#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:42:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179390 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/87/4328709.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_4328709
loop_
_publ_author_name
'Sinisa Vukovic'
'Lori A. Watson'
'Sung Ok Kang'
'Radu Custelcean'
'Benjamin P. Hay'
_publ_contact_author_email       custelceanr@ornl.gov
_publ_contact_author_name        'Custelcean Radu'
_publ_section_title
;
 How Amidoximate Binds the Uranyl Cation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3855
_journal_page_last               3859
_journal_paper_doi               10.1021/ic300062s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C16 H22 N4 O6 U'
_chemical_formula_weight         604.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.6170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5257(8)
_cell_length_b                   5.7345(5)
_cell_length_c                   16.0667(13)
_cell_measurement_temperature    173(2)
_cell_volume                     946.36(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8915
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    8.616
_exptl_absorpt_correction_T_max  0.8465
_exptl_absorpt_correction_T_min  0.2913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0180
_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)+(0.0229P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0437
_reflns_number_gt                1856
_reflns_number_total             2351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300062s_si_002.cif
_cod_data_source_block           c:\frames\403\work\p21c
_cod_database_code               4328709
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.5000 0.01493(5) Uani 1 2 d S
O1 O 0.03008(18) 0.3017(3) 0.40698(12) 0.0196(4) Uani 1 1 d .
N1 N 0.0952(3) 0.2322(5) 0.26099(17) 0.0276(6) Uani 1 1 d .
C1 C 0.1608(3) 0.1215(5) 0.33071(17) 0.0172(5) Uani 1 1 d .
H1N H 0.052(3) 0.344(7) 0.273(2) 0.044(11) Uiso 1 1 d .
H1O H 0.107(5) -0.455(7) 0.461(3) 0.048(14) Uiso 1 1 d .
O2 O 0.1364(2) -0.3235(4) 0.47798(13) 0.0219(4) Uani 1 1 d .
N2 N 0.1339(2) 0.1445(4) 0.40499(14) 0.0192(5) Uani 1 1 d .
C2 C 0.2669(3) -0.0426(5) 0.32336(19) 0.0183(6) Uani 1 1 d .
H2N H 0.127(3) 0.236(6) 0.221(2) 0.032(10) Uiso 1 1 d .
O3 O 0.11871(18) 0.1223(4) 0.58652(11) 0.0201(4) Uani 1 1 d .
C3 C 0.2509(3) -0.2047(5) 0.25779(19) 0.0266(7) Uani 1 1 d .
H3 H 0.1728 -0.2059 0.2149 0.032 Uiso 1 1 calc R
C4 C 0.3484(3) -0.3647(6) 0.2546(2) 0.0306(7) Uani 1 1 d .
H4 H 0.3355 -0.4785 0.2106 0.037 Uiso 1 1 calc R
C5 C 0.4638(3) -0.3601(6) 0.3148(2) 0.0297(7) Uani 1 1 d .
H5 H 0.5303 -0.4704 0.3124 0.036 Uiso 1 1 calc R
C6 C 0.4825(3) -0.1931(6) 0.37898(18) 0.0310(7) Uani 1 1 d .
H6 H 0.5629 -0.1863 0.4196 0.037 Uiso 1 1 calc R
C7 C 0.3841(3) -0.0367(5) 0.3837(2) 0.0262(7) Uani 1 1 d .
H7 H 0.3966 0.0752 0.4284 0.031 Uiso 1 1 calc R
C8 C 0.2617(3) -0.3838(6) 0.5277(2) 0.0331(7) Uani 1 1 d .
H8A H 0.3081 -0.2417 0.5507 0.050 Uiso 1 1 calc R
H8B H 0.3114 -0.4657 0.4918 0.050 Uiso 1 1 calc R
H8C H 0.2515 -0.4854 0.5749 0.050 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'
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
O3 U1 O3 180.0 3_556 .
O3 U1 O1 92.13(8) 3_556 3_556
O3 U1 O1 87.87(8) . 3_556
O3 U1 O1 87.87(8) 3_556 .
O3 U1 O1 92.13(8) . .
O1 U1 O1 180.0 3_556 .
O3 U1 O2 85.55(8) 3_556 .
O3 U1 O2 94.45(8) . .
O1 U1 O2 72.27(7) 3_556 .
O1 U1 O2 107.73(7) . .
O3 U1 O2 94.45(8) 3_556 3_556
O3 U1 O2 85.55(8) . 3_556
O1 U1 O2 107.73(7) 3_556 3_556
O1 U1 O2 72.27(7) . 3_556
O2 U1 O2 179.998(1) . 3_556
O3 U1 N2 87.27(8) 3_556 3_556
O3 U1 N2 92.73(8) . 3_556
O1 U1 N2 34.49(7) 3_556 3_556
O1 U1 N2 145.51(7) . 3_556
O2 U1 N2 105.89(7) . 3_556
O2 U1 N2 74.11(7) 3_556 3_556
O3 U1 N2 92.73(8) 3_556 .
O3 U1 N2 87.27(8) . .
O1 U1 N2 145.51(7) 3_556 .
O1 U1 N2 34.49(7) . .
O2 U1 N2 74.11(7) . .
O2 U1 N2 105.89(7) 3_556 .
N2 U1 N2 180.0 3_556 .
N2 O1 U1 76.04(12) . .
N2 C1 N1 123.1(3) . .
N2 C1 C2 117.3(2) . .
N1 C1 C2 119.5(2) . .
C8 O2 U1 127.54(19) . .
C1 N2 O1 114.2(2) . .
C1 N2 U1 144.8(2) . .
O1 N2 U1 69.47(11) . .
C3 C2 C7 119.2(3) . .
C3 C2 C1 121.1(3) . .
C7 C2 C1 119.8(3) . .
C4 C3 C2 120.2(3) . .
C5 C4 C3 120.5(3) . .
C4 C5 C6 119.6(3) . .
C7 C6 C5 120.1(3) . .
C6 C7 C2 120.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O3 1.7962(19) 3_556
U1 O3 1.7962(19) .
U1 O1 2.3525(18) 3_556
U1 O1 2.3525(18) .
U1 O2 2.419(2) .
U1 O2 2.419(2) 3_556
U1 N2 2.438(2) 3_556
U1 N2 2.438(2) .
O1 N2 1.422(3) .
N1 C1 1.341(4) .
C1 N2 1.292(3) .
C1 C2 1.485(4) .
O2 C8 1.427(3) .
C2 C3 1.387(4) .
C2 C7 1.393(4) .
C3 C4 1.386(4) .
C4 C5 1.378(4) .
C5 C6 1.389(4) .
C6 C7 1.385(4) .
