#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:11:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179443 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/40/4334082.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_4334082
loop_
_publ_author_name
'Chao Xu'
'Guoxin Tian'
'Simon J. Teat'
'Linfeng Rao'
_publ_section_title
;
 Complexation of U(VI) with Dipicolinic Acid: Thermodynamics and
 Coordination Modes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2750
_journal_page_last               2756
_journal_paper_doi               10.1021/ic4000389
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C14 H22 N2 Na2 O18 U'
_chemical_formula_weight         790.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 124.316(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.397(8)
_cell_length_b                   7.036(4)
_cell_length_c                   13.178(11)
_cell_measurement_reflns_used    4333
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.95
_cell_measurement_theta_min      4.05
_cell_volume                     1179.1(13)
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchtrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8659
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         33.87
_diffrn_reflns_theta_min         4.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.845
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.216
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1962
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0336
_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)+(0.0674P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                1953
_reflns_number_total             1962
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic4000389_si_002.cif
_cod_data_source_block           udpa
_cod_database_code               4334082
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.0000 0.0000 0.0000 0.03050(11) Uani 1 4 d S
Na1 Na 0.2694(2) 0.0000 0.5232(3) 0.0431(6) Uani 1 2 d S
O1 O 0.0000 0.2491(9) 0.0000 0.0529(13) Uani 1 2 d S
O3 O 0.1484(5) 0.0000 0.2148(6) 0.0599(15) Uani 1 2 d SU
O4 O 0.0312(4) 0.0000 -0.1652(5) 0.0484(13) Uani 1 2 d S
O5 O 0.3131(4) 0.0000 0.3749(5) 0.0532(14) Uani 1 2 d S
O6 O 0.1236(5) 0.0000 -0.2481(5) 0.0589(17) Uani 1 2 d S
N1 N 0.1941(4) 0.0000 0.0564(5) 0.0321(9) Uani 1 2 d S
C7 C 0.1168(5) 0.0000 -0.1588(6) 0.0386(12) Uani 1 2 d S
C4 C 0.3996(6) 0.0000 0.1191(7) 0.0471(16) Uani 1 2 d S
H4A H 0.4682 0.0000 0.1401 0.056 Uiso 1 2 calc SR
C2 C 0.2763(5) 0.0000 0.1743(6) 0.0347(11) Uani 1 2 d S
C1 C 0.2461(6) 0.0000 0.2642(7) 0.0450(15) Uani 1 2 d S
C3 C 0.3796(5) 0.0000 0.2087(7) 0.0425(14) Uani 1 2 d S
H3A H 0.4348 0.0000 0.2914 0.051 Uiso 1 2 calc SR
C6 C 0.2144(4) 0.0000 -0.0298(6) 0.0319(10) Uani 1 2 d S
C5 C 0.3150(5) 0.0000 -0.0030(7) 0.0411(13) Uani 1 2 d S
H5A H 0.3258 0.0000 -0.0657 0.049 Uiso 1 2 calc SR
O1W O 0.3807(3) -0.2734(6) 0.6031(4) 0.0510(9) Uani 1 1 d .
O2W O 0.2782(9) 0.0000 0.7050(10) 0.090(3) Uani 1 2 d SU
O3W O 0.5000 0.206(2) 0.5000 0.057(3) Uani 0.50 2 d SP
O4W O 0.5000 -0.362(3) 0.5000 0.071(4) Uani 0.50 2 d SP
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Na Na 0.0394 0.0302
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
U U -8.0145 4.5872
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
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 . 5
O1 U1 O3 90.0 . .
O1 U1 O3 90.0 5 5
O1 U1 O3 90.0 . 5
O1 U1 O3 90.0 5 .
O1 U1 O4 90.0 . .
O1 U1 O4 90.0 5 5
O1 U1 O4 90.0 . 5
O1 U1 O4 90.0 5 .
O1 U1 N1 90.0 . .
O1 U1 N1 90.0 5 5
O1 U1 N1 90.0 . 5
O1 U1 N1 90.0 5 .
O3 U1 O3 180.0 . 5
O3 U1 O4 120.08(19) . .
O3 U1 O4 120.08(19) 5 5
O3 U1 O4 59.92(19) . 5
O3 U1 O4 59.92(19) 5 .
O3 U1 N1 60.15(18) . .
O3 U1 N1 60.15(18) 5 5
O3 U1 N1 119.85(18) . 5
O3 U1 N1 119.85(18) 5 .
O4 U1 O4 180.0 . 5
O4 U1 N1 59.93(16) . .
O4 U1 N1 59.93(16) 5 5
O4 U1 N1 120.07(16) . 5
O4 U1 N1 120.07(16) 5 .
N1 U1 N1 180.0 . 5
Na1 Na1 Na1 161.78(19) 7_546 7_556
Na1 Na1 O5 87.55(10) 7_546 .
Na1 Na1 O5 87.55(10) 7_556 .
Na1 Na1 O1W 151.58(18) 7_546 6
Na1 Na1 O1W 44.77(11) 7_546 .
Na1 Na1 O1W 42.05(11) 7_546 7_546
Na1 Na1 O1W 120.68(17) 7_546 4_556
Na1 Na1 O1W 44.77(11) 7_556 6
Na1 Na1 O1W 151.58(18) 7_556 .
Na1 Na1 O1W 120.68(17) 7_556 7_546
Na1 Na1 O1W 42.05(11) 7_556 4_556
Na1 Na1 O2W 94.79(11) 7_546 .
Na1 Na1 O2W 94.79(11) 7_556 .
O5 Na1 O1W 84.15(16) . .
O5 Na1 O1W 84.15(16) . 6
O5 Na1 O1W 92.08(18) . 7_546
O5 Na1 O1W 92.08(18) . 4_556
O5 Na1 O2W 163.8(3) . .
O1W Na1 O1W 107.2(2) . 6
O1W Na1 O1W 164.96(17) 6 7_546
O1W Na1 O1W 86.82(14) . 7_546
O1W Na1 O1W 86.82(14) 6 4_556
O1W Na1 O1W 164.96(17) . 4_556
O1W Na1 O1W 78.8(2) 7_546 4_556
O1W Na1 O2W 86.3(2) . .
O1W Na1 O2W 86.3(2) 6 .
O1W Na1 O2W 100.4(3) 7_546 .
O1W Na1 O2W 100.4(3) 4_556 .
U1 O3 C1 131.6(5) . .
U1 O4 C7 130.4(4) . .
Na1 O5 C1 122.5(5) . .
U1 N1 C2 120.3(4) . .
U1 N1 C6 122.0(4) . .
C2 N1 C6 117.7(5) . .
O4 C7 O6 125.2(6) . .
O4 C7 C6 114.3(5) . .
O6 C7 C6 120.6(6) . .
C3 C4 C5 118.5(6) . .
N1 C2 C1 113.9(5) . .
N1 C2 C3 122.5(6) . .
C1 C2 C3 123.5(6) . .
O3 C1 O5 125.1(7) . .
O3 C1 C2 113.9(6) . .
O5 C1 C2 121.0(6) . .
C4 C3 C2 119.3(6) . .
N1 C6 C7 113.4(5) . .
N1 C6 C5 123.3(6) . .
C7 C6 C5 123.3(6) . .
C4 C5 C6 118.7(6) . .
Na1 O1W Na1 93.18(14) . 7_546
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.753(6) .
U1 O1 1.753(6) 5
U1 O3 2.437(7) .
U1 O3 2.437(7) 5
U1 O4 2.479(5) .
U1 O4 2.479(5) 5
U1 N1 2.641(5) .
U1 N1 2.641(5) 5
Na1 Na1 3.563(2) 7_546
Na1 Na1 3.563(2) 7_556
Na1 O5 2.399(6) .
Na1 O1W 2.390(5) .
Na1 O1W 2.390(5) 6
Na1 O1W 2.513(5) 7_546
Na1 O1W 2.513(5) 4_556
Na1 O2W 2.322(10) .
O3 C1 1.259(9) .
O4 C7 1.274(8) .
O5 C1 1.223(9) .
O6 C7 1.239(8) .
N1 C2 1.341(8) .
N1 C6 1.337(8) .
C7 C6 1.506(9) .
C4 C3 1.377(10) .
C4 C5 1.387(10) .
C2 C1 1.495(9) .
C2 C3 1.386(8) .
C6 C5 1.381(8) .
O1W Na1 2.513(5) 7_546
O3W O4W 1.09(2) 5_656
O4W O3W 1.09(2) 5_656
