#------------------------------------------------------------------------------
#$Date: 2016-12-23 17:13:03 +0200 (Fri, 23 Dec 2016) $
#$Revision: 189367 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/41/4304125.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_4304125
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         'C28 H18 N4 O11 Th'
_chemical_formula_sum            'C28 H18 N4 O11 Th'
_chemical_formula_weight         818.50
_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                94.93(3)
_cell_angle_beta                 97.57(3)
_cell_angle_gamma                109.26(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6190(15)
_cell_length_b                   10.423(2)
_cell_length_c                   17.367(4)
_cell_measurement_reflns_used    10511
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.09
_cell_volume                     1278.2(5)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '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  0.1122
_diffrn_reflns_av_sigmaI/netI    0.1851
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9412
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    5.909
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0267P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                2796
_reflns_number_total             4474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701574j-file002.cif
_cod_data_source_block           pbar1
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-23
;
_cod_original_cell_volume        1278.3(4)
_cod_database_code               4304125
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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Th1 Th 0.52989(8) 0.34221(6) 0.77701(4) 0.02690(17) Uani 1 1 d . . . 0
O2 O 0.9393(13) 0.1216(10) 0.7751(6) 0.049(3) Uani 1 1 d . . . 0
O5 O 0.6248(14) 0.5367(9) 0.8772(6) 0.043(3) Uani 1 1 d . . . 0
O6 O 0.7170(15) 0.6537(10) 0.9974(6) 0.051(3) Uani 1 1 d . . . 0
O4 O 0.0920(14) 0.5317(10) 0.6854(7) 0.053(3) Uani 1 1 d . . . 0
O3 O 0.3186(14) 0.4727(10) 0.7541(6) 0.048(3) Uani 1 1 d . . . 0
O1 O 0.8311(12) 0.2976(10) 0.7960(6) 0.038(3) Uani 1 1 d . . . 0
OW1 O 0.2755(12) 0.2649(9) 0.8555(6) 0.039(3) Uani 1 1 d . . . 2
OW2 O 0.7826(12) 0.5413(9) 0.7383(6) 0.042(3) Uani 1 1 d . . . 2
OW3 O 0.8861(15) 0.8227(10) 0.7600(8) 0.077(4) Uani 1 1 d . . . 2
N3 N 0.6622(14) 0.3187(11) 0.9226(7) 0.026(3) Uani 1 1 d . . . 0
N2 N 0.4002(15) 0.3691(11) 0.6263(8) 0.037(3) Uani 1 1 d . . . 0
N1 N 0.6622(15) 0.2509(11) 0.6533(7) 0.036(3) Uani 1 1 d . . . 0
N4 N 0.4969(16) 0.0963(11) 0.8168(8) 0.035(3) Uani 1 1 d . . . 0
C25 C 0.509(2) -0.1575(16) 0.8443(11) 0.052(5) Uani 1 1 d . . . 0
H25 H 0.5190 -0.2427 0.8508 0.063 Uiso 1 1 calc R . . 0
C6 C 0.5890(19) 0.2514(13) 0.5771(9) 0.033(4) Uani 1 1 d . . . 0
C15 C 0.6887(19) 0.5491(14) 0.9510(10) 0.029(4) Uani 1 1 d . . . 0
C11 C 0.228(3) 0.3761(17) 0.4798(12) 0.062(6) Uani 1 1 d . . . 0
H11 H 0.1680 0.3793 0.4301 0.075 Uiso 1 1 calc R . . 0
C5 C 0.644(2) 0.1934(15) 0.5137(9) 0.040(4) Uani 1 1 d . . . 0
C17 C 0.824(2) 0.4268(15) 1.0534(9) 0.039(4) Uani 1 1 d . . . 0
H17 H 0.8613 0.5040 1.0910 0.047 Uiso 1 1 calc R . . 0
C2 C 0.783(2) 0.1903(14) 0.6657(9) 0.035(4) Uani 1 1 d . . . 0
C18 C 0.857(2) 0.3112(16) 1.0701(9) 0.040(4) Uani 1 1 d . . . 0
H18 H 0.9261 0.3105 1.1184 0.048 Uiso 1 1 calc R . . 0
C10 C 0.449(2) 0.3154(14) 0.5629(10) 0.037(4) Uani 1 1 d . . . 0
C1 C 0.8595(19) 0.2041(13) 0.7530(9) 0.033(4) Uani 1 1 d . . . 0
C9 C 0.368(2) 0.3138(16) 0.4855(10) 0.048(4) Uani 1 1 d . . . 0
C13 C 0.269(2) 0.4270(14) 0.6171(10) 0.039(4) Uani 1 1 d . . . 0
C24 C 0.5995(19) 0.0823(14) 0.8829(10) 0.033(4) Uani 1 1 d . . . 0
C22 C 0.722(2) -0.0484(16) 0.9713(11) 0.051(5) Uani 1 1 d . . . 0
H22 H 0.7401 -0.1301 0.9801 0.061 Uiso 1 1 calc R . . 0
C3 C 0.844(2) 0.1241(14) 0.6075(10) 0.040(4) Uani 1 1 d . . . 0
H3 H 0.9279 0.0783 0.6199 0.048 Uiso 1 1 calc R . . 0
C16 C 0.730(2) 0.4266(13) 0.9774(10) 0.032(4) Uani 1 1 d . . . 0
C20 C 0.689(2) 0.2020(14) 0.9413(9) 0.034(4) Uani 1 1 d . . . 0
C19 C 0.7889(19) 0.1932(15) 1.0146(10) 0.039(4) Uani 1 1 d . . . 0
C8 C 0.430(2) 0.2555(17) 0.4242(10) 0.054(5) Uani 1 1 d . . . 0
H8 H 0.3759 0.2552 0.3729 0.064 Uiso 1 1 calc R . . 0
C4 C 0.776(2) 0.1287(16) 0.5300(11) 0.052(5) Uani 1 1 d . . . 0
H4 H 0.8170 0.0889 0.4894 0.063 Uiso 1 1 calc R . . 0
C14 C 0.216(2) 0.4800(15) 0.6892(10) 0.044(4) Uani 1 1 d . . . 0
C7 C 0.565(3) 0.2002(16) 0.4361(10) 0.058(5) Uani 1 1 d . . . 0
H7 H 0.6067 0.1661 0.3936 0.070 Uiso 1 1 calc R . . 0
C12 C 0.177(2) 0.4313(16) 0.5431(10) 0.049(5) Uani 1 1 d . . . 0
H12 H 0.0831 0.4705 0.5373 0.059 Uiso 1 1 calc R . . 0
C23 C 0.6110(19) -0.0453(14) 0.9006(9) 0.033(4) Uani 1 1 d . . . 0
C21 C 0.803(2) 0.0616(16) 1.0271(10) 0.046(4) Uani 1 1 d . . . 0
H21 H 0.8680 0.0525 1.0742 0.055 Uiso 1 1 calc R . . 0
O7 O 0.2958(12) 0.1422(9) 0.6992(5) 0.034(2) Uani 1 1 d . . . 0
C28 C 0.267(2) 0.0159(17) 0.7004(9) 0.038(4) Uani 1 1 d . . . 0
O8 O 0.1449(15) -0.0836(11) 0.6596(7) 0.057(3) Uani 1 1 d . . . 0
C27 C 0.392(2) -0.0154(13) 0.7687(9) 0.036(4) Uani 1 1 d . . . 0
C26 C 0.395(2) -0.1458(14) 0.7796(10) 0.043(4) Uani 1 1 d . . . 0
H26 H 0.3213 -0.2225 0.7440 0.052 Uiso 1 1 calc R . . 0
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'
Th Th -7.2400 8.8979 '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'
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
O5 Th1 O7 152.0(3) . . ?
O5 Th1 O3 70.8(3) . . ?
O7 Th1 O3 90.3(3) . . ?
O5 Th1 OW1 80.1(3) . . ?
O7 Th1 OW1 74.2(3) . . ?
O3 Th1 OW1 71.4(3) . . ?
O5 Th1 O1 96.5(3) . . ?
O7 Th1 O1 107.4(3) . . ?
O3 Th1 O1 157.8(3) . . ?
OW1 Th1 O1 125.6(3) . . ?
O5 Th1 OW2 70.0(3) . . ?
O7 Th1 OW2 131.1(3) . . ?
O3 Th1 OW2 86.9(3) . . ?
OW1 Th1 OW2 147.6(3) . . ?
O1 Th1 OW2 71.5(3) . . ?
O5 Th1 N4 119.6(4) . . ?
O7 Th1 N4 60.7(4) . . ?
O3 Th1 N4 135.7(3) . . ?
OW1 Th1 N4 68.9(3) . . ?
O1 Th1 N4 66.2(3) . . ?
OW2 Th1 N4 137.3(3) . . ?
O5 Th1 N3 60.5(3) . . ?
O7 Th1 N3 117.5(3) . . ?
O3 Th1 N3 120.1(3) . . ?
OW1 Th1 N3 67.9(3) . . ?
O1 Th1 N3 63.8(3) . . ?
OW2 Th1 N3 105.7(3) . . ?
N4 Th1 N3 60.1(4) . . ?
O5 Th1 N1 138.6(3) . . ?
O7 Th1 N1 68.5(3) . . ?
O3 Th1 N1 118.8(3) . . ?
OW1 Th1 N1 141.0(3) . . ?
O1 Th1 N1 59.0(3) . . ?
OW2 Th1 N1 70.6(3) . . ?
N4 Th1 N1 82.9(3) . . ?
N3 Th1 N1 120.6(3) . . ?
O5 Th1 N2 119.2(3) . . ?
O7 Th1 N2 63.2(3) . . ?
O3 Th1 N2 60.4(3) . . ?
OW1 Th1 N2 113.1(3) . . ?
O1 Th1 N2 115.3(3) . . ?
OW2 Th1 N2 73.3(3) . . ?
N4 Th1 N2 120.4(4) . . ?
N3 Th1 N2 178.9(4) . . ?
N1 Th1 N2 58.8(3) . . ?
C15 O5 Th1 130.6(9) . . ?
C14 O3 Th1 130.0(9) . . ?
C1 O1 Th1 122.5(9) . . ?
C16 N3 C20 116.6(13) . . ?
C16 N3 Th1 120.8(9) . . ?
C20 N3 Th1 121.9(10) . . ?
C13 N2 C10 119.4(14) . . ?
C13 N2 Th1 116.8(10) . . ?
C10 N2 Th1 123.4(10) . . ?
C2 N1 C6 117.7(12) . . ?
C2 N1 Th1 119.1(10) . . ?
C6 N1 Th1 122.7(8) . . ?
C27 N4 C24 118.3(13) . . ?
C27 N4 Th1 120.4(10) . . ?
C24 N4 Th1 121.1(9) . . ?
C26 C25 C23 121.6(14) . . ?
C26 C25 H25 119.2 . . ?
C23 C25 H25 119.2 . . ?
N1 C6 C5 123.0(13) . . ?
N1 C6 C10 117.9(13) . . ?
C5 C6 C10 119.1(15) . . ?
O6 C15 O5 123.3(13) . . ?
O6 C15 C16 121.7(15) . . ?
O5 C15 C16 115.0(13) . . ?
C12 C11 C9 123.4(17) . . ?
C12 C11 H11 118.3 . . ?
C9 C11 H11 118.3 . . ?
C6 C5 C4 117.3(15) . . ?
C6 C5 C7 120.0(14) . . ?
C4 C5 C7 122.8(15) . . ?
C18 C17 C16 118.3(14) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
N1 C2 C3 124.8(15) . . ?
N1 C2 C1 111.7(12) . . ?
C3 C2 C1 123.5(13) . . ?
C17 C18 C19 120.0(15) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
N2 C10 C9 124.4(14) . . ?
N2 C10 C6 116.6(15) . . ?
C9 C10 C6 119.0(14) . . ?
O2 C1 O1 126.9(15) . . ?
O2 C1 C2 117.9(12) . . ?
O1 C1 C2 115.1(12) . . ?
C8 C9 C10 119.3(16) . . ?
C8 C9 C11 127.4(17) . . ?
C10 C9 C11 113.4(15) . . ?
N2 C13 C12 121.9(14) . . ?
N2 C13 C14 117.1(15) . . ?
C12 C13 C14 120.8(14) . . ?
N4 C24 C23 123.4(14) . . ?
N4 C24 C20 117.8(12) . . ?
C23 C24 C20 118.6(15) . . ?
C21 C22 C23 123.1(14) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C4 C3 C2 117.8(14) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
N3 C16 C17 124.4(12) . . ?
N3 C16 C15 112.0(14) . . ?
C17 C16 C15 123.5(14) . . ?
N3 C20 C19 123.4(14) . . ?
N3 C20 C24 115.6(14) . . ?
C19 C20 C24 121.0(13) . . ?
C18 C19 C20 117.2(14) . . ?
C18 C19 C21 125.4(16) . . ?
C20 C19 C21 117.3(14) . . ?
C7 C8 C9 122.6(17) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C3 C4 C5 119.4(14) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
O4 C14 O3 124.9(16) . . ?
O4 C14 C13 121.0(15) . . ?
O3 C14 C13 114.0(14) . . ?
C8 C7 C5 120.0(15) . . ?
C8 C7 H7 120.0 . . ?
C5 C7 H7 120.0 . . ?
C11 C12 C13 117.5(15) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C25 C23 C22 125.9(14) . . ?
C25 C23 C24 115.4(15) . . ?
C22 C23 C24 118.7(14) . . ?
C22 C21 C19 120.9(16) . . ?
C22 C21 H21 119.6 . . ?
C19 C21 H21 119.6 . . ?
C28 O7 Th1 131.1(10) . . ?
O8 C28 O7 129.1(16) . . ?
O8 C28 C27 116.4(14) . . ?
O7 C28 C27 114.2(14) . . ?
N4 C27 C26 122.9(16) . . ?
N4 C27 C28 112.2(13) . . ?
C26 C27 C28 124.9(14) . . ?
C25 C26 C27 118.1(15) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
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
Th1 O5 2.399(10) . ?
Th1 O7 2.405(9) . ?
Th1 O3 2.443(9) . ?
Th1 OW1 2.473(9) . ?
Th1 O1 2.474(8) . ?
Th1 OW2 2.532(9) . ?
Th1 N4 2.652(11) . ?
Th1 N3 2.658(12) . ?
Th1 N1 2.718(11) . ?
Th1 N2 2.744(13) . ?
O2 C1 1.264(15) . ?
O5 C15 1.289(17) . ?
O6 C15 1.238(15) . ?
O4 C14 1.232(16) . ?
O3 C14 1.307(17) . ?
O1 C1 1.270(14) . ?
N3 C16 1.320(17) . ?
N3 C20 1.357(16) . ?
N2 C13 1.325(15) . ?
N2 C10 1.342(18) . ?
N1 C2 1.287(15) . ?
N1 C6 1.367(17) . ?
N4 C27 1.317(15) . ?
N4 C24 1.349(18) . ?
C25 C26 1.37(2) . ?
C25 C23 1.39(2) . ?
C25 H25 0.9300 . ?
C6 C5 1.389(19) . ?
C6 C10 1.442(18) . ?
C15 C16 1.506(18) . ?
C11 C12 1.36(2) . ?
C11 C9 1.42(2) . ?
C11 H11 0.9300 . ?
C5 C4 1.396(19) . ?
C5 C7 1.42(2) . ?
C17 C18 1.358(18) . ?
C17 C16 1.41(2) . ?
C17 H17 0.9300 . ?
C2 C3 1.388(19) . ?
C2 C1 1.53(2) . ?
C18 C19 1.397(19) . ?
C18 H18 0.9300 . ?
C10 C9 1.40(2) . ?
C9 C8 1.39(2) . ?
C13 C12 1.39(2) . ?
C13 C14 1.48(2) . ?
C24 C23 1.418(18) . ?
C24 C20 1.445(19) . ?
C22 C21 1.35(2) . ?
C22 C23 1.40(2) . ?
C22 H22 0.9300 . ?
C3 C4 1.39(2) . ?
C3 H3 0.9300 . ?
C20 C19 1.42(2) . ?
C19 C21 1.442(19) . ?
C8 C7 1.335(19) . ?
C8 H8 0.9300 . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C12 H12 0.9300 . ?
C21 H21 0.9300 . ?
O7 C28 1.264(15) . ?
C28 O8 1.228(17) . ?
C28 C27 1.55(2) . ?
C27 C26 1.396(18) . ?
C26 H26 0.9300 . ?
