#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:19:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178845 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109968.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_4109968
loop_
_publ_author_name
'Christopher R. Graves'
'Brian L. Scott'
'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
;
 Facile Access to Pentavalent Uranium Organometallics: One-Electron
 Oxidation of Uranium(IV) Imido Complexes with Copper(I) Salts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11914
_journal_page_last               11915
_journal_paper_doi               10.1021/ja074889w
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C41 H73 I N U'
_chemical_formula_weight         944.93
_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                 103.9870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4776(9)
_cell_length_b                   13.8658(11)
_cell_length_c                   13.1682(10)
_cell_measurement_temperature    141(2)
_cell_volume                     2033.5(3)
_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 0.999
_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  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21556
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.777
_exptl_absorpt_correction_T_max  0.8319
_exptl_absorpt_correction_T_min  0.3935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.616
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0358
_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)+(0.0484P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                3855
_reflns_number_total             4622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074889wsi20070817_025549_2.cif
_cod_data_source_block           apx412s
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4109968
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 0.18511(2) 0.2500 0.342163(19) 0.01423(9) Uani 1 2 d S
I1 I 0.44321(4) 0.2500 0.46476(4) 0.02816(13) Uani 1 2 d S
N1 N 0.1114(5) 0.2500 0.4631(4) 0.0157(12) Uani 1 2 d S
C1 C 0.2503(5) 0.0578(4) 0.3460(4) 0.0272(12) Uani 1 1 d .
C2 C 0.2918(5) 0.0929(4) 0.2608(5) 0.0292(13) Uani 1 1 d .
C3 C 0.1921(5) 0.1168(4) 0.1798(4) 0.0251(12) Uani 1 1 d .
C4 C 0.0879(5) 0.0957(4) 0.2125(4) 0.0246(12) Uani 1 1 d .
C5 C 0.1231(5) 0.0584(4) 0.3157(4) 0.0244(12) Uani 1 1 d .
C6 C 0.3235(6) 0.0081(5) 0.4422(5) 0.0422(16) Uani 1 1 d .
H6A H 0.3298 -0.0593 0.4278 0.063 Uiso 1 1 calc R
H6B H 0.2850 0.0159 0.4988 0.063 Uiso 1 1 calc R
H6C H 0.4023 0.0361 0.4612 0.063 Uiso 1 1 calc R
C7 C 0.4210(6) 0.0895(5) 0.2517(6) 0.052(2) Uani 1 1 d .
H7A H 0.4738 0.0867 0.3203 0.078 Uiso 1 1 calc R
H7B H 0.4382 0.1463 0.2162 0.078 Uiso 1 1 calc R
H7C H 0.4326 0.0333 0.2126 0.078 Uiso 1 1 calc R
C8 C 0.1962(8) 0.1343(5) 0.0678(5) 0.059(2) Uani 1 1 d .
H8A H 0.1927 0.0737 0.0319 0.089 Uiso 1 1 calc R
H8B H 0.2694 0.1669 0.0661 0.089 Uiso 1 1 calc R
H8C H 0.1289 0.1735 0.0340 0.089 Uiso 1 1 calc R
C9 C -0.0365(5) 0.0909(5) 0.1414(5) 0.0414(16) Uani 1 1 d .
H9A H -0.0383 0.0433 0.0881 0.062 Uiso 1 1 calc R
H9B H -0.0575 0.1527 0.1093 0.062 Uiso 1 1 calc R
H9C H -0.0930 0.0736 0.1814 0.062 Uiso 1 1 calc R
C10 C 0.0432(6) 0.0135(4) 0.3794(5) 0.0373(15) Uani 1 1 d .
H10A H -0.0390 0.0168 0.3405 0.056 Uiso 1 1 calc R
H10B H 0.0526 0.0480 0.4441 0.056 Uiso 1 1 calc R
H10C H 0.0656 -0.0527 0.3938 0.056 Uiso 1 1 calc R
C11 C 0.0386(6) 0.2500 0.5360(5) 0.0175(15) Uani 1 2 d S
C12 C 0.0907(6) 0.2500 0.6472(5) 0.0193(15) Uani 1 2 d S
C13 C 0.0146(7) 0.2500 0.7157(5) 0.0219(16) Uani 1 2 d S
H13 H 0.0496 0.2500 0.7872 0.026 Uiso 1 2 calc SR
C14 C -0.1076(6) 0.2500 0.6844(5) 0.0167(14) Uani 1 2 d S
C15 C -0.1572(6) 0.2500 0.5775(6) 0.0190(15) Uani 1 2 d S
H15 H -0.2404 0.2500 0.5545 0.023 Uiso 1 2 calc SR
C16 C -0.0901(6) 0.2500 0.5024(5) 0.0169(14) Uani 1 2 d S
C17 C 0.2265(7) 0.2500 0.6945(6) 0.0274(18) Uani 1 2 d S
C18 C 0.2814(5) 0.1576(5) 0.6610(4) 0.0337(14) Uani 1 1 d .
H18A H 0.2518 0.1025 0.6912 0.050 Uiso 1 1 calc R
H18B H 0.3673 0.1603 0.6849 0.050 Uiso 1 1 calc R
H18C H 0.2594 0.1523 0.5861 0.050 Uiso 1 1 calc R
C19 C 0.2573(7) 0.2500 0.8139(6) 0.043(3) Uani 1 2 d S
H19A H 0.2402 0.3123 0.8386 0.065 Uiso 0.50 1 calc PR
H19B H 0.3410 0.2357 0.8402 0.065 Uiso 0.50 1 calc PR
H19C H 0.2101 0.2020 0.8381 0.065 Uiso 0.50 1 calc PR
C20 C -0.1814(7) 0.2500 0.7684(6) 0.0231(16) Uani 1 2 d S
C21 C -0.1520(5) 0.1594(4) 0.8369(4) 0.0296(13) Uani 1 1 d .
H21A H -0.0667 0.1551 0.8645 0.044 Uiso 1 1 calc R
H21B H -0.1799 0.1033 0.7954 0.044 Uiso 1 1 calc R
H21C H -0.1910 0.1633 0.8935 0.044 Uiso 1 1 calc R
C22 C -0.3185(7) 0.2500 0.7203(6) 0.0271(18) Uani 1 2 d S
H22A H -0.3601 0.2424 0.7749 0.041 Uiso 0.50 1 calc PR
H22B H -0.3388 0.1977 0.6715 0.041 Uiso 0.50 1 calc PR
H22C H -0.3415 0.3100 0.6846 0.041 Uiso 0.50 1 calc PR
C23 C -0.1677(6) 0.2500 0.3879(5) 0.0178(15) Uani 1 2 d S
C24 C -0.0959(6) 0.2500 0.3036(5) 0.0213(16) Uani 1 2 d S
H24A H -0.0586 0.3118 0.3022 0.032 Uiso 0.50 1 calc PR
H24B H -0.1489 0.2373 0.2365 0.032 Uiso 0.50 1 calc PR
H24C H -0.0352 0.2009 0.3192 0.032 Uiso 0.50 1 calc PR
C25 C -0.2477(5) 0.1603(4) 0.3683(4) 0.0235(12) Uani 1 1 d .
H25A H -0.2884 0.1572 0.2955 0.035 Uiso 1 1 calc R
H25B H -0.3057 0.1638 0.4098 0.035 Uiso 1 1 calc R
H25C H -0.1991 0.1037 0.3871 0.035 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'
I I -0.4742 1.8119 '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 C5 87.36(12) . .
N1 U1 C5 87.36(12) . 4_565
C5 U1 C5 149.9(2) . 4_565
N1 U1 C1 98.74(12) . 4_565
C5 U1 C1 173.59(15) . 4_565
C5 U1 C1 29.79(16) 4_565 4_565
N1 U1 C1 98.74(12) . .
C5 U1 C1 29.79(16) . .
C5 U1 C1 173.59(15) 4_565 .
C1 U1 C1 149.1(2) 4_565 .
N1 U1 C4 107.86(15) . .
C5 U1 C4 29.60(15) . .
C5 U1 C4 127.51(17) 4_565 .
C1 U1 C4 144.60(16) 4_565 .
C1 U1 C4 48.68(16) . .
N1 U1 C4 107.86(15) . 4_565
C5 U1 C4 127.51(17) . 4_565
C5 U1 C4 29.60(15) 4_565 4_565
C1 U1 C4 48.68(16) 4_565 4_565
C1 U1 C4 144.60(16) . 4_565
C4 U1 C4 99.9(2) . 4_565
N1 U1 C2 127.83(12) . .
C5 U1 C2 48.08(15) . .
C5 U1 C2 144.78(16) 4_565 .
C1 U1 C2 127.45(17) 4_565 .
C1 U1 C2 29.09(16) . .
C4 U1 C2 47.61(16) . .
C4 U1 C2 120.18(17) 4_565 .
N1 U1 C2 127.83(12) . 4_565
C5 U1 C2 144.78(16) . 4_565
C5 U1 C2 48.08(16) 4_565 4_565
C1 U1 C2 29.09(16) 4_565 4_565
C1 U1 C2 127.45(16) . 4_565
C4 U1 C2 120.18(17) . 4_565
C4 U1 C2 47.61(16) 4_565 4_565
C2 U1 C2 100.5(2) . 4_565
N1 U1 C3 134.59(13) . .
C5 U1 C3 47.96(15) . .
C5 U1 C3 125.86(16) 4_565 .
C1 U1 C3 125.70(16) 4_565 .
C1 U1 C3 47.98(16) . .
C4 U1 C3 28.67(15) . .
C4 U1 C3 96.76(16) 4_565 .
C2 U1 C3 28.63(16) . .
C2 U1 C3 97.00(16) 4_565 .
N1 U1 C3 134.59(12) . 4_565
C5 U1 C3 125.86(16) . 4_565
C5 U1 C3 47.96(15) 4_565 4_565
C1 U1 C3 47.98(16) 4_565 4_565
C1 U1 C3 125.70(16) . 4_565
C4 U1 C3 96.76(16) . 4_565
C4 U1 C3 28.67(15) 4_565 4_565
C2 U1 C3 97.00(16) . 4_565
C2 U1 C3 28.63(16) 4_565 4_565
C3 U1 C3 81.1(2) . 4_565
N1 U1 I1 97.20(16) . .
C5 U1 I1 105.01(12) . .
C5 U1 I1 105.01(12) 4_565 .
C1 U1 I1 76.32(12) 4_565 .
C1 U1 I1 76.32(12) . .
C4 U1 I1 121.52(11) . .
C4 U1 I1 121.52(11) 4_565 .
C2 U1 I1 75.14(12) . .
C2 U1 I1 75.14(12) 4_565 .
C3 U1 I1 101.56(12) . .
C3 U1 I1 101.56(12) 4_565 .
C11 N1 U1 169.7(5) . .
C2 C1 C5 107.3(5) . .
C2 C1 C6 126.9(5) . .
C5 C1 C6 124.5(5) . .
C2 C1 U1 78.1(3) . .
C5 C1 U1 74.5(3) . .
C6 C1 U1 123.4(4) . .
C3 C2 C1 108.5(5) . .
C3 C2 C7 125.5(6) . .
C1 C2 C7 125.3(6) . .
C3 C2 U1 76.0(3) . .
C1 C2 U1 72.8(3) . .
C7 C2 U1 125.1(4) . .
C4 C3 C2 108.5(5) . .
C4 C3 C8 124.6(6) . .
C2 C3 C8 124.8(6) . .
C4 C3 U1 73.9(3) . .
C2 C3 U1 75.3(3) . .
C8 C3 U1 130.2(4) . .
C3 C4 C5 107.8(5) . .
C3 C4 C9 124.8(5) . .
C5 C4 C9 125.9(5) . .
C3 C4 U1 77.5(3) . .
C5 C4 U1 73.4(3) . .
C9 C4 U1 126.2(4) . .
C4 C5 C1 107.9(5) . .
C4 C5 C10 127.5(5) . .
C1 C5 C10 124.1(5) . .
C4 C5 U1 77.0(3) . .
C1 C5 U1 75.7(3) . .
C10 C5 U1 119.9(3) . .
N1 C11 C16 121.5(6) . .
N1 C11 C12 121.3(6) . .
C16 C11 C12 117.2(6) . .
C13 C12 C11 118.9(6) . .
C13 C12 C17 118.1(6) . .
C11 C12 C17 123.0(6) . .
C14 C13 C12 124.2(6) . .
C13 C14 C15 116.6(6) . .
C13 C14 C20 119.0(6) . .
C15 C14 C20 124.4(6) . .
C14 C15 C16 124.1(7) . .
C15 C16 C11 119.0(6) . .
C15 C16 C23 113.8(6) . .
C11 C16 C23 127.2(6) . .
C19 C17 C12 112.2(6) . .
C19 C17 C18 106.6(4) . .
C12 C17 C18 109.3(4) . .
C19 C17 C18 106.6(4) . 4_565
C12 C17 C18 109.3(4) . 4_565
C18 C17 C18 112.8(6) . 4_565
C21 C20 C21 109.8(6) 4_565 .
C21 C20 C22 107.4(4) 4_565 .
C21 C20 C22 107.4(4) . .
C21 C20 C14 109.8(4) 4_565 .
C21 C20 C14 109.8(4) . .
C22 C20 C14 112.7(6) . .
C25 C23 C25 108.7(6) . 4_565
C25 C23 C24 106.4(4) . .
C25 C23 C24 106.4(4) 4_565 .
C25 C23 C16 110.1(4) . .
C25 C23 C16 110.1(4) 4_565 .
C24 C23 C16 114.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.975(6) .
U1 C5 2.750(5) .
U1 C5 2.750(5) 4_565
U1 C1 2.765(5) 4_565
U1 C1 2.765(5) .
U1 C4 2.796(5) .
U1 C4 2.796(5) 4_565
U1 C2 2.833(5) .
U1 C2 2.833(5) 4_565
U1 C3 2.842(5) .
U1 C3 2.842(5) 4_565
U1 I1 3.0116(6) .
N1 C11 1.418(8) .
C1 C2 1.408(8) .
C1 C5 1.418(8) .
C1 C6 1.507(8) .
C2 C3 1.403(8) .
C2 C7 1.517(8) .
C3 C4 1.396(7) .
C3 C8 1.506(8) .
C4 C5 1.417(7) .
C4 C9 1.509(8) .
C5 C10 1.518(7) .
C11 C16 1.436(9) .
C11 C12 1.442(9) .
C12 C13 1.400(10) .
C12 C17 1.532(10) .
C13 C14 1.362(10) .
C14 C15 1.385(10) .
C14 C20 1.548(9) .
C15 C16 1.392(9) .
C16 C23 1.555(9) .
C17 C19 1.527(11) .
C17 C18 1.539(7) .
C17 C18 1.539(7) 4_565
C20 C21 1.535(7) 4_565
C20 C21 1.535(7) .
C20 C22 1.547(10) .
C23 C25 1.530(6) .
C23 C25 1.530(6) 4_565
C23 C24 1.535(9) .
