#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179355 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325238.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_4325238
loop_
_publ_author_name
'Jessie L. Brown'
'Charles C. Mokhtarzadeh'
'Jeremie M. Lever'
'Guang Wu'
'Trevor W. Hayton'
_publ_section_title
;
 Facile Reduction of a Uranyl(VI) β-Ketoiminate Complex to U(IV) Upon Oxo
 Silylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5105
_journal_page_last               5112
_journal_paper_doi               10.1021/ic200387n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C24 H33 I5 O2 P Si2 U'
_chemical_formula_weight         1313.18
_chemical_name_systematic
; 
 Triphenylmonoiodophosphonium Uranium(V) tetraiodo-bistrimethylsilyloxide  
;
_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                103.327(12)
_cell_angle_beta                 90.511(13)
_cell_angle_gamma                101.222(12)
_cell_formula_units_Z            2
_cell_length_a                   9.452(7)
_cell_length_b                   9.961(8)
_cell_length_c                   20.940(16)
_cell_measurement_temperature    150(2)
_cell_volume                     1879(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'omega scan'
_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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15723
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    8.553
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.346
_refine_diff_density_min         -4.005
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0494
_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)+(0.0671P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                5626
_reflns_number_total             7383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200387n_si_001_2.cif
_cod_data_source_block           Complex_2
_cod_database_code               4325238
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
U2 U 1.0000 0.5000 0.5000 0.01708(13) Uani 1 2 d S
I5 I 0.61432(7) 0.63341(6) 0.38147(3) 0.02878(17) Uani 1 1 d .
I4 I 0.67883(7) 0.42793(6) 0.48805(3) 0.02885(17) Uani 1 1 d .
I3 I 1.00134(7) 0.20025(6) 0.49721(3) 0.03133(18) Uani 1 1 d .
P1 P 0.5785(3) 0.7810(2) 0.30891(11) 0.0215(5) Uani 1 1 d .
Si2 Si 1.0086(3) 0.4205(3) 0.32048(12) 0.0239(6) Uani 1 1 d .
O2 O 1.0053(7) 0.4605(6) 0.4025(3) 0.0270(15) Uani 1 1 d .
C7 C 0.7514(10) 0.8465(8) 0.2813(5) 0.025(2) Uani 1 1 d .
C13 C 0.4623(11) 0.6800(9) 0.2407(5) 0.024(2) Uani 1 1 d .
C24 C 0.4144(11) 0.9155(10) 0.4053(5) 0.029(2) Uani 1 1 d .
H24 H 0.4010 0.8358 0.4223 0.035 Uiso 1 1 calc R
C14 C 0.4850(15) 0.5481(11) 0.2053(5) 0.043(3) Uani 1 1 d .
H14 H 0.5596 0.5116 0.2195 0.051 Uiso 1 1 calc R
C12 C 0.8658(11) 0.9124(9) 0.3274(5) 0.029(2) Uani 1 1 d .
H12 H 0.8516 0.9218 0.3720 0.035 Uiso 1 1 calc R
C20 C 0.5165(11) 1.0429(9) 0.3257(5) 0.029(2) Uani 1 1 d .
H20 H 0.5721 1.0494 0.2898 0.035 Uiso 1 1 calc R
C8 C 0.7726(13) 0.8310(11) 0.2156(5) 0.036(3) Uani 1 1 d .
H8 H 0.6963 0.7888 0.1847 0.043 Uiso 1 1 calc R
C18 C 0.3480(12) 0.7306(11) 0.2191(5) 0.035(2) Uani 1 1 d .
H18 H 0.3315 0.8180 0.2412 0.042 Uiso 1 1 calc R
C19 C 0.5027(10) 0.9228(9) 0.3514(4) 0.023(2) Uani 1 1 d .
U1 U 0.5000 0.0000 0.0000 0.02816(15) Uani 1 2 d S
I2 I 0.41348(10) 0.06994(7) 0.13934(4) 0.0480(2) Uani 1 1 d .
I1 I 0.61640(10) -0.23893(7) 0.02875(4) 0.0481(2) Uani 1 1 d .
Si1 Si 0.8459(3) 0.2430(3) 0.05385(14) 0.0319(7) Uani 1 1 d .
O1 O 0.6890(8) 0.1279(7) 0.0274(4) 0.0392(19) Uani 1 1 d .
C16 C 0.2905(14) 0.5237(11) 0.1286(6) 0.043(3) Uani 1 1 d .
H16 H 0.2369 0.4745 0.0900 0.052 Uiso 1 1 calc R
C15 C 0.4016(14) 0.4730(11) 0.1513(5) 0.043(3) Uani 1 1 d .
H15 H 0.4195 0.3861 0.1292 0.051 Uiso 1 1 calc R
C11 C 1.0002(12) 0.9637(11) 0.3072(6) 0.039(3) Uani 1 1 d .
H11 H 1.0756 1.0112 0.3379 0.047 Uiso 1 1 calc R
C9 C 0.9103(13) 0.8792(12) 0.1953(6) 0.041(3) Uani 1 1 d .
H9 H 0.9253 0.8669 0.1506 0.050 Uiso 1 1 calc R
C10 C 1.0213(13) 0.9431(11) 0.2397(6) 0.041(3) Uani 1 1 d .
H10 H 1.1123 0.9736 0.2255 0.049 Uiso 1 1 calc R
C1 C 0.9327(15) 0.2859(15) -0.0195(7) 0.058(4) Uani 1 1 d .
H1A H 0.9104 0.2049 -0.0559 0.086 Uiso 1 1 calc R
H1B H 1.0354 0.3124 -0.0107 0.086 Uiso 1 1 calc R
H1C H 0.8973 0.3626 -0.0302 0.086 Uiso 1 1 calc R
C22 C 0.3645(11) 1.1419(11) 0.4062(6) 0.037(3) Uani 1 1 d .
H22 H 0.3178 1.2144 0.4246 0.045 Uiso 1 1 calc R
C21 C 0.4476(13) 1.1525(10) 0.3536(6) 0.041(3) Uani 1 1 d .
H21 H 0.4581 1.2321 0.3366 0.049 Uiso 1 1 calc R
C23 C 0.3493(13) 1.0231(11) 0.4323(6) 0.041(3) Uani 1 1 d .
H23 H 0.2940 1.0181 0.4685 0.049 Uiso 1 1 calc R
C5 C 0.8400(12) 0.2883(11) 0.2897(5) 0.037(3) Uani 1 1 d .
H5A H 0.8380 0.2073 0.3074 0.055 Uiso 1 1 calc R
H5B H 0.8373 0.2604 0.2426 0.055 Uiso 1 1 calc R
H5C H 0.7577 0.3289 0.3032 0.055 Uiso 1 1 calc R
C3 C 0.8024(17) 0.4020(12) 0.1084(7) 0.058(4) Uani 1 1 d .
H3A H 0.7397 0.4411 0.0848 0.087 Uiso 1 1 calc R
H3B H 0.8899 0.4702 0.1232 0.087 Uiso 1 1 calc R
H3C H 0.7549 0.3772 0.1457 0.087 Uiso 1 1 calc R
C6 C 1.1747(13) 0.3536(11) 0.2997(6) 0.041(3) Uani 1 1 d .
H6A H 1.2564 0.4207 0.3229 0.062 Uiso 1 1 calc R
H6B H 1.1858 0.3393 0.2532 0.062 Uiso 1 1 calc R
H6C H 1.1687 0.2658 0.3121 0.062 Uiso 1 1 calc R
C2 C 0.9569(16) 0.1607(15) 0.0997(7) 0.063(4) Uani 1 1 d .
H2A H 0.9095 0.1442 0.1384 0.095 Uiso 1 1 calc R
H2B H 1.0494 0.2221 0.1123 0.095 Uiso 1 1 calc R
H2C H 0.9699 0.0727 0.0725 0.095 Uiso 1 1 calc R
C4 C 1.0097(15) 0.5890(12) 0.2951(6) 0.049(3) Uani 1 1 d .
H4A H 0.9321 0.6306 0.3146 0.074 Uiso 1 1 calc R
H4B H 0.9974 0.5700 0.2481 0.074 Uiso 1 1 calc R
H4C H 1.1001 0.6528 0.3097 0.074 Uiso 1 1 calc R
C17 C 0.2585(15) 0.6527(13) 0.1652(6) 0.050(3) Uani 1 1 d .
H17 H 0.1784 0.6842 0.1529 0.060 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'
Si Si 0.0817 0.0704 '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'
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
O2 U2 O2 180.000(1) 2_766 .
O2 U2 I4 90.0(2) 2_766 .
O2 U2 I4 90.0(2) . .
O2 U2 I4 90.0(2) 2_766 2_766
O2 U2 I4 90.0(2) . 2_766
I4 U2 I4 180.00(3) . 2_766
O2 U2 I3 90.82(18) 2_766 2_766
O2 U2 I3 89.18(18) . 2_766
I4 U2 I3 91.13(3) . 2_766
I4 U2 I3 88.87(3) 2_766 2_766
O2 U2 I3 89.18(18) 2_766 .
O2 U2 I3 90.82(18) . .
I4 U2 I3 88.87(3) . .
I4 U2 I3 91.13(3) 2_766 .
I3 U2 I3 180.0 2_766 .
C19 P1 C13 110.0(5) . .
C19 P1 C7 110.0(4) . .
C13 P1 C7 109.7(4) . .
C19 P1 I5 109.9(3) . .
C13 P1 I5 109.5(3) . .
C7 P1 I5 107.6(3) . .
O2 Si2 C6 107.1(5) . .
O2 Si2 C5 106.1(4) . .
C6 Si2 C5 113.7(5) . .
O2 Si2 C4 105.8(5) . .
C6 Si2 C4 112.0(5) . .
C5 Si2 C4 111.6(6) . .
Si2 O2 U2 177.8(4) . .
C8 C7 C12 119.9(9) . .
C8 C7 P1 120.8(8) . .
C12 C7 P1 119.3(7) . .
C18 C13 C14 117.8(10) . .
C18 C13 P1 120.9(7) . .
C14 C13 P1 121.3(9) . .
C23 C24 C19 120.7(9) . .
C15 C14 C13 122.0(12) . .
C11 C12 C7 120.3(9) . .
C21 C20 C19 120.7(9) . .
C7 C8 C9 119.5(12) . .
C17 C18 C13 120.9(10) . .
C20 C19 C24 117.9(9) . .
C20 C19 P1 118.2(6) . .
C24 C19 P1 123.4(7) . .
O1 U1 O1 180.0(8) 2_655 .
O1 U1 I1 90.4(2) 2_655 2_655
O1 U1 I1 89.6(2) . 2_655
O1 U1 I1 89.6(2) 2_655 .
O1 U1 I1 90.4(2) . .
I1 U1 I1 180.00(5) 2_655 .
O1 U1 I2 90.7(2) 2_655 .
O1 U1 I2 89.3(2) . .
I1 U1 I2 90.96(4) 2_655 .
I1 U1 I2 89.04(4) . .
O1 U1 I2 89.3(2) 2_655 2_655
O1 U1 I2 90.7(2) . 2_655
I1 U1 I2 89.04(4) 2_655 2_655
I1 U1 I2 90.96(4) . 2_655
I2 U1 I2 180.000(11) . 2_655
O1 Si1 C2 108.5(5) . .
O1 Si1 C1 107.1(5) . .
C2 Si1 C1 112.5(7) . .
O1 Si1 C3 107.8(6) . .
C2 Si1 C3 110.0(7) . .
C1 Si1 C3 110.6(6) . .
Si1 O1 U1 176.9(5) . .
C15 C16 C17 119.1(11) . .
C14 C15 C16 120.6(11) . .
C12 C11 C10 119.1(11) . .
C10 C9 C8 120.8(11) . .
C9 C10 C11 120.3(10) . .
C21 C22 C23 120.6(10) . .
C22 C21 C20 119.5(9) . .
C24 C23 C22 120.4(9) . .
C18 C17 C16 119.3(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U2 O2 1.990(6) 2_766
U2 O2 1.990(6) .
U2 I4 2.975(2) .
U2 I4 2.975(2) 2_766
U2 I3 2.975(2) 2_766
U2 I3 2.975(2) .
I5 P1 2.408(3) .
P1 C19 1.768(10) .
P1 C13 1.772(10) .
P1 C7 1.791(9) .
Si2 O2 1.674(7) .
Si2 C6 1.840(11) .
Si2 C5 1.861(11) .
Si2 C4 1.871(10) .
C7 C8 1.369(14) .
C7 C12 1.395(15) .
C13 C18 1.391(15) .
C13 C14 1.409(13) .
C24 C23 1.354(14) .
C24 C19 1.416(12) .
C14 C15 1.350(17) .
C12 C11 1.383(14) .
C20 C21 1.394(14) .
C20 C19 1.405(13) .
C8 C9 1.402(15) .
C18 C17 1.384(16) .
U1 O1 1.976(8) 2_655
U1 O1 1.976(8) .
U1 I1 2.9841(19) 2_655
U1 I1 2.9841(19) .
U1 I2 2.999(2) .
U1 I2 2.999(2) 2_655
Si1 O1 1.688(8) .
Si1 C2 1.838(13) .
Si1 C1 1.845(11) .
Si1 C3 1.847(12) .
C16 C15 1.376(17) .
C16 C17 1.424(16) .
C11 C10 1.402(16) .
C9 C10 1.350(18) .
C22 C21 1.370(15) .
C22 C23 1.398(16) .
