#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:49:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179079 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/41/4304124.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_4304124
loop_
_publ_author_name
'Nolan E. Dean'
'Robert D. Hancock'
'Christopher L. Cahill'
'Mark Frisch'
_publ_section_title
;
Affinity of the Highly Preorganized Ligand PDA
(1,10-Phenanthroline-2,9-dicarboxylic acid) for Large Metal Ions of Higher
Charge. A Crystallographic and Thermodynamic Study of PDA Complexes of
Thorium(IV) and the Uranyl(VI) ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2000
_journal_page_last               2010
_journal_paper_doi               10.1021/ic701574j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C14 H6 N2 O6 U'
_chemical_formula_sum            'C14 H6 N2 O6 U'
_chemical_formula_weight         536.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1318(7)
_cell_length_b                   6.6926(4)
_cell_length_c                   17.3114(12)
_cell_measurement_reflns_used    21066
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.18
_cell_volume                     1289.71(14)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2005)'
_computing_data_collection       'APEX II (Bruker AXS, 2005)'
_computing_data_reduction        'SAINTPLUS (Bruker AXS, 2005)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 2004)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20119
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    12.623
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0313
_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)+(0.0175P)²+3.0833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0527
_reflns_number_gt                1164
_reflns_number_total             1453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701574j-file001.cif
_cod_data_source_block           pnma
_cod_database_code               4304124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.28147(3) 0.2500 0.653852(18) 0.01974(10) Uani 1 2 d S . .
O1 O 0.2766(4) -0.0138(6) 0.6547(2) 0.0322(10) Uani 1 1 d . . .
O2 O 0.0921(5) 0.2500 0.7229(3) 0.0323(17) Uani 1 2 d S . .
O3 O -0.1085(5) 0.2500 0.7306(3) 0.0292(16) Uani 1 2 d S . .
O4 O 0.4724(6) 0.2500 0.6063(4) 0.0361(19) Uani 1 2 d S . .
O5 O 0.6146(5) 0.2500 0.5147(4) 0.057(3) Uani 1 2 d S . .
N1 N 0.0878(6) 0.2500 0.5729(4) 0.0164(16) Uani 1 2 d S . .
N2 N 0.3015(6) 0.2500 0.5075(4) 0.0207(17) Uani 1 2 d S . .
C13 C 0.4093(8) 0.2500 0.4770(5) 0.023(2) Uani 1 2 d S . .
C10 C 0.2063(7) 0.2500 0.4589(4) 0.0175(18) Uani 1 2 d S . .
C6 C 0.0914(7) 0.2500 0.4946(5) 0.0147(18) Uani 1 2 d S . .
C5 C -0.0132(7) 0.2500 0.4490(5) 0.0166(19) Uani 1 2 d S . .
C4 C -0.1233(7) 0.2500 0.4868(5) 0.021(2) Uani 1 2 d S . .
H4 H -0.1942 0.2500 0.4583 0.025 Uiso 1 2 calc SR . .
C3 C -0.1279(7) 0.2500 0.5659(5) 0.019(2) Uani 1 2 d S . .
H3 H -0.2012 0.2500 0.5916 0.023 Uiso 1 2 calc SR . .
C2 C -0.0205(8) 0.2500 0.6068(5) 0.018(2) Uani 1 2 d S . .
C14 C 0.5097(8) 0.2500 0.5352(6) 0.032(2) Uani 1 2 d S . .
C1 C -0.0113(8) 0.2500 0.6933(6) 0.026(2) Uani 1 2 d S . .
C7 C 0.0007(8) 0.2500 0.3665(5) 0.023(2) Uani 1 2 d S . .
H7 H -0.0673 0.2500 0.3354 0.027 Uiso 1 2 calc SR . .
C8 C 0.1097(8) 0.2500 0.3334(5) 0.027(2) Uani 1 2 d S . .
H8 H 0.1155 0.2500 0.2798 0.032 Uiso 1 2 calc SR . .
C9 C 0.2160(9) 0.2500 0.3783(4) 0.0239(19) Uani 1 2 d S . .
C11 C 0.3347(9) 0.2500 0.3479(6) 0.037(2) Uani 1 2 d S . .
H11 H 0.3469 0.2500 0.2948 0.045 Uiso 1 2 calc SR . .
C12 C 0.4306(8) 0.2500 0.3971(6) 0.036(3) Uani 1 2 d S . .
H12 H 0.5087 0.2500 0.3779 0.044 Uiso 1 2 calc SR . .
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
_geom_angle_publ_flag
O1 U1 O1 176.4(3) 7_565 . ?
O1 U1 O4 91.80(14) 7_565 . ?
O1 U1 O4 91.80(14) . . ?
O1 U1 O3 90.54(13) 7_565 6_657 ?
O1 U1 O3 90.54(13) . 6_657 ?
O4 U1 O3 79.7(2) . 6_657 ?
O1 U1 O2 88.25(14) 7_565 . ?
O1 U1 O2 88.25(14) . . ?
O4 U1 O2 171.6(2) . . ?
O3 U1 O2 91.9(2) 6_657 . ?
O1 U1 N2 90.60(13) 7_565 . ?
O1 U1 N2 90.60(13) . . ?
O4 U1 N2 63.8(2) . . ?
O3 U1 N2 143.49(19) 6_657 . ?
O2 U1 N2 124.6(2) . . ?
O1 U1 N1 88.77(13) 7_565 . ?
O1 U1 N1 88.77(13) . . ?
O4 U1 N1 125.8(2) . . ?
O3 U1 N1 154.5(2) 6_657 . ?
O2 U1 N1 62.58(19) . . ?
N2 U1 N1 62.0(2) . . ?
C1 O2 U1 126.5(6) . . ?
C1 O3 U1 152.3(6) . 6_557 ?
C14 O4 U1 129.8(6) . . ?
C2 N1 C6 117.6(7) . . ?
C2 N1 U1 121.1(6) . . ?
C6 N1 U1 121.3(5) . . ?
C13 N2 C10 117.8(8) . . ?
C13 N2 U1 118.8(6) . . ?
C10 N2 U1 123.4(5) . . ?
N2 C13 C12 123.5(8) . . ?
N2 C13 C14 114.1(8) . . ?
C12 C13 C14 122.4(8) . . ?
N2 C10 C9 124.0(8) . . ?
N2 C10 C6 115.7(7) . . ?
C9 C10 C6 120.3(8) . . ?
N1 C6 C5 122.4(8) . . ?
N1 C6 C10 117.5(7) . . ?
C5 C6 C10 120.0(8) . . ?
C4 C5 C6 117.8(8) . . ?
C4 C5 C7 124.3(8) . . ?
C6 C5 C7 118.0(8) . . ?
C3 C4 C5 120.2(8) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C3 C2 118.5(8) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
N1 C2 C3 123.5(8) . . ?
N1 C2 C1 112.0(8) . . ?
C3 C2 C1 124.5(8) . . ?
O5 C14 O4 125.6(9) . . ?
O5 C14 C13 121.0(9) . . ?
O4 C14 C13 113.4(8) . . ?
O3 C1 O2 125.2(9) . . ?
O3 C1 C2 117.0(8) . . ?
O2 C1 C2 117.9(8) . . ?
C8 C7 C5 121.5(8) . . ?
C8 C7 H7 119.2 . . ?
C5 C7 H7 119.2 . . ?
C7 C8 C9 121.4(8) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C10 C9 C8 118.9(8) . . ?
C10 C9 C11 116.2(8) . . ?
C8 C9 C11 125.0(7) . . ?
C12 C11 C9 119.7(9) . . ?
C12 C11 H11 120.1 . . ?
C9 C11 H11 120.1 . . ?
C11 C12 C13 118.8(9) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.767(4) 7_565 ?
U1 O1 1.767(4) . ?
U1 O4 2.279(6) . ?
U1 O3 2.345(6) 6_657 ?
U1 O2 2.423(6) . ?
U1 N2 2.543(7) . ?
U1 N1 2.572(7) . ?
O2 C1 1.261(10) . ?
O3 C1 1.260(10) . ?
O3 U1 2.345(6) 6_557 ?
O4 C14 1.298(11) . ?
O5 C14 1.220(10) . ?
N1 C2 1.340(10) . ?
N1 C6 1.356(9) . ?
N2 C13 1.312(10) . ?
N2 C10 1.353(10) . ?
C13 C12 1.404(12) . ?
C13 C14 1.505(12) . ?
C10 C9 1.399(10) . ?
C10 C6 1.421(10) . ?
C6 C5 1.406(11) . ?
C5 C4 1.390(11) . ?
C5 C7 1.436(11) . ?
C4 C3 1.370(11) . ?
C4 H4 0.9300 . ?
C3 C2 1.389(11) . ?
C3 H3 0.9300 . ?
C2 C1 1.502(11) . ?
C7 C8 1.342(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.417(12) . ?
C8 H8 0.9300 . ?
C9 C11 1.422(12) . ?
C11 C12 1.366(13) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
