#------------------------------------------------------------------------------
#$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $
#$Revision: 130086 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/72/4117292.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_4117292
loop_
_publ_author_name
'Nathan A. Siladke'
'Katie R. Meihaus'
'Joseph W. Ziller'
'Ming Fang'
'Filipp Furche'
'Jeffrey R. Long'
'William J. Evans'
_publ_section_title
;
 Synthesis, Structure, and Magnetism of an f Element Nitrosyl Complex,
 (C5Me4H)3UNO
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1243
_journal_page_last               1249
_journal_paper_doi               10.1021/ja2096128
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C27 H39 N O U'
_chemical_formula_weight         631.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4239(7)
_cell_length_b                   13.4239(7)
_cell_length_c                   13.4239(7)
_cell_measurement_reflns_used    8469
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.63
_cell_volume                     2419.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21558
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    6.728
_exptl_absorpt_correction_T_max  0.3772
_exptl_absorpt_correction_T_min  0.3323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.034(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+2.1163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0339
_refine_ls_wR_factor_ref         0.0342
_reflns_number_gt                1940
_reflns_number_total             1993
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    ja2096128_si_002.cif
_[local]_cod_data_source_block   nas35
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4117292
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/2, -z, x+1/2'
'z+1/2, -x+1/2, -y'
'-y, z+1/2, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, 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 0.247157(5) 0.247157(5) 0.247157(5) 0.00982(4) Uani 1 3 d S
N1 N 0.33375(17) 0.33375(17) 0.33375(17) 0.0155(9) Uani 1 3 d S
O1 O 0.38668(15) 0.38668(15) 0.38668(15) 0.0194(8) Uani 1 3 d S
C1 C 0.3016(2) 0.1358(2) 0.4111(2) 0.0160(6) Uani 1 1 d .
C2 C 0.2034(2) 0.1667(2) 0.4355(2) 0.0160(7) Uani 1 1 d .
C3 C 0.1356(2) 0.1172(2) 0.3706(2) 0.0148(6) Uani 1 1 d .
C4 C 0.1925(2) 0.0587(2) 0.3036(2) 0.0155(6) Uani 1 1 d .
C5 C 0.2942(2) 0.0706(2) 0.3295(2) 0.0150(6) Uani 1 1 d .
H5A H 0.3487 0.0393 0.2969 0.018 Uiso 1 1 calc R
C6 C 0.3936(2) 0.1572(3) 0.4715(3) 0.0224(7) Uani 1 1 d .
H6A H 0.3871 0.1265 0.5374 0.034 Uiso 1 1 calc R
H6B H 0.4015 0.2294 0.4790 0.034 Uiso 1 1 calc R
H6C H 0.4520 0.1297 0.4375 0.034 Uiso 1 1 calc R
C7 C 0.1771(2) 0.2315(2) 0.5236(2) 0.0232(7) Uani 1 1 d .
H7A H 0.1789 0.1915 0.5846 0.035 Uiso 1 1 calc R
H7B H 0.1101 0.2590 0.5144 0.035 Uiso 1 1 calc R
H7C H 0.2253 0.2861 0.5288 0.035 Uiso 1 1 calc R
C8 C 0.0239(2) 0.1101(2) 0.3835(2) 0.0206(6) Uani 1 1 d .
H8A H -0.0092 0.1362 0.3240 0.031 Uiso 1 1 calc R
H8B H 0.0036 0.1492 0.4418 0.031 Uiso 1 1 calc R
H8C H 0.0049 0.0403 0.3933 0.031 Uiso 1 1 calc R
C9 C 0.1486(2) -0.0125(2) 0.2279(3) 0.0240(7) Uani 1 1 d .
H9A H 0.1866 -0.0748 0.2282 0.036 Uiso 1 1 calc R
H9B H 0.1519 0.0176 0.1614 0.036 Uiso 1 1 calc R
H9C H 0.0790 -0.0263 0.2449 0.036 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.00982(4) 0.00982(4) 0.00982(4) 0.00009(6) 0.00009(6) 0.00009(6)
N1 0.0155(9) 0.0155(9) 0.0155(9) -0.0015(9) -0.0015(9) -0.0015(9)
O1 0.0194(8) 0.0194(8) 0.0194(8) -0.0040(8) -0.0040(8) -0.0040(8)
C1 0.0184(15) 0.0164(16) 0.0132(14) 0.0059(12) -0.0026(12) -0.0012(12)
C2 0.0195(15) 0.0163(15) 0.0123(14) 0.0020(11) -0.0004(11) -0.0032(11)
C3 0.0173(14) 0.0134(14) 0.0136(14) 0.0029(11) 0.0012(11) -0.0024(10)
C4 0.0179(16) 0.0118(14) 0.0167(16) 0.0012(11) -0.0005(12) -0.0033(11)
C5 0.0165(15) 0.0114(13) 0.0171(15) 0.0048(12) 0.0010(11) 0.0014(11)
C6 0.0213(16) 0.0251(17) 0.0208(16) 0.0057(13) -0.0063(13) -0.0053(13)
C7 0.0317(17) 0.0227(16) 0.0152(13) -0.0009(13) 0.0023(12) 0.0000(14)
C8 0.0169(15) 0.0219(16) 0.0229(17) 0.0065(13) 0.0021(12) -0.0044(13)
C9 0.0254(15) 0.0186(14) 0.0280(17) -0.0030(13) 0.0001(14) -0.0050(12)
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'
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
Cnt U1 N1 96.5 . .
Cnt U1 Cnt 118.8 . .
N1 U1 C5 97.82(6) . .
N1 U1 C5 97.82(6) . 3
C5 U1 C5 118.18(3) . 3
N1 U1 C5 97.82(7) . 2
C5 U1 C5 118.18(3) . 2
C5 U1 C5 118.18(3) 3 2
N1 U1 C4 121.86(7) . .
C5 U1 C4 30.24(9) . .
C5 U1 C4 94.51(9) 3 .
C5 U1 C4 124.76(9) 2 .
N1 U1 C4 121.86(7) . 3
C5 U1 C4 124.75(9) . 3
C5 U1 C4 30.24(9) 3 3
C5 U1 C4 94.51(9) 2 3
C4 U1 C4 94.71(9) . 3
N1 U1 C4 121.86(7) . 2
C5 U1 C4 94.51(9) . 2
C5 U1 C4 124.76(9) 3 2
C5 U1 C4 30.24(9) 2 2
C4 U1 C4 94.71(9) . 2
C4 U1 C4 94.71(9) 3 2
N1 U1 C1 72.51(6) . .
C5 U1 C1 29.86(9) . .
C5 U1 C1 105.60(10) 3 .
C5 U1 C1 136.13(9) 2 .
C4 U1 C1 49.47(9) . .
C4 U1 C1 127.43(9) 3 .
C4 U1 C1 121.19(10) 2 .
N1 U1 C1 72.51(6) . 2
C5 U1 C1 105.60(10) . 2
C5 U1 C1 136.13(9) 3 2
C5 U1 C1 29.86(9) 2 2
C4 U1 C1 127.43(9) . 2
C4 U1 C1 121.19(10) 3 2
C4 U1 C1 49.47(9) 2 2
C1 U1 C1 111.38(6) . 2
N1 U1 C1 72.51(6) . 3
C5 U1 C1 136.13(9) . 3
C5 U1 C1 29.86(9) 3 3
C5 U1 C1 105.60(10) 2 3
C4 U1 C1 121.19(10) . 3
C4 U1 C1 49.47(9) 3 3
C4 U1 C1 127.43(9) 2 3
C1 U1 C1 111.38(6) . 3
C1 U1 C1 111.38(6) 2 3
N1 U1 C2 79.81(6) . .
C5 U1 C2 48.79(9) . .
C5 U1 C2 76.28(9) 3 .
C5 U1 C2 165.53(9) 2 .
C4 U1 C2 48.77(9) . .
C4 U1 C2 98.86(10) 3 .
C4 U1 C2 141.73(10) 2 .
C1 U1 C2 29.53(9) . .
C1 U1 C2 139.09(9) 2 .
C1 U1 C2 87.41(9) 3 .
N1 U1 C2 79.81(6) . 3
C5 U1 C2 165.53(9) . 3
C5 U1 C2 48.79(9) 3 3
C5 U1 C2 76.28(9) 2 3
C4 U1 C2 141.73(10) . 3
C4 U1 C2 48.77(9) 3 3
C4 U1 C2 98.86(10) 2 3
C1 U1 C2 139.09(9) . 3
C1 U1 C2 87.41(9) 2 3
C1 U1 C2 29.53(9) 3 3
C2 U1 C2 116.94(4) . 3
N1 U1 C2 79.81(6) . 2
C5 U1 C2 76.28(9) . 2
C5 U1 C2 165.53(9) 3 2
C5 U1 C2 48.79(9) 2 2
C4 U1 C2 98.86(10) . 2
C4 U1 C2 141.73(10) 3 2
C4 U1 C2 48.77(9) 2 2
C1 U1 C2 87.41(9) . 2
C1 U1 C2 29.53(9) 2 2
C1 U1 C2 139.09(9) 3 2
C2 U1 C2 116.94(4) . 2
C2 U1 C2 116.94(4) 3 2
N1 U1 C3 108.83(5) . 2
C5 U1 C3 69.54(9) . 2
C5 U1 C3 151.24(8) 3 2
C5 U1 C3 48.80(9) 2 2
C4 U1 C3 80.75(8) . 2
C4 U1 C3 121.40(9) 3 2
C4 U1 C3 29.39(8) 2 2
C1 U1 C3 92.86(9) . 2
C1 U1 C3 48.69(8) 2 2
C1 U1 C3 154.33(9) 3 2
C2 U1 C3 118.23(9) . 2
C2 U1 C3 124.82(9) 3 2
C2 U1 C3 29.22(8) 2 2
N1 U1 C3 108.83(5) . 3
C5 U1 C3 151.24(8) . 3
C5 U1 C3 48.80(9) 3 3
C5 U1 C3 69.54(9) 2 3
C4 U1 C3 121.40(9) . 3
C4 U1 C3 29.39(8) 3 3
C4 U1 C3 80.75(8) 2 3
C1 U1 C3 154.33(9) . 3
C1 U1 C3 92.86(9) 2 3
C1 U1 C3 48.69(8) 3 3
C2 U1 C3 124.82(9) . 3
C2 U1 C3 29.22(8) 3 3
C2 U1 C3 118.23(9) 2 3
C3 U1 C3 110.10(5) 2 3
N1 U1 C3 108.83(5) . .
C5 U1 C3 48.80(9) . .
C5 U1 C3 69.54(9) 3 .
C5 U1 C3 151.24(8) 2 .
C4 U1 C3 29.39(8) . .
C4 U1 C3 80.75(8) 3 .
C4 U1 C3 121.40(9) 2 .
C1 U1 C3 48.69(8) . .
C1 U1 C3 154.33(9) 2 .
C1 U1 C3 92.86(9) 3 .
C2 U1 C3 29.22(8) . .
C2 U1 C3 118.23(9) 3 .
C2 U1 C3 124.82(9) 2 .
C3 U1 C3 110.10(5) 2 .
C3 U1 C3 110.10(5) 3 .
O1 N1 U1 180.0(4) . .
C5 C1 C2 107.2(3) . .
C5 C1 C6 126.6(3) . .
C2 C1 C6 125.5(3) . .
C5 C1 U1 72.39(16) . .
C2 C1 U1 77.28(18) . .
C6 C1 U1 122.9(2) . .
C1 C2 C3 108.3(3) . .
C1 C2 C7 124.5(3) . .
C3 C2 C7 126.8(3) . .
C1 C2 U1 73.19(18) . .
C3 C2 U1 76.24(16) . .
C7 C2 U1 122.1(2) . .
C4 C3 C2 107.7(3) . .
C4 C3 C8 124.9(3) . .
C2 C3 C8 126.3(3) . .
C4 C3 U1 71.67(16) . .
C2 C3 U1 74.53(16) . .
C8 C3 U1 129.04(19) . .
C3 C4 C5 107.5(3) . .
C3 C4 C9 124.5(3) . .
C5 C4 C9 127.6(3) . .
C3 C4 U1 78.94(17) . .
C5 C4 U1 72.94(18) . .
C9 C4 U1 120.1(2) . .
C1 C5 C4 109.2(3) . .
C1 C5 U1 77.75(17) . .
C4 C5 U1 76.82(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
U1 Cnt 2.491
U1 N1 2.013(4)
U1 C5 2.691(3)
U1 C4 2.741(3)
U1 C1 2.759(3)
U1 C2 2.812(3)
U1 C3 2.834(3)
N1 O1 1.231(5)
C1 C5 1.406(4)
C1 C2 1.421(4)
C1 C6 1.505(4)
C2 C3 1.424(4)
C2 C7 1.509(4)
C3 C4 1.417(4)
C3 C8 1.513(4)
C4 C5 1.417(4)
C4 C9 1.515(4)