#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:45:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178822 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/76/4107685.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_4107685
loop_
_publ_author_name
'Christopher R. Graves'
'Ping Yang'
'Stosh A. Kozimor'
'Anthony E. Vaughn'
'David L. Clark'
'Steven D. Conradson'
'Eric J. Schelter'
'Brian L. Scott'
'J. D. Thompson'
'P. Jeffrey Hay'
'David E. Morris'
'Jaqueline L. Kiplinger'
_publ_contact_author_address
;
Los Alamos National Laboratory
Los Alamos, NM 87545
USA
;
_publ_contact_author_email       kiplinger@lanl.gov
_publ_contact_author_fax         '+1 505 667 9905'
_publ_contact_author_name        'Jaqueline L. Kiplinger'
_publ_contact_author_phone       '+1 505 665 9553'
_publ_section_title
;
 Organometallic Uranium(V)-Imido Halide Complexes: From Synthesis to
 Electronic Structure and Bonding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5272
_journal_page_last               5285
_journal_paper_doi               10.1021/ja711010h
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C38 H59 F N U'
_chemical_formula_weight         786.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.573(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.862(4)
_cell_length_b                   13.817(6)
_cell_length_c                   12.801(5)
_cell_measurement_temperature    141(2)
_cell_volume                     1729.1(12)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2007
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5586
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.724
_exptl_absorpt_correction_T_max  0.9114
_exptl_absorpt_correction_T_min  0.4835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       'rectangular slab'
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.856
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         5586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.701
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0511
_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)+(0.0372P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                3401
_reflns_number_total             5586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711010h-file004_3.cif
_cod_data_source_block           apx452_hklf5_50
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4107685
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_refinement_flags
U1 U 0.71828(5) 0.7500 0.72284(3) 0.02013(12) Uani 1 2 d S
N1 N 0.6245(8) 0.7500 0.5775(6) 0.020(2) Uani 1 2 d S
C1 C 0.8520(8) 0.8996(5) 0.8371(6) 0.0247(19) Uani 1 1 d .
C2 C 0.7361(8) 0.8866(5) 0.8886(5) 0.0271(18) Uani 1 1 d .
C3 C 0.6184(7) 0.9125(5) 0.8196(6) 0.0243(19) Uani 1 1 d .
C4 C 0.6622(8) 0.9455(5) 0.7244(6) 0.026(2) Uani 1 1 d .
C5 C 0.8054(8) 0.9380(5) 0.7354(6) 0.026(2) Uani 1 1 d .
C6 C 0.9980(7) 0.8890(6) 0.8850(6) 0.042(2) Uani 1 1 d .
H6A H 1.0353 0.9516 0.9043 0.063 Uiso 1 1 calc R
H6B H 1.0496 0.8597 0.8349 0.063 Uiso 1 1 calc R
H6C H 1.0026 0.8489 0.9467 0.063 Uiso 1 1 calc R
C7 C 0.7349(9) 0.8681(5) 1.0047(5) 0.045(2) Uani 1 1 d .
H7A H 0.7306 0.9287 1.0408 0.067 Uiso 1 1 calc R
H7B H 0.8168 0.8343 1.0326 0.067 Uiso 1 1 calc R
H7C H 0.6566 0.8295 1.0145 0.067 Uiso 1 1 calc R
C8 C 0.4785(7) 0.9246(6) 0.8506(6) 0.039(2) Uani 1 1 d .
H8A H 0.4552 0.8681 0.8881 0.059 Uiso 1 1 calc R
H8B H 0.4135 0.9329 0.7886 0.059 Uiso 1 1 calc R
H8C H 0.4771 0.9804 0.8951 0.059 Uiso 1 1 calc R
C9 C 0.5732(7) 0.9897(5) 0.6317(6) 0.033(2) Uani 1 1 d .
H9A H 0.5794 1.0590 0.6360 0.049 Uiso 1 1 calc R
H9B H 0.4800 0.9701 0.6328 0.049 Uiso 1 1 calc R
H9C H 0.6037 0.9681 0.5674 0.049 Uiso 1 1 calc R
C10 C 0.8984(8) 0.9755(5) 0.6628(6) 0.036(2) Uani 1 1 d .
H10A H 0.8457 0.9954 0.5979 0.054 Uiso 1 1 calc R
H10B H 0.9611 0.9255 0.6488 0.054 Uiso 1 1 calc R
H10C H 0.9485 1.0298 0.6946 0.054 Uiso 1 1 calc R
C11 C 0.5377(10) 0.7500 0.4802(8) 0.021(2) Uani 1 2 d S
C12 C 0.5977(10) 0.7500 0.3831(8) 0.022(3) Uani 1 2 d S
C13 C 0.5067(10) 0.7500 0.2894(8) 0.024(3) Uani 1 2 d S
H13 H 0.5443 0.7500 0.2265 0.029 Uiso 1 2 calc SR
C14 C 0.3667(10) 0.7500 0.2825(8) 0.019(2) Uani 1 2 d S
C15 C 0.3122(11) 0.7500 0.3766(8) 0.021(3) Uani 1 2 d S
H15 H 0.2176 0.7500 0.3746 0.025 Uiso 1 2 calc SR
C16 C 0.3952(10) 0.7500 0.4765(7) 0.017(2) Uani 1 2 d S
C18 C 0.8148(8) 0.8405(6) 0.4327(6) 0.055(3) Uani 1 1 d .
H18A H 0.7739 0.8969 0.3979 0.083 Uiso 1 1 calc R
H18B H 0.9112 0.8402 0.4282 0.083 Uiso 1 1 calc R
H18C H 0.8003 0.8413 0.5054 0.083 Uiso 1 1 calc R
C19 C 0.7840(14) 0.7500 0.2685(9) 0.076(5) Uani 1 2 d S
H19A H 0.7955 0.6846 0.2460 0.115 Uiso 0.50 1 calc PR
H19B H 0.8673 0.7854 0.2658 0.115 Uiso 0.50 1 calc PR
H19C H 0.7111 0.7801 0.2227 0.115 Uiso 0.50 1 calc PR
C20 C 0.3135(10) 0.7500 0.5697(8) 0.023(3) Uani 1 2 d S
C21 C 0.3953(10) 0.7500 0.6773(8) 0.037(3) Uani 1 2 d S
H21A H 0.4319 0.6865 0.6930 0.056 Uiso 0.50 1 calc PR
H21B H 0.3374 0.7679 0.7288 0.056 Uiso 0.50 1 calc PR
H21C H 0.4690 0.7956 0.6790 0.056 Uiso 0.50 1 calc PR
C22 C 0.2206(7) 0.8408(5) 0.5655(6) 0.035(2) Uani 1 1 d .
H22A H 0.1712 0.8409 0.6253 0.052 Uiso 1 1 calc R
H22B H 0.1570 0.8397 0.5019 0.052 Uiso 1 1 calc R
H22C H 0.2760 0.8980 0.5667 0.052 Uiso 1 1 calc R
C23 C 0.2798(11) 0.7500 0.1738(8) 0.024(3) Uani 1 2 d S
C24 C 0.1284(10) 0.7500 0.1829(8) 0.036(3) Uani 1 2 d S
H24A H 0.0815 0.7084 0.1299 0.054 Uiso 0.50 1 calc PR
H24B H 0.0932 0.8146 0.1732 0.054 Uiso 0.50 1 calc PR
H24C H 0.1143 0.7270 0.2514 0.054 Uiso 0.50 1 calc PR
C25 C 0.3137(8) 0.8395(5) 0.1128(5) 0.035(2) Uani 1 1 d .
H25A H 0.2641 0.8374 0.0431 0.053 Uiso 1 1 calc R
H25B H 0.4101 0.8410 0.1084 0.053 Uiso 1 1 calc R
H25C H 0.2883 0.8965 0.1484 0.053 Uiso 1 1 calc R
C26 C 0.7497(10) 0.7500 0.3797(8) 0.034(3) Uani 1 2 d S
F1 F 0.9212(5) 0.7500 0.6845(4) 0.0245(14) Uani 1 2 d S
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'
F F 0.0171 0.0103 '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 F1 97.0(3) . .
N1 U1 C5 99.25(17) . .
F1 U1 C5 73.44(16) . .
N1 U1 C5 99.25(17) . 4_575
F1 U1 C5 73.44(16) . 4_575
C5 U1 C5 143.6(3) . 4_575
N1 U1 C4 86.40(17) . 4_575
F1 U1 C4 101.41(16) . 4_575
C5 U1 C4 172.7(3) . 4_575
C5 U1 C4 29.63(19) 4_575 4_575
N1 U1 C4 86.40(17) . .
F1 U1 C4 101.41(17) . .
C5 U1 C4 29.63(19) . .
C5 U1 C4 172.7(3) 4_575 .
C4 U1 C4 156.7(3) 4_575 .
N1 U1 C1 129.27(17) . .
F1 U1 C1 73.95(18) . .
C5 U1 C1 30.02(19) . .
C5 U1 C1 123.7(2) 4_575 .
C4 U1 C1 144.2(2) 4_575 .
C4 U1 C1 49.1(2) . .
N1 U1 C1 129.27(17) . 4_575
F1 U1 C1 73.95(18) . 4_575
C5 U1 C1 123.7(2) . 4_575
C5 U1 C1 30.02(19) 4_575 4_575
C4 U1 C1 49.1(2) 4_575 4_575
C4 U1 C1 144.2(2) . 4_575
C1 U1 C1 96.8(3) . 4_575
N1 U1 C3 105.6(2) . .
F1 U1 C3 119.91(16) . .
C5 U1 C3 48.7(2) . .
C5 U1 C3 149.4(2) 4_575 .
C4 U1 C3 134.3(2) 4_575 .
C4 U1 C3 29.6(2) . .
C1 U1 C3 48.6(2) . .
C1 U1 C3 122.4(2) 4_575 .
N1 U1 C3 105.6(2) . 4_575
F1 U1 C3 119.91(15) . 4_575
C5 U1 C3 149.4(2) . 4_575
C5 U1 C3 48.7(2) 4_575 4_575
C4 U1 C3 29.6(2) 4_575 4_575
C4 U1 C3 134.3(2) . 4_575
C1 U1 C3 122.4(2) . 4_575
C1 U1 C3 48.6(2) 4_575 4_575
C3 U1 C3 106.4(3) . 4_575
N1 U1 C2 133.25(17) . .
F1 U1 C2 101.90(19) . .
C5 U1 C2 48.2(2) . .
C5 U1 C2 127.0(2) 4_575 .
C4 U1 C2 129.8(2) 4_575 .
C4 U1 C2 48.2(2) . .
C1 U1 C2 29.1(2) . .
C1 U1 C2 97.1(2) 4_575 .
C3 U1 C2 28.96(19) . .
C3 U1 C2 101.2(2) 4_575 .
N1 U1 C2 133.25(17) . 4_575
F1 U1 C2 101.90(19) . 4_575
C5 U1 C2 127.0(2) . 4_575
C5 U1 C2 48.2(2) 4_575 4_575
C4 U1 C2 48.2(2) 4_575 4_575
C4 U1 C2 129.8(2) . 4_575
C1 U1 C2 97.1(2) . 4_575
C1 U1 C2 29.1(2) 4_575 4_575
C3 U1 C2 101.2(2) . 4_575
C3 U1 C2 28.96(19) 4_575 4_575
C2 U1 C2 83.7(3) . 4_575
C11 N1 U1 171.0(7) . .
C2 C1 C5 107.0(7) . .
C2 C1 C6 126.4(7) . .
C5 C1 C6 126.1(7) . .
C2 C1 U1 78.0(4) . .
C5 C1 U1 73.8(4) . .
C6 C1 U1 120.7(5) . .
C1 C2 C3 109.1(6) . .
C1 C2 C7 126.6(7) . .
C3 C2 C7 123.2(7) . .
C1 C2 U1 73.0(4) . .
C3 C2 U1 74.6(4) . .
C7 C2 U1 128.2(5) . .
C2 C3 C4 107.5(7) . .
C2 C3 C8 125.1(7) . .
C4 C3 C8 126.0(7) . .
C2 C3 U1 76.4(4) . .
C4 C3 U1 73.4(4) . .
C8 C3 U1 126.6(5) . .
C5 C4 C3 107.8(7) . .
C5 C4 C9 125.5(7) . .
C3 C4 C9 126.4(7) . .
C5 C4 U1 74.3(5) . .
C3 C4 U1 77.1(4) . .
C9 C4 U1 119.1(5) . .
C4 C5 C1 108.5(7) . .
C4 C5 C10 127.5(7) . .
C1 C5 C10 123.5(7) . .
C4 C5 U1 76.1(5) . .
C1 C5 U1 76.2(4) . .
C10 C5 U1 120.7(5) . .
C16 C11 N1 121.1(9) . .
C16 C11 C12 119.6(9) . .
N1 C11 C12 119.3(9) . .
C13 C12 C11 116.6(9) . .
C13 C12 C26 120.2(9) . .
C11 C12 C26 123.1(9) . .
C14 C13 C12 125.5(10) . .
C13 C14 C15 116.6(10) . .
C13 C14 C23 119.7(10) . .
C15 C14 C23 123.7(9) . .
C14 C15 C16 122.6(10) . .
C11 C16 C15 119.0(9) . .
C11 C16 C20 127.3(9) . .
C15 C16 C20 113.7(9) . .
C21 C20 C16 116.2(9) . .
C21 C20 C22 106.0(6) . 4_575
C16 C20 C22 110.1(5) . 4_575
C21 C20 C22 106.0(6) . .
C16 C20 C22 110.1(5) . .
C22 C20 C22 108.0(8) 4_575 .
C24 C23 C25 109.0(6) . 4_575
C24 C23 C25 109.0(6) . .
C25 C23 C25 108.6(8) 4_575 .
C24 C23 C14 111.6(9) . .
C25 C23 C14 109.3(6) 4_575 .
C25 C23 C14 109.3(6) . .
C12 C26 C19 112.1(9) . .
C12 C26 C18 110.5(6) . .
C19 C26 C18 106.7(6) . .
C12 C26 C18 110.5(6) . 4_575
C19 C26 C18 106.7(6) . 4_575
C18 C26 C18 110.3(9) . 4_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.965(8) .
U1 F1 2.122(5) .
U1 C5 2.734(8) .
U1 C5 2.734(8) 4_575
U1 C4 2.758(7) 4_575
U1 C4 2.758(7) .
U1 C1 2.764(7) .
U1 C1 2.764(7) 4_575
U1 C3 2.805(7) .
U1 C3 2.805(7) 4_575
U1 C2 2.828(7) .
U1 C2 2.828(7) 4_575
N1 C11 1.415(11) .
C1 C2 1.405(10) .
C1 C5 1.425(9) .
C1 C6 1.496(9) .
C2 C3 1.409(9) .
C2 C7 1.509(9) .
C3 C4 1.420(10) .
C3 C8 1.494(9) .
C4 C5 1.404(9) .
C4 C9 1.509(9) .
C5 C10 1.482(9) .
C11 C16 1.400(12) .
C11 C12 1.445(13) .
C12 C13 1.400(13) .
C12 C26 1.505(13) .
C13 C14 1.372(12) .
C14 C15 1.382(13) .
C14 C23 1.535(13) .
C15 C16 1.425(12) .
C16 C20 1.524(13) .
C18 C26 1.523(9) .
C19 C26 1.506(14) .
C20 C21 1.503(12) .
C20 C22 1.550(8) 4_575
C20 C22 1.550(8) .
C23 C24 1.513(15) .
C23 C25 1.523(8) 4_575
C23 C25 1.523(8) .
C26 C18 1.523(9) 4_575
