#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:03:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178800 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/54/4105407.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_4105407
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            'C40 H74 Si4 U2'
_chemical_formula_weight         1143.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                99.8602(3)
_cell_angle_beta                 104.2888(3)
_cell_angle_gamma                99.0500(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6310(3)
_cell_length_b                   11.2450(3)
_cell_length_c                   12.1742(4)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.28
_cell_volume                     1103.19(6)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12615
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    7.464
_exptl_absorpt_correction_T_max  0.5695
_exptl_absorpt_correction_T_min  0.2674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0132
_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/[σ²(Fo²)+(0.0205P)²+0.4257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0327
_refine_ls_wR_factor_ref         0.0329
_reflns_number_gt                4855
_reflns_number_total             4998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9075259_si_002_1.cif
_cod_data_source_block           cat10
_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_database_code               4105407
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
U1 U 0.689607(7) 0.567114(6) 0.659977(5) 0.01107(3) Uani 1 1 d
Si1 Si 0.61067(7) 0.88634(5) 0.78177(5) 0.01472(10) Uani 1 1 d
Si2 Si 0.90548(6) 0.85563(5) 0.67064(5) 0.01484(10) Uani 1 1 d
C1 C 0.6935(2) 0.40543(18) 0.80489(16) 0.0144(4) Uani 1 1 d
C2 C 0.7980(2) 0.36865(17) 0.73810(16) 0.0145(4) Uani 1 1 d
C3 C 0.9407(2) 0.46346(18) 0.77007(17) 0.0152(4) Uani 1 1 d
C4 C 0.9268(2) 0.55818(18) 0.85846(17) 0.0156(4) Uani 1 1 d
C5 C 0.7721(2) 0.52234(18) 0.87862(16) 0.0157(4) Uani 1 1 d
C6 C 0.5372(3) 0.3273(2) 0.8097(2) 0.0203(4) Uani 1 1 d
C7 C 0.7793(3) 0.24532(19) 0.66016(18) 0.0193(4) Uani 1 1 d
C8 C 1.0865(3) 0.4545(2) 0.7238(2) 0.0216(4) Uani 1 1 d
C9 C 1.0585(3) 0.6670(2) 0.93048(19) 0.0217(4) Uani 1 1 d
C10 C 0.7127(3) 0.5888(2) 0.97273(19) 0.0242(5) Uani 1 1 d
C11 C 0.7573(2) 0.79503(17) 0.74398(17) 0.0136(4) Uani 1 1 d
C12 C 0.4730(3) 0.9255(2) 0.65331(19) 0.0205(4) Uani 1 1 d
C13 C 0.4722(3) 0.8015(2) 0.8530(2) 0.0246(5) Uani 1 1 d
C14 C 0.7150(3) 1.0364(2) 0.8883(2) 0.0256(5) Uani 1 1 d
C15 C 1.0119(3) 0.7278(2) 0.62475(19) 0.0198(4) Uani 1 1 d
C16 C 1.0744(3) 0.9866(2) 0.7646(2) 0.0235(4) Uani 1 1 d
C17 C 0.8135(3) 0.9048(2) 0.53342(19) 0.0203(4) Uani 1 1 d
C18 C 0.4027(2) 0.44031(18) 0.56502(16) 0.0139(4) Uani 1 1 d
C19 C 0.5020(2) 0.37343(17) 0.50724(16) 0.0130(3) Uani 1 1 d
C20 C 0.6137(2) 0.43662(18) 0.45312(16) 0.0142(4) Uani 1 1 d
H6A H 0.556(3) 0.287(3) 0.872(2) 0.029(7) Uiso 1 1 d
H6B H 0.460(3) 0.375(3) 0.822(2) 0.029(7) Uiso 1 1 d
H6C H 0.485(4) 0.270(3) 0.741(3) 0.034(8) Uiso 1 1 d
H7A H 0.851(4) 0.204(3) 0.696(3) 0.034(8) Uiso 1 1 d
H7B H 0.665(3) 0.194(3) 0.641(2) 0.030(7) Uiso 1 1 d
H7C H 0.797(3) 0.256(2) 0.583(2) 0.028(7) Uiso 1 1 d
H8A H 1.122(4) 0.382(3) 0.735(2) 0.036(8) Uiso 1 1 d
H8B H 1.062(3) 0.451(2) 0.641(3) 0.029(7) Uiso 1 1 d
H8C H 1.174(4) 0.525(3) 0.760(2) 0.033(7) Uiso 1 1 d
H9A H 1.122(4) 0.653(3) 1.001(3) 0.064(11) Uiso 1 1 d
H9B H 1.133(4) 0.693(3) 0.890(3) 0.042(8) Uiso 1 1 d
H9C H 1.001(4) 0.737(3) 0.948(3) 0.054(10) Uiso 1 1 d
H10A H 0.734(4) 0.556(3) 1.033(3) 0.043(9) Uiso 1 1 d
H10B H 0.762(4) 0.673(3) 0.995(3) 0.031(7) Uiso 1 1 d
H10C H 0.600(4) 0.581(3) 0.948(3) 0.037(8) Uiso 1 1 d
H11A H 0.817(4) 0.790(3) 0.815(3) 0.033(8) Uiso 1 1 d
H12A H 0.530(4) 0.965(3) 0.604(3) 0.034(8) Uiso 1 1 d
H12B H 0.398(4) 0.855(3) 0.605(3) 0.034(8) Uiso 1 1 d
H12C H 0.416(3) 0.985(3) 0.680(2) 0.033(7) Uiso 1 1 d
H13A H 0.420(4) 0.720(3) 0.806(3) 0.038(8) Uiso 1 1 d
H13B H 0.526(4) 0.795(3) 0.926(3) 0.044(9) Uiso 1 1 d
H13C H 0.388(4) 0.842(3) 0.861(3) 0.045(9) Uiso 1 1 d
H14A H 0.770(4) 1.094(3) 0.853(3) 0.038(8) Uiso 1 1 d
H14B H 0.642(3) 1.078(3) 0.920(2) 0.032(7) Uiso 1 1 d
H14C H 0.778(5) 1.019(3) 0.945(3) 0.058(11) Uiso 1 1 d
H15A H 1.084(4) 0.758(3) 0.588(2) 0.032(7) Uiso 1 1 d
H15B H 1.069(3) 0.701(3) 0.688(3) 0.028(7) Uiso 1 1 d
H15C H 0.941(3) 0.652(3) 0.568(2) 0.033(7) Uiso 1 1 d
H16A H 1.152(4) 1.018(3) 0.726(3) 0.045(9) Uiso 1 1 d
H16B H 1.033(4) 1.057(3) 0.794(3) 0.033(7) Uiso 1 1 d
H16C H 1.132(4) 0.958(3) 0.827(3) 0.033(8) Uiso 1 1 d
H17A H 0.785(3) 0.982(3) 0.549(2) 0.026(7) Uiso 1 1 d
H17B H 0.720(3) 0.845(3) 0.485(2) 0.026(7) Uiso 1 1 d
H17C H 0.891(4) 0.914(3) 0.492(3) 0.035(8) Uiso 1 1 d
H18A H 0.330(3) 0.395(2) 0.601(2) 0.021(6) Uiso 1 1 d
H19A H 0.502(3) 0.291(2) 0.517(2) 0.014(6) Uiso 1 1 d
H20A H 0.682(3) 0.397(2) 0.419(2) 0.018(6) Uiso 1 1 d
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'
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
Cnt1 U1 C11 108.3 . .
Cnt2 U1 C11 117.4 . .
Cnt1 U1 Cnt2 132.9 . .
C11 U1 C18 124.59(6) . .
C11 U1 C19 83.19(6) . 2_666
C18 U1 C19 59.16(6) . 2_666
C11 U1 C20 133.66(6) . .
C18 U1 C20 59.61(6) . .
C19 U1 C20 59.17(6) 2_666 .
C11 U1 C19 150.38(6) . .
C18 U1 C19 32.77(6) . .
C19 U1 C19 68.02(7) 2_666 .
C20 U1 C19 32.72(6) . .
C11 U1 C20 94.49(6) . 2_666
C18 U1 C20 32.82(6) . 2_666
C19 U1 C20 32.67(6) 2_666 2_666
C20 U1 C20 68.89(7) . 2_666
C19 U1 C20 57.42(6) . 2_666
C11 U1 C18 101.67(6) . 2_666
C18 U1 C18 68.40(7) . 2_666
C19 U1 C18 32.51(6) 2_666 2_666
C20 U1 C18 32.60(6) . 2_666
C19 U1 C18 56.97(6) . 2_666
C20 U1 C18 57.39(6) 2_666 2_666
C11 U1 C5 90.30(6) . .
C18 U1 C5 104.88(6) . .
C19 U1 C5 152.48(6) 2_666 .
C20 U1 C5 135.54(6) . .
C19 U1 C5 111.89(6) . .
C20 U1 C5 122.34(6) 2_666 .
C18 U1 C5 168.03(6) 2_666 .
C11 U1 C1 119.66(6) . .
C18 U1 C1 82.32(6) . .
C19 U1 C1 141.24(6) 2_666 .
C20 U1 C1 106.68(6) . .
C19 U1 C1 82.20(6) . .
C20 U1 C1 109.92(6) 2_666 .
C18 U1 C1 138.21(6) 2_666 .
C5 U1 C1 30.00(6) . .
C11 U1 C2 133.26(6) . .
C18 U1 C2 92.08(6) . .
C19 U1 C2 143.55(6) 2_666 .
C20 U1 C2 87.87(6) . .
C19 U1 C2 75.78(6) . .
C20 U1 C2 124.79(6) 2_666 .
C18 U1 C2 119.83(6) 2_666 .
C5 U1 C2 49.18(6) . .
C1 U1 C2 29.78(6) . .
C11 U1 C4 84.36(6) . .
C18 U1 C4 131.48(6) . .
C19 U1 C4 167.28(6) 2_666 .
C20 U1 C4 130.15(6) . .
C19 U1 C4 124.65(6) . .
C20 U1 C4 151.95(6) 2_666 .
C18 U1 C4 150.28(6) 2_666 .
C5 U1 C4 29.92(6) . .
C1 U1 C4 49.31(6) . .
C2 U1 C4 48.96(6) . .
C11 U1 C3 108.72(6) . .
C18 U1 C3 121.55(6) . .
C19 U1 C3 157.53(6) 2_666 .
C20 U1 C3 100.58(6) . .
C19 U1 C3 100.75(6) . .
C20 U1 C3 154.34(6) 2_666 .
C18 U1 C3 125.03(6) 2_666 .
C5 U1 C3 49.08(6) . .
C1 U1 C3 49.06(6) . .
C2 U1 C3 29.57(6) . .
C4 U1 C3 29.57(6) . .
C11 Si1 C13 111.41(10) . .
C11 Si1 C12 113.86(9) . .
C13 Si1 C12 106.13(11) . .
C11 Si1 C14 112.40(10) . .
C13 Si1 C14 105.71(11) . .
C12 Si1 C14 106.77(11) . .
C11 Si2 C17 114.94(9) . .
C11 Si2 C16 114.72(10) . .
C17 Si2 C16 107.45(11) . .
C11 Si2 C15 108.44(9) . .
C17 Si2 C15 105.26(10) . .
C16 Si2 C15 105.18(10) . .
C5 C1 C2 108.01(17) . .
C5 C1 C6 125.23(18) . .
C2 C1 C6 126.26(18) . .
C5 C1 U1 74.81(11) . .
C2 C1 U1 76.51(11) . .
C6 C1 U1 121.21(12) . .
C1 C2 C3 107.92(17) . .
C1 C2 C7 127.79(18) . .
C3 C2 C7 123.70(18) . .
C1 C2 U1 73.71(10) . .
C3 C2 U1 75.52(10) . .
C7 C2 U1 123.66(13) . .
C2 C3 C4 108.42(17) . .
C2 C3 C8 123.78(18) . .
C4 C3 C8 127.53(18) . .
C2 C3 U1 74.91(10) . .
C4 C3 U1 75.19(11) . .
C8 C3 U1 120.78(13) . .
C3 C4 C5 107.32(17) . .
C3 C4 C9 126.88(19) . .
C5 C4 C9 125.24(19) . .
C3 C4 U1 75.23(11) . .
C5 C4 U1 73.18(11) . .
C9 C4 U1 123.89(13) . .
C1 C5 C4 108.31(17) . .
C1 C5 C10 125.6(2) . .
C4 C5 C10 125.6(2) . .
C1 C5 U1 75.18(10) . .
C4 C5 U1 76.90(11) . .
C10 C5 U1 120.42(13) . .
Si2 C11 Si1 120.43(10) . .
Si2 C11 U1 103.53(8) . .
Si1 C11 U1 124.93(9) . .
C19 C18 C20 119.61(17) . 2_666
C19 C18 U1 76.76(11) . .
C20 C18 U1 77.26(11) 2_666 .
C19 C18 U1 70.18(10) . 2_666
C20 C18 U1 70.60(10) 2_666 2_666
U1 C18 U1 111.60(7) . 2_666
C18 C19 C20 120.64(17) . .
C18 C19 U1 77.32(11) . 2_666
C20 C19 U1 76.84(11) . 2_666
C18 C19 U1 70.48(10) . .
C20 C19 U1 71.47(10) . .
U1 C19 U1 111.98(7) 2_666 .
C19 C20 C18 118.34(16) . 2_666
C19 C20 U1 75.81(11) . .
C18 C20 U1 76.79(11) 2_666 .
C19 C20 U1 70.48(10) . 2_666
C18 C20 U1 69.92(10) 2_666 2_666
U1 C20 U1 111.11(7) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 Cnt1 2.486 .
U1 Cnt2 2.139 .
U1 C11 2.5084(19) .
U1 C18 2.5323(19) .
U1 C19 2.5455(19) 2_666
U1 C20 2.5577(19) .
U1 C19 2.6153(19) .
U1 C20 2.6298(19) 2_666
U1 C18 2.6398(19) 2_666
U1 C5 2.7353(18) .
U1 C1 2.7400(18) .
U1 C2 2.7759(18) .
U1 C4 2.7832(19) .
U1 C3 2.7837(18) .
Si1 C11 1.845(2) .
Si1 C13 1.878(2) .
Si1 C12 1.880(2) .
Si1 C14 1.881(2) .
Si2 C11 1.842(2) .
Si2 C17 1.878(2) .
Si2 C16 1.878(2) .
Si2 C15 1.901(2) .
C1 C5 1.417(3) .
C1 C2 1.418(3) .
C1 C6 1.510(3) .
C2 C3 1.419(3) .
C2 C7 1.501(3) .
C3 C4 1.421(3) .
C3 C8 1.510(3) .
C4 C5 1.426(3) .
C4 C9 1.504(3) .
C5 C10 1.500(3) .
C18 C19 1.454(3) .
C18 C20 1.461(3) 2_666
C18 U1 2.6398(19) 2_666
C19 C20 1.458(3) .
C19 U1 2.5455(19) 2_666
C20 C18 1.461(3) 2_666
C20 U1 2.6298(19) 2_666
