#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:43:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178821 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/75/4107534.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_4107534
loop_
_publ_author_name
'Liam P. Spencer'
'Ping Yang'
'Brian L. Scott'
'Enrique R. Batista'
'James M. Boncella'
_publ_section_title
;
 Imido Exchange in Bis(imido) Uranium(VI) Complexes with Aryl Isocyanates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2930
_journal_page_last               2931
_journal_paper_doi               10.1021/ja7107454
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C55 H54 Cl2 I2 N2 O2 P2 U'
_chemical_formula_weight         1399.67
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.471(2)
_cell_angle_beta                 112.773(2)
_cell_angle_gamma                101.480(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7202(19)
_cell_length_b                   11.445(2)
_cell_length_c                   12.290(2)
_cell_measurement_temperature    141(2)
_cell_volume                     1326.3(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.916
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14549
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.427
_exptl_absorpt_correction_T_max  0.8428
_exptl_absorpt_correction_T_min  0.5377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.771
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0419
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                4448
_reflns_number_total             5948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7107454-file002.cif
_cod_data_source_block           apx463s
_cod_original_cell_volume        1326.2(4)
_cod_database_code               4107534
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
_atom_site_refinement_flags
U1 U 0.0000 0.0000 0.0000 0.01646(12) Uani 1 2 d S
I1 I -0.16605(5) -0.17286(4) 0.09731(4) 0.02497(14) Uani 1 1 d .
P1 P 0.15647(19) 0.27403(16) 0.26667(16) 0.0190(4) Uani 1 1 d .
N1 N 0.1586(6) -0.0522(5) 0.0807(5) 0.0173(12) Uani 1 1 d .
O1 O 0.0733(5) 0.1603(4) 0.1657(4) 0.0217(10) Uani 1 1 d .
C1 C 0.0940(7) 0.2720(6) 0.3833(6) 0.0212(15) Uani 1 1 d .
C2 C 0.1288(8) 0.3760(6) 0.4720(6) 0.0236(15) Uani 1 1 d .
H2 H 0.1831 0.4492 0.4697 0.028 Uiso 1 1 calc R
C3 C 0.0854(8) 0.3737(7) 0.5626(7) 0.0266(16) Uani 1 1 d .
H3 H 0.1102 0.4442 0.6220 0.032 Uiso 1 1 calc R
C4 C 0.0026(8) 0.2630(8) 0.5645(7) 0.0294(17) Uani 1 1 d .
H4 H -0.0279 0.2596 0.6257 0.035 Uiso 1 1 calc R
C5 C -0.0335(8) 0.1596(7) 0.4762(7) 0.0287(17) Uani 1 1 d .
H5 H -0.0896 0.0869 0.4774 0.034 Uiso 1 1 calc R
C6 C 0.0126(8) 0.1616(7) 0.3849(6) 0.0219(15) Uani 1 1 d .
H6 H -0.0104 0.0909 0.3264 0.026 Uiso 1 1 calc R
C7 C 0.1361(8) 0.4104(7) 0.2148(6) 0.0236(15) Uani 1 1 d .
C8 C 0.2379(8) 0.4814(7) 0.1886(6) 0.0257(16) Uani 1 1 d .
H8 H 0.3196 0.4585 0.1990 0.031 Uiso 1 1 calc R
C9 C 0.2174(8) 0.5867(7) 0.1469(7) 0.0289(17) Uani 1 1 d .
H9 H 0.2847 0.6332 0.1282 0.035 Uiso 1 1 calc R
C10 C 0.0956(8) 0.6224(7) 0.1331(6) 0.0293(17) Uani 1 1 d .
H10 H 0.0839 0.6945 0.1085 0.035 Uiso 1 1 calc R
C11 C -0.0076(8) 0.5506(7) 0.1562(7) 0.0284(17) Uani 1 1 d .
H11 H -0.0903 0.5723 0.1438 0.034 Uiso 1 1 calc R
C12 C 0.0136(8) 0.4458(7) 0.1978(6) 0.0251(16) Uani 1 1 d .
H12 H -0.0549 0.3985 0.2147 0.030 Uiso 1 1 calc R
C13 C 0.3417(7) 0.2800(7) 0.3297(6) 0.0232(15) Uani 1 1 d .
C14 C 0.4292(8) 0.3368(7) 0.4521(7) 0.0279(16) Uani 1 1 d .
H14 H 0.3942 0.3738 0.5017 0.033 Uiso 1 1 calc R
C15 C 0.5686(8) 0.3361(7) 0.4965(8) 0.0361(19) Uani 1 1 d .
H15 H 0.6285 0.3732 0.5772 0.043 Uiso 1 1 calc R
C16 C 0.6202(8) 0.2814(7) 0.4230(7) 0.0344(19) Uani 1 1 d .
H16 H 0.7145 0.2822 0.4544 0.041 Uiso 1 1 calc R
C17 C 0.5348(8) 0.2260(7) 0.3047(7) 0.0332(18) Uani 1 1 d .
H17 H 0.5702 0.1887 0.2556 0.040 Uiso 1 1 calc R
C18 C 0.3944(9) 0.2258(8) 0.2583(7) 0.0336(19) Uani 1 1 d .
H18 H 0.3356 0.1882 0.1775 0.040 Uiso 1 1 calc R
C19 C 0.2836(7) -0.0816(6) 0.1463(6) 0.0237(15) Uani 1 1 d .
C20 C 0.3295(7) -0.0798(6) 0.2701(6) 0.0212(15) Uani 1 1 d .
C21 C 0.4556(8) -0.1066(7) 0.3305(6) 0.0266(16) Uani 1 1 d .
H21 H 0.4863 -0.1043 0.4129 0.032 Uiso 1 1 calc R
C22 C 0.5375(8) -0.1367(7) 0.2739(6) 0.0250(16) Uani 1 1 d .
C23 C 0.4877(7) -0.1407(6) 0.1487(7) 0.0240(15) Uani 1 1 d .
H23 H 0.5408 -0.1614 0.1085 0.029 Uiso 1 1 calc R
C24 C 0.3612(7) -0.1147(6) 0.0830(6) 0.0230(15) Uani 1 1 d .
C25 C 0.2442(8) -0.0495(7) 0.3364(6) 0.0251(16) Uani 1 1 d .
H25A H 0.1609 -0.0330 0.2815 0.038 Uiso 1 1 calc R
H25B H 0.2989 0.0215 0.4015 0.038 Uiso 1 1 calc R
H25C H 0.2181 -0.1175 0.3688 0.038 Uiso 1 1 calc R
C26 C 0.6714(8) -0.1702(9) 0.3401(7) 0.037(2) Uani 1 1 d .
H26A H 0.7131 -0.1876 0.2856 0.055 Uiso 1 1 calc R
H26B H 0.6507 -0.2413 0.3705 0.055 Uiso 1 1 calc R
H26C H 0.7356 -0.1031 0.4066 0.055 Uiso 1 1 calc R
C27 C 0.3118(8) -0.1234(7) -0.0493(6) 0.0277(17) Uani 1 1 d .
H27A H 0.3780 -0.1483 -0.0754 0.042 Uiso 1 1 calc R
H27B H 0.3036 -0.0450 -0.0661 0.042 Uiso 1 1 calc R
H27C H 0.2217 -0.1827 -0.0919 0.042 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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 N1 180.0(5) 2 .
N1 U1 O1 89.9(2) 2 2
N1 U1 O1 90.1(2) . 2
N1 U1 O1 90.1(2) 2 .
N1 U1 O1 89.9(2) . .
O1 U1 O1 180.0(3) 2 .
N1 U1 I1 90.42(17) 2 .
N1 U1 I1 89.58(17) . .
O1 U1 I1 87.11(12) 2 .
O1 U1 I1 92.89(12) . .
N1 U1 I1 89.58(17) 2 2
N1 U1 I1 90.42(17) . 2
O1 U1 I1 92.89(12) 2 2
O1 U1 I1 87.11(12) . 2
I1 U1 I1 180.000(14) . 2
O1 P1 C7 111.9(3) . .
O1 P1 C1 109.6(3) . .
C7 P1 C1 106.9(3) . .
O1 P1 C13 109.8(3) . .
C7 P1 C13 108.6(3) . .
C1 P1 C13 109.9(3) . .
C19 N1 U1 175.4(5) . .
P1 O1 U1 164.1(3) . .
C2 C1 C6 120.1(7) . .
C2 C1 P1 121.4(6) . .
C6 C1 P1 118.4(5) . .
C3 C2 C1 121.5(7) . .
C2 C3 C4 118.8(7) . .
C5 C4 C3 120.0(7) . .
C4 C5 C6 121.2(7) . .
C5 C6 C1 118.4(7) . .
C8 C7 C12 119.2(7) . .
C8 C7 P1 121.7(6) . .
C12 C7 P1 119.1(6) . .
C7 C8 C9 120.0(7) . .
C8 C9 C10 120.1(7) . .
C11 C10 C9 120.1(7) . .
C10 C11 C12 119.5(7) . .
C11 C12 C7 121.1(7) . .
C18 C13 C14 120.3(7) . .
C18 C13 P1 119.4(5) . .
C14 C13 P1 120.3(6) . .
C15 C14 C13 118.1(7) . .
C16 C15 C14 120.9(8) . .
C17 C16 C15 120.8(8) . .
C16 C17 C18 119.3(8) . .
C13 C18 C17 120.7(7) . .
C20 C19 N1 121.5(6) . .
C20 C19 C24 120.8(7) . .
N1 C19 C24 117.7(6) . .
C21 C20 C19 118.8(7) . .
C21 C20 C25 120.3(6) . .
C19 C20 C25 120.9(6) . .
C22 C21 C20 122.9(7) . .
C21 C22 C23 117.4(6) . .
C21 C22 C26 122.0(6) . .
C23 C22 C26 120.5(7) . .
C24 C23 C22 122.3(7) . .
C23 C24 C19 117.8(6) . .
C23 C24 C27 120.1(6) . .
C19 C24 C27 122.1(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.867(5) 2
U1 N1 1.867(5) .
U1 O1 2.313(4) 2
U1 O1 2.313(4) .
U1 I1 3.0618(5) .
U1 I1 3.0618(5) 2
P1 O1 1.513(5) .
P1 C7 1.782(7) .
P1 C1 1.803(7) .
P1 C13 1.814(7) .
N1 C19 1.404(8) .
C1 C2 1.384(9) .
C1 C6 1.393(10) .
C2 C3 1.365(10) .
C3 C4 1.404(11) .
C4 C5 1.375(11) .
C5 C6 1.390(10) .
C7 C8 1.393(10) .
C7 C12 1.398(10) .
C8 C9 1.394(10) .
C9 C10 1.401(11) .
C10 C11 1.386(11) .
C11 C12 1.389(10) .
C13 C18 1.363(10) .
C13 C14 1.405(10) .
C14 C15 1.381(11) .
C15 C16 1.375(11) .
C16 C17 1.360(11) .
C17 C18 1.387(11) .
C19 C20 1.402(10) .
C19 C24 1.411(10) .
C20 C21 1.386(9) .
C20 C25 1.501(10) .
C21 C22 1.381(10) .
C22 C23 1.410(10) .
C22 C26 1.505(9) .
C23 C24 1.398(9) .
C24 C27 1.484(10) .
