#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:03:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178800 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/54/4105408.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_4105408
loop_
_publ_author_name
'William J. Evans'
'Christopher A. Traina'
'Joseph W. Ziller'
_publ_section_title
;
 Synthesis of Heteroleptic Uranium (μ-η6:η6-C6H6)2- Sandwich Complexes
 via Facile Displacement of (η5-C5Me5)1- by Ligands of Lower Hapticity
 and Their Conversion to Heteroleptic Bis(imido) Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17473
_journal_page_last               17481
_journal_paper_doi               10.1021/ja9075259
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C56 H82 O2 U2'
_chemical_formula_weight         1263.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.3839(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0169(17)
_cell_length_b                   17.007(3)
_cell_length_c                   13.543(2)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.20
_cell_volume                     2537.4(7)
_computing_cell_refinement       'Bruker SMART APEX2/SAINT'
_computing_data_collection       'Bruker SMART APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega'
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26811
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    6.413
_exptl_absorpt_correction_T_max  0.6054
_exptl_absorpt_correction_T_min  0.3461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.305
_refine_diff_density_min         -4.523
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0552
_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)+(0.0288P)²+69.1063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                4590
_reflns_number_total             5199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9075259_si_002_2.cif
_cod_data_source_block           cat11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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_original_cell_volume        2537.3(7)
_cod_database_code               4105408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.00928(5) 0.07459(2) 0.37378(3) 0.01612(14) Uani 0.95 1 d P . .
U1B U 0.0610(14) 0.0747(7) 0.3707(8) 0.036(2) Uiso 0.05 1 d P A 2
O1 O -0.1847(7) 0.1133(5) 0.3244(6) 0.0261(18) Uani 1 1 d . . .
C1 C 0.1291(12) 0.0916(8) 0.2055(10) 0.035(3) Uani 1 1 d . . .
C2 C 0.2141(11) 0.0699(8) 0.2806(10) 0.031(3) Uani 1 1 d . . .
C3 C 0.2234(12) 0.1300(8) 0.3447(10) 0.032(3) Uani 1 1 d . . .
C4 C 0.1459(12) 0.1926(8) 0.3170(10) 0.032(3) Uani 1 1 d . . .
C5 C 0.0869(12) 0.1680(8) 0.2282(10) 0.035(3) Uani 1 1 d . . .
C6 C 0.1089(15) 0.0469(11) 0.1124(14) 0.061(5) Uani 1 1 d . . .
H6A H 0.0369 0.0676 0.0782 0.091 Uiso 1 1 calc R . .
H6B H 0.0964 -0.0088 0.1278 0.091 Uiso 1 1 calc R . .
H6C H 0.1799 0.0526 0.0698 0.091 Uiso 1 1 calc R . .
C7 C 0.2918(13) -0.0041(9) 0.2778(12) 0.041(3) Uani 1 1 d . . .
H7A H 0.3419 -0.0069 0.3378 0.061 Uiso 1 1 calc R . .
H7B H 0.3444 -0.0025 0.2198 0.061 Uiso 1 1 calc R . .
H7C H 0.2392 -0.0504 0.2741 0.061 Uiso 1 1 calc R . .
C8 C 0.3203(14) 0.1380(10) 0.4260(11) 0.045(4) Uani 1 1 d . . .
H8A H 0.3379 0.0861 0.4540 0.068 Uiso 1 1 calc R . .
H8B H 0.2903 0.1728 0.4781 0.068 Uiso 1 1 calc R . .
H8C H 0.3945 0.1602 0.3979 0.068 Uiso 1 1 calc R . .
C9 C 0.1481(15) 0.2724(9) 0.3673(15) 0.059(5) Uani 1 1 d . . .
H9A H 0.1093 0.3114 0.3242 0.088 Uiso 1 1 calc R . .
H9B H 0.2324 0.2879 0.3802 0.088 Uiso 1 1 calc R . .
H9C H 0.1041 0.2693 0.4298 0.088 Uiso 1 1 calc R . .
C10 C 0.0028(15) 0.2171(10) 0.1623(12) 0.055(4) Uani 1 1 d . . .
H10A H 0.0382 0.2219 0.0964 0.082 Uiso 1 1 calc R . .
H10B H -0.0072 0.2695 0.1912 0.082 Uiso 1 1 calc R . .
H10C H -0.0766 0.1913 0.1572 0.082 Uiso 1 1 calc R . .
C11 C -0.2924(10) 0.1383(7) 0.2819(8) 0.023(2) Uani 1 1 d . . .
C12 C -0.3432(11) 0.2104(7) 0.3137(10) 0.029(3) Uani 1 1 d . . .
C13 C -0.4481(11) 0.2374(8) 0.2648(9) 0.029(3) Uani 1 1 d . . .
H13 H -0.4819 0.2866 0.2832 0.034 Uiso 1 1 calc R . .
C14 C -0.5039(12) 0.1941(7) 0.1899(8) 0.026(2) Uani 1 1 d . . .
C15 C -0.4569(11) 0.1207(7) 0.1661(9) 0.027(3) Uani 1 1 d . . .
H15 H -0.4978 0.0893 0.1184 0.032 Uiso 1 1 calc R . .
C16 C -0.3512(11) 0.0919(7) 0.2107(9) 0.026(2) Uani 1 1 d . . .
C17 C -0.2941(11) 0.2556(7) 0.4036(10) 0.029(3) Uani 1 1 d . . .
C18 C -0.3045(13) 0.2021(8) 0.4964(10) 0.036(3) Uani 1 1 d . . .
H18A H -0.2645 0.2277 0.5527 0.054 Uiso 1 1 calc R . .
H18B H -0.2651 0.1515 0.4834 0.054 Uiso 1 1 calc R . .
H18C H -0.3903 0.1934 0.5115 0.054 Uiso 1 1 calc R . .
C19 C -0.3666(13) 0.3294(8) 0.4253(10) 0.037(3) Uani 1 1 d . . .
H19A H -0.3765 0.3601 0.3645 0.055 Uiso 1 1 calc R . .
H19B H -0.3236 0.3610 0.4748 0.055 Uiso 1 1 calc R . .
H19C H -0.4467 0.3148 0.4505 0.055 Uiso 1 1 calc R . .
C20 C -0.1616(13) 0.2819(8) 0.3855(12) 0.041(3) Uani 1 1 d . . .
H20A H -0.1612 0.3279 0.3418 0.062 Uiso 1 1 calc R . .
H20B H -0.1165 0.2389 0.3545 0.062 Uiso 1 1 calc R . .
H20C H -0.1231 0.2956 0.4486 0.062 Uiso 1 1 calc R . .
C21 C -0.3093(11) 0.0064(7) 0.1884(10) 0.029(3) Uani 1 1 d . . .
C22 C -0.1755(12) 0.0038(8) 0.1557(12) 0.042(4) Uani 1 1 d . . .
H22A H -0.1596 -0.0458 0.1214 0.063 Uiso 1 1 calc R . .
H22B H -0.1224 0.0079 0.2138 0.063 Uiso 1 1 calc R . .
H22C H -0.1594 0.0479 0.1110 0.063 Uiso 1 1 calc R . .
C23 C -0.3301(13) -0.0442(8) 0.2791(10) 0.034(3) Uani 1 1 d . . .
H23A H -0.4170 -0.0457 0.2939 0.051 Uiso 1 1 calc R . .
H23B H -0.2857 -0.0219 0.3354 0.051 Uiso 1 1 calc R . .
H23C H -0.3010 -0.0977 0.2664 0.051 Uiso 1 1 calc R . .
C24 C -0.3818(12) -0.0295(8) 0.1022(10) 0.033(3) Uani 1 1 d . . .
H24A H -0.3503 -0.0821 0.0875 0.050 Uiso 1 1 calc R . .
H24B H -0.3738 0.0040 0.0438 0.050 Uiso 1 1 calc R . .
H24C H -0.4675 -0.0334 0.1204 0.050 Uiso 1 1 calc R . .
C25 C -0.6149(12) 0.2258(10) 0.1382(11) 0.043(3) Uani 1 1 d . . .
H25A H -0.6869 0.2149 0.1781 0.064 Uiso 1 1 calc R . .
H25B H -0.6238 0.2004 0.0735 0.064 Uiso 1 1 calc R . .
H25C H -0.6064 0.2827 0.1292 0.064 Uiso 1 1 calc R . .
C26 C 0.0744(11) 0.0602(6) 0.5511(8) 0.024(2) Uani 1 1 d . . .
H26 H 0.1218 0.1004 0.5811 0.029 Uiso 1 1 calc R . .
C27 C 0.1306(10) -0.0029(7) 0.4944(9) 0.022(2) Uani 1 1 d . . .
H27 H 0.2166 -0.0071 0.4932 0.027 Uiso 1 1 calc R . .
C28 C 0.0584(11) -0.0590(6) 0.4402(8) 0.023(2) Uani 1 1 d . . .
H28 H 0.0972 -0.0958 0.3981 0.028 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'
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
Cnt1 U1 O1 113.1 . .
Cnt2 U1 O1 118.1 . .
Cnt1 U1 Cnt2 128.7 . .
O1 U1 C27 83.6(3) . 3_556
O1 U1 C28 130.0(4) . .
C27 U1 C28 58.7(4) 3_556 .
O1 U1 C26 129.4(4) . .
C27 U1 C26 59.2(4) 3_556 .
C28 U1 C26 59.0(3) . .
O1 U1 C28 98.1(3) . 3_556
C27 U1 C28 32.5(4) 3_556 3_556
C28 U1 C28 68.2(4) . 3_556
C26 U1 C28 33.0(4) . 3_556
O1 U1 C27 151.8(3) . .
C27 U1 C27 68.2(4) 3_556 .
C28 U1 C27 32.5(4) . .
C26 U1 C27 32.8(4) . .
C28 U1 C27 57.6(4) 3_556 .
O1 U1 C26 98.1(3) . 3_556
C27 U1 C26 32.9(4) 3_556 3_556
C28 U1 C26 33.0(4) . 3_556
C26 U1 C26 69.6(4) . 3_556
C28 U1 C26 58.1(3) 3_556 3_556
C27 U1 C26 58.2(4) . 3_556
O1 U1 C4 104.5(4) . .
C27 U1 C4 151.1(4) 3_556 .
C28 U1 C4 124.6(4) . .
C26 U1 C4 96.3(4) . .
C28 U1 C4 118.7(4) 3_556 .
C27 U1 C4 100.3(4) . .
C26 U1 C4 157.4(4) 3_556 .
O1 U1 C5 87.1(4) . .
C27 U1 C5 170.2(4) 3_556 .
C28 U1 C5 130.8(4) . .
C26 U1 C5 125.8(4) . .
C28 U1 C5 147.1(4) 3_556 .
C27 U1 C5 120.9(4) . .
C26 U1 C5 153.5(4) 3_556 .
C4 U1 C5 30.1(4) . .
O1 U1 C3 133.3(3) . .
C27 U1 C3 139.0(4) 3_556 .
C28 U1 C3 94.9(4) . .
C26 U1 C3 80.7(4) . .
C28 U1 C3 111.9(4) 3_556 .
C27 U1 C3 73.5(4) . .
C26 U1 C3 127.8(4) 3_556 .
C4 U1 C3 29.7(4) . .
C5 U1 C3 48.5(4) . .
O1 U1 C1 102.2(4) . .
C27 U1 C1 157.2(4) 3_556 .
C28 U1 C1 102.8(4) . .
C26 U1 C1 125.6(4) . .
C28 U1 C1 158.5(4) 3_556 .
C27 U1 C1 104.1(4) . .
C26 U1 C1 124.6(4) 3_556 .
C4 U1 C1 49.2(4) . .
C5 U1 C1 29.7(4) . .
C3 U1 C1 47.9(4) . .
O1 U1 C2 131.9(4) . .
C27 U1 C2 140.9(4) 3_556 .
C28 U1 C2 82.9(4) . .
C26 U1 C2 96.2(4) . .
C28 U1 C2 129.1(4) 3_556 .
C27 U1 C2 75.3(4) . .
C26 U1 C2 113.5(4) 3_556 .
C4 U1 C2 48.6(4) . .
C5 U1 C2 48.9(4) . .
C3 U1 C2 28.1(4) . .
C1 U1 C2 29.8(4) . .
C11 O1 U1 173.5(7) . .
C5 C1 C2 107.4(12) . .
C5 C1 C6 127.3(15) . .
C2 C1 C6 124.5(14) . .
C5 C1 U1 74.5(7) . .
C2 C1 U1 75.4(7) . .
C6 C1 U1 124.4(9) . .
C3 C2 C1 108.0(12) . .
C3 C2 C7 127.2(13) . .
C1 C2 C7 124.3(13) . .
C3 C2 U1 75.4(8) . .
C1 C2 U1 74.7(7) . .
C7 C2 U1 122.4(8) . .
C2 C3 C4 111.0(13) . .
C2 C3 C8 125.4(13) . .
C4 C3 C8 122.7(13) . .
C2 C3 U1 76.5(8) . .
C4 C3 U1 74.6(7) . .
C8 C3 U1 124.7(8) . .
C3 C4 C5 105.9(12) . .
C3 C4 C9 123.1(14) . .
C5 C4 C9 130.3(14) . .
C3 C4 U1 75.7(7) . .
C5 C4 U1 75.0(7) . .
C9 C4 U1 122.4(8) . .
C1 C5 C4 107.7(12) . .
C1 C5 C10 125.0(14) . .
C4 C5 C10 127.0(14) . .
C1 C5 U1 75.8(7) . .
C4 C5 U1 74.9(7) . .
C10 C5 U1 119.9(9) . .
O1 C11 C16 120.4(10) . .
O1 C11 C12 118.6(11) . .
C16 C11 C12 121.0(11) . .
C13 C12 C11 117.7(12) . .
C13 C12 C17 119.6(11) . .
C11 C12 C17 122.5(11) . .
C14 C13 C12 121.8(12) . .
C15 C14 C13 118.8(11) . .
C15 C14 C25 121.1(12) . .
C13 C14 C25 120.1(11) . .
C14 C15 C16 121.7(12) . .
C15 C16 C11 118.7(11) . .
C15 C16 C21 119.4(11) . .
C11 C16 C21 121.6(11) . .
C19 C17 C12 112.6(11) . .
C19 C17 C20 106.9(11) . .
C12 C17 C20 110.3(10) . .
C19 C17 C18 106.6(10) . .
C12 C17 C18 108.6(10) . .
C20 C17 C18 111.8(11) . .
C23 C21 C24 108.0(10) . .
C23 C21 C22 111.5(12) . .
C24 C21 C22 105.3(11) . .
C23 C21 C16 109.0(10) . .
C24 C21 C16 111.4(10) . .
C22 C21 C16 111.5(10) . .
C27 C26 C28 117.3(10) . 3_556
C27 C26 U1 74.3(6) . .
C28 C26 U1 74.1(6) 3_556 .
C27 C26 U1 71.2(6) . 3_556
C28 C26 U1 71.3(6) 3_556 3_556
U1 C26 U1 110.4(4) . 3_556
C28 C27 C26 121.3(10) . .
C28 C27 U1 75.5(6) . 3_556
C26 C27 U1 75.9(6) . 3_556
C28 C27 U1 72.1(6) . .
C26 C27 U1 72.9(6) . .
U1 C27 U1 111.8(4) 3_556 .
C27 C28 C26 121.1(11) . 3_556
C27 C28 U1 75.5(6) . .
C26 C28 U1 75.7(6) 3_556 .
C27 C28 U1 72.0(6) . 3_556
C26 C28 U1 72.9(6) 3_556 3_556
U1 C28 U1 111.8(4) . 3_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 Cnt1 2.488 .
U1 Cnt2 2.131 .
U1 O1 2.144(8) .
U1 C27 2.548(11) 3_556
U1 C28 2.553(11) .
U1 C26 2.578(11) .
U1 C28 2.594(11) 3_556
U1 C27 2.597(12) .
U1 C26 2.611(11) 3_556
U1 C4 2.749(12) .
U1 C5 2.749(12) .
U1 C3 2.762(13) .
U1 C1 2.765(13) .
U1 C2 2.774(12) .
O1 C11 1.383(14) .
C1 C5 1.41(2) .
C1 C2 1.426(19) .
C1 C6 1.49(2) .
C2 C3 1.345(19) .
C2 C7 1.522(19) .
C3 C4 1.413(19) .
C3 C8 1.53(2) .
C4 C5 1.43(2) .
C4 C9 1.52(2) .
C5 C10 1.53(2) .
C11 C16 1.400(17) .
C11 C12 1.417(17) .
C12 C13 1.406(18) .
C12 C17 1.535(18) .
C13 C14 1.393(18) .
C14 C15 1.389(17) .
C14 C25 1.506(17) .
C15 C16 1.397(17) .
C16 C21 1.557(16) .
C17 C19 1.517(17) .
C17 C20 1.549(18) .
C17 C18 1.556(18) .
C21 C23 1.518(18) .
C21 C24 1.536(18) .
C21 C22 1.543(17) .
C26 C27 1.460(17) .
C26 C28 1.468(16) 3_556
C26 U1 2.611(11) 3_556
C27 C28 1.440(17) .
C27 U1 2.548(11) 3_556
C28 C26 1.468(16) 3_556
C28 U1 2.594(11) 3_556
