0.18610(10) 0.0490(10) Uani 1 1 d .
H5 H 0.3922 -0.0530 0.1915 0.065 Uiso 1 1 calc R
C6 C 0.4134(3) 0.0651(3) 0.16521(9) 0.0475(10) Uani 1 1 d .
H6 H 0.3465 0.0301 0.1569 0.063 Uiso 1 1 calc R
C7 C 0.4866(3) 0.1670(3) 0.15658(8) 0.0391(8) Uani 1 1 d .
H7 H 0.4682 0.1999 0.1424 0.052 Uiso 1 1 calc R
C8 C 0.4847(3) 0.3850(3) 0.10757(8) 0.0391(8) Uani 1 1 d .
H8a H 0.4806 0.3524 0.1259 0.059 Uiso 1 1 calc R
H8b H 0.4521 0.4279 0.1090 0.059 Uiso 1 1 calc R
H8c H 0.5576 0.4284 0.1022 0.059 Uiso 1 1 calc R
C9 C 0.3014(3) 0.1621(3) 0.09734(9) 0.0462(9) Uani 1 1 d .
H9a H 0.2575 0.1124 0.0829 0.069 Uiso 1 1 calc R
H9b H 0.2605 0.1846 0.1083 0.069 Uiso 1 1 calc R
H9c H 0.3286 0.1292 0.1099 0.069 Uiso 1 1 calc R
C10 C 0.3553(4) 0.3372(4) 0.05467(10) 0.0559(12) Uani 1 1 d .
H10a H 0.4106 0.3938 0.0438 0.084 Uiso 1 1 calc R
H10b H 0.3181 0.3638 0.0657 0.084 Uiso 1 1 calc R
H10c H 0.3070 0.2834 0.0417 0.084 Uiso 1 1 calc R
C11 C 0.3933(4) 0.0125(3) 0.05511(11) 0.0593(12) Uani 1 1 d .
H11a H 0.4468 0.0071 0.0657 0.089 Uiso 1 1 calc R
H11b H 0.3653 -0.0407 0.0404 0.089 Uiso 1 1 calc R
H11c H 0.3375 0.0025 0.0680 0.089 Uiso 1 1 calc R
C12 C 0.3452(4) 0.1437(5) 0.01541(11) 0.0640(14) Uani 1 1 d .
H12a H 0.2860 0.1300 0.0274 0.096 Uiso 1 1 calc R
H12b H 0.3233 0.0891 0.0011 0.096 Uiso 1 1 calc R
H12c H 0.3717 0.2109 0.0061 0.096 Uiso 1 1 calc R
C13 C 0.5548(4) 0.1620(4) 0.01175(9) 0.0497(10) Uani 1 1 d .
H13a H 0.5757 0.2246 0.0005 0.074 Uiso 1 1 calc R
H13b H 0.5266 0.1016 -0.0008 0.074 Uiso 1 1 calc R
H13c H 0.6151 0.1683 0.0218 0.074 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 N2 113.90(7) . 2_655
N1 U1 N2 113.90(7) . .
N2 U1 N2 104.70(8) 2_655 .
N1 U1 N2 113.90(7) . 3_665
N2 U1 N2 104.70(8) 2_655 3_665
N2 U1 N2 104.70(8) . 3_665
N1 U1 Si1 93.420(17) . 2_655
N2 U1 Si1 28.34(8) 2_655 2_655
N2 U1 Si1 97.45(8) . 2_655
N2 U1 Si1 132.68(8) 3_665 2_655
N1 U1 Si1 93.420(17) . 3_665
N2 U1 Si1 97.45(8) 2_655 3_665
N2 U1 Si1 132.68(8) . 3_665
N2 U1 Si1 28.34(7) 3_665 3_665
Si1 U1 Si1 119.647(4) 2_655 3_665
N1 U1 Si1 93.420(17) . .
N2 U1 Si1 132.68(8) 2_655 .
N2 U1 Si1 28.34(7) . .
N2 U1 Si1 97.45(8) 3_665 .
Si1 U1 Si1 119.647(4) 2_655 .
Si1 U1 Si1 119.647(4) 3_665 .
N2 Si1 C10 116.23(19) . .
N2 Si1 C9 111.30(18) . .
C10 Si1 C9 107.1(2) . .
N2 Si1 C8 109.20(16) . .
C10 Si1 C8 104.2(2) . .
C9 Si1 C8 108.41(19) . .
N2 Si1 U1 37.95(10) . .
C10 Si1 U1 128.78(18) . .
C9 Si1 U1 123.04(14) . .
C8 Si1 U1 71.29(12) . .
N2 Si2 C13 111.65(17) . .
N2 Si2 C11 111.77(19) . .
C13 Si2 C11 109.5(2) . .
N2 Si2 C12 113.58(19) . .
C13 Si2 C12 103.9(2) . .
C11 Si2 C12 106.0(3) . .
C1 N1 U1 180.0 . .
Si1 N2 Si2 116.77(17) . .
Si1 N2 U1 113.71(14) . .
Si2 N2 U1 129.28(16) . .
N1 C1 C2 108.8(2) . 2_655
N1 C1 C2 108.8(2) . .
C2 C1 C2 110.1(2) 2_655 .
N1 C1 C2 108.8(2) . 3_665
C2 C1 C2 110.1(2) 2_655 3_665
C2 C1 C2 110.1(2) . 3_665
C3 C2 C7 118.3(3) . .
C3 C2 C1 122.4(3) . .
C7 C2 C1 119.3(3) . .
C2 C3 C4 120.3(4) . .
C5 C4 C3 120.6(4) . .
C4 C5 C6 119.9(4) . .
C5 C6 C7 119.7(4) . .
C6 C7 C2 121.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.959(5) .
U1 N2 2.264(3) 2_655
U1 N2 2.264(3) .
U1 N2 2.264(3) 3_665
U1 Si1 3.3706(10) 2_655
U1 Si1 3.3706(10) 3_665
U1 Si1 3.3706(10) .
Si1 N2 1.748(3) .
Si1 C10 1.870(4) .
Si1 C9 1.871(4) .
Si1 C8 1.881(4) .
Si2 N2 1.752(3) .
Si2 C13 1.858(4) .
Si2 C11 1.860(5) .
Si2 C12 1.874(5) .
N1 C1 1.478(7) .
C1 C2 1.548(4) 2_655
C1 C2 1.548(4) .
C1 C2 1.548(4) 3_665
C2 C3 1.387(5) .
C2 C7 1.388(5) .
C3 C4 1.384(5) .
C4 C5 1.377(6) .
C5 C6 1.371(6) .
C6 C7 1.388(5) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 334 37 ' '
2 0.000 0.000 0.500 512 53 ' '
3 0.333 0.667 0.667 336 37 ' '
4 0.333 0.667 0.167 510 53 ' '
5 0.667 0.333 0.333 333 37 ' '
6 0.667 0.333 0.833 508 53 ' '
