#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179355 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325237.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_4325237
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            'C40 H44 Cl4 N2 O4 U'
_chemical_formula_weight         996.60
_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                98.382(3)
_cell_angle_beta                 97.715(3)
_cell_angle_gamma                99.983(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5091(19)
_cell_length_b                   9.552(2)
_cell_length_c                   11.408(2)
_cell_measurement_temperature    150(2)
_cell_volume                     996.0(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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8559
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.384
_exptl_absorpt_correction_T_max  0.405
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0333
_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)+(0.0235P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                3893
_reflns_number_total             3968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200387n_si_001_1.cif
_cod_data_source_block           Complex_1
_cod_original_cell_volume        996.1(4)
_cod_database_code               4325237
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 0.5000 0.5000 0.0000 0.02286(8) Uani 1 2 d S
O2 O 0.6318(3) 0.3463(3) 0.0639(2) 0.0211(6) Uani 1 1 d .
O1 O 0.4825(3) 0.3989(3) -0.1459(2) 0.0229(6) Uani 1 1 d .
N1 N 0.2401(3) 0.3714(3) -0.0170(3) 0.0190(7) Uani 1 1 d .
C11 C 0.7320(4) 0.3812(4) 0.1595(3) 0.0191(8) Uani 1 1 d .
C1 C 0.1495(4) 0.3791(4) -0.1119(3) 0.0174(8) Uani 1 1 d .
C18 C 0.8299(4) 0.5090(4) 0.1843(3) 0.0208(9) Uani 1 1 d .
H18 H 0.8915 0.5262 0.2576 0.025 Uiso 1 1 calc R
C7 C 0.0190(4) 0.1450(4) -0.2385(3) 0.0235(9) Uani 1 1 d .
H7 H 0.1085 0.1235 -0.2497 0.028 Uiso 1 1 calc R
C2 C 0.0126(4) 0.2718(4) -0.1641(3) 0.0192(8) Uani 1 1 d .
C5 C -0.2400(5) 0.0809(4) -0.2813(4) 0.0275(10) Uani 1 1 d .
H5 H -0.3243 0.0167 -0.3192 0.033 Uiso 1 1 calc R
C13 C 0.6477(4) 0.1346(4) 0.2013(4) 0.0245(9) Uani 1 1 d .
H13 H 0.5934 0.1123 0.1245 0.029 Uiso 1 1 calc R
C12 C 0.7326(4) 0.2710(4) 0.2410(3) 0.0198(8) Uani 1 1 d .
C3 C -0.1232(4) 0.3036(4) -0.1526(4) 0.0252(9) Uani 1 1 d .
H3 H -0.1297 0.3899 -0.1060 0.030 Uiso 1 1 calc R
C8 C 0.2117(4) 0.2632(4) 0.0648(3) 0.0213(9) Uani 1 1 d .
C9 C 0.2581(5) 0.1237(4) 0.0118(4) 0.0279(10) Uani 1 1 d .
H9A H 0.1913 0.0770 -0.0595 0.042 Uiso 1 1 calc R
H9B H 0.2583 0.0602 0.0697 0.042 Uiso 1 1 calc R
H9C H 0.3535 0.1470 -0.0077 0.042 Uiso 1 1 calc R
C6 C -0.1067(5) 0.0500(4) -0.2964(4) 0.0278(10) Uani 1 1 d .
H6 H -0.1009 -0.0348 -0.3455 0.033 Uiso 1 1 calc R
C15 C 0.7230(4) 0.0635(4) 0.3887(4) 0.0282(10) Uani 1 1 d .
H15 H 0.7204 -0.0058 0.4382 0.034 Uiso 1 1 calc R
C14 C 0.6427(4) 0.0304(4) 0.2752(4) 0.0292(10) Uani 1 1 d .
H14 H 0.5854 -0.0609 0.2479 0.035 Uiso 1 1 calc R
C16 C 0.8068(5) 0.1983(5) 0.4291(4) 0.0307(10) Uani 1 1 d .
H16 H 0.8599 0.2204 0.5064 0.037 Uiso 1 1 calc R
C17 C 0.8131(4) 0.3022(4) 0.3556(4) 0.0276(9) Uani 1 1 d .
H17 H 0.8715 0.3929 0.3833 0.033 Uiso 1 1 calc R
C10 C 0.3078(4) 0.3271(5) 0.1852(4) 0.0286(10) Uani 1 1 d .
H10A H 0.4076 0.3372 0.1755 0.043 Uiso 1 1 calc R
H10B H 0.2884 0.2643 0.2420 0.043 Uiso 1 1 calc R
H10C H 0.2880 0.4200 0.2139 0.043 Uiso 1 1 calc R
C23 C 0.0553(4) 0.2297(5) 0.0880(4) 0.0307(10) Uani 1 1 d .
H23A H 0.0202 0.3180 0.1025 0.046 Uiso 1 1 calc R
H23B H 0.0521 0.1829 0.1568 0.046 Uiso 1 1 calc R
H23C H -0.0043 0.1673 0.0190 0.046 Uiso 1 1 calc R
C4 C -0.2474(4) 0.2088(5) -0.2092(4) 0.0291(10) Uani 1 1 d .
H4 H -0.3372 0.2304 -0.1991 0.035 Uiso 1 1 calc R
Cl1 Cl 0.18382(14) 0.31794(15) 0.49558(12) 0.0529(3) Uani 1 1 d .
Cl2 Cl 0.48359(14) 0.28349(15) 0.51856(13) 0.0537(3) Uani 1 1 d .
C19 C 0.3570(5) 0.3728(6) 0.5813(5) 0.0491(13) Uani 1 1 d .
H19A H 0.3533 0.3530 0.6620 0.059 Uiso 1 1 calc R
H19B H 0.3881 0.4761 0.5869 0.059 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'
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'
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
O1 U1 O1 180.0 2_665 .
O1 U1 O2 87.00(10) 2_665 2_665
O1 U1 O2 93.00(10) . 2_665
O1 U1 O2 93.00(10) 2_665 .
O1 U1 O2 87.00(10) . .
O2 U1 O2 180.0 2_665 .
O1 U1 N1 97.55(11) 2_665 .
O1 U1 N1 82.45(11) . .
O2 U1 N1 75.28(9) 2_665 .
O2 U1 N1 104.72(9) . .
O1 U1 N1 82.45(11) 2_665 2_665
O1 U1 N1 97.55(11) . 2_665
O2 U1 N1 104.72(9) 2_665 2_665
O2 U1 N1 75.28(9) . 2_665
N1 U1 N1 180.0 . 2_665
C11 O2 U1 123.1(2) . .
C1 N1 C8 124.2(3) . .
C1 N1 U1 117.4(2) . .
C8 N1 U1 116.5(2) . .
O2 C11 C18 122.7(3) . .
O2 C11 C12 115.5(3) . .
C18 C11 C12 121.9(3) . .
N1 C1 C18 124.5(3) . 2_665
N1 C1 C2 125.5(3) . .
C18 C1 C2 110.0(3) 2_665 .
C11 C18 C1 128.8(3) . 2_665
C6 C7 C2 120.7(4) . .
C7 C2 C3 118.3(4) . .
C7 C2 C1 119.6(3) . .
C3 C2 C1 121.6(3) . .
C6 C5 C4 119.4(4) . .
C12 C13 C14 120.7(4) . .
C13 C12 C17 118.9(3) . .
C13 C12 C11 118.9(3) . .
C17 C12 C11 122.2(4) . .
C4 C3 C2 120.8(4) . .
N1 C8 C10 106.6(3) . .
N1 C8 C23 115.0(3) . .
C10 C8 C23 107.5(3) . .
N1 C8 C9 108.2(3) . .
C10 C8 C9 109.0(3) . .
C23 C8 C9 110.4(3) . .
C5 C6 C7 120.2(4) . .
C16 C15 C14 120.2(4) . .
C15 C14 C13 119.6(4) . .
C15 C16 C17 120.5(4) . .
C12 C17 C16 120.2(4) . .
C3 C4 C5 120.5(4) . .
Cl1 C19 Cl2 111.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.770(3) 2_665
U1 O1 1.770(3) .
U1 O2 2.228(2) 2_665
U1 O2 2.228(2) .
U1 N1 2.531(3) .
U1 N1 2.531(3) 2_665
O2 C11 1.309(4) .
N1 C1 1.310(5) .
N1 C8 1.504(5) .
C11 C18 1.368(5) .
C11 C12 1.503(5) .
C1 C18 1.447(5) 2_665
C1 C2 1.500(5) .
C18 C1 1.447(5) 2_665
C7 C6 1.387(6) .
C7 C2 1.390(5) .
C2 C3 1.395(5) .
C5 C6 1.377(6) .
C5 C4 1.388(6) .
C13 C12 1.386(5) .
C13 C14 1.393(6) .
C12 C17 1.387(5) .
C3 C4 1.373(6) .
C8 C10 1.523(5) .
C8 C23 1.533(5) .
C8 C9 1.541(5) .
C15 C16 1.371(6) .
C15 C14 1.375(6) .
C16 C17 1.388(5) .
Cl1 C19 1.750(5) .
Cl2 C19 1.761(5) .
