#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:12:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179780 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/76/7007653.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_7007653
loop_
_publ_author_name
'Frisch, Mark'
'Cahill, Christopher L.'
_publ_section_title
;
 Synthesis, structure and fluorescent studies of novel uranium
 coordination polymers in the pyridinedicarboxylic acid system.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4679
_journal_page_last               4690
_journal_paper_doi               10.1039/b608187h
_journal_year                    2006
_chemical_formula_moiety         'C7 H3 N O10 U2'
_chemical_formula_sum            'C7 H3 N O10 U2'
_chemical_formula_weight         737.16
_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                86.151(2)
_cell_angle_beta                 71.627(2)
_cell_angle_gamma                77.395(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7478(10)
_cell_length_b                   9.1757(11)
_cell_length_c                   9.3460(12)
_cell_measurement_reflns_used    3348
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      2.27
_cell_volume                     615.35(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0940
_diffrn_reflns_av_sigmaI/netI    0.1078
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11904
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    26.335
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.790
_refine_diff_density_min         -2.316
_refine_diff_density_rms         0.494
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0471
_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)+(0.0305P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                2209
_reflns_number_total             3336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608187h.txt
_cod_data_source_block           pbar1
_cod_database_code               7007653
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
U1 U 0.28490(6) 0.95934(5) 0.13822(5) 0.00912(14) Uani 1 1 d . . .
U2 U 0.72281(6) 0.63879(5) 0.07009(5) 0.00891(13) Uani 1 1 d . . .
O1 O 0.1523(11) 0.6455(10) 0.4165(10) 0.016(2) Uani 1 1 d . . .
O2 O 0.5898(12) 0.8606(9) 0.0144(10) 0.014(2) Uani 1 1 d . . .
O3 O 0.7936(12) 0.7165(10) 0.2084(10) 0.016(2) Uani 1 1 d . . .
O4 O 0.3935(11) 0.6961(9) 0.2249(9) 0.0115(13) Uani 1 1 d . . .
O5 O 0.9503(12) 0.4009(9) 0.0875(9) 0.0115(13) Uani 1 1 d . . .
O6 O 0.6739(12) 0.5518(10) -0.0735(10) 0.014(2) Uani 1 1 d . . .
O7 O 0.3366(12) 1.0123(10) 0.2958(10) 0.015(2) Uani 1 1 d . . .
O9 O 0.2164(12) 0.8991(9) -0.0064(10) 0.013(2) Uani 1 1 d . . .
O10 O 0.0374(13) 1.1819(9) 0.1824(11) 0.019(2) Uani 1 1 d . . .
N1 N 0.6064(13) 0.4397(11) 0.2621(11) 0.009(2) Uani 1 1 d . . .
C1 C 0.3114(19) 0.6145(14) 0.3305(14) 0.012(2) Uani 1 1 d . . .
C2 C 0.9136(19) 0.2951(13) 0.1774(14) 0.012(2) Uani 1 1 d . . .
C3 C 0.3543(18) 0.3555(13) 0.4503(14) 0.0137(19) Uani 1 1 d . . .
H3 H 0.2295 0.3747 0.5077 0.016 Uiso 1 1 calc R . .
C4 C 0.4712(17) 0.2217(13) 0.4630(14) 0.0116(19) Uani 1 1 d . . .
H4 H 0.4244 0.1484 0.5280 0.014 Uiso 1 1 calc R . .
C5 C 0.7175(16) 0.3075(13) 0.2764(13) 0.007(2) Uani 1 1 d . . .
C6 C 0.4290(17) 0.4614(13) 0.3487(14) 0.0116(19) Uani 1 1 d . . .
C7 C 0.6596(18) 0.1955(14) 0.3787(13) 0.0137(19) Uani 1 1 d . . .
H7 H 0.7422 0.1085 0.3898 0.016 Uiso 1 1 calc R . .
O8 O -0.0052(12) 0.8859(9) 0.3074(10) 0.0138(19) Uiso 1 1 d . . .
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
O9 U1 O7 174.5(4) . . ?
O9 U1 O2 91.2(4) . 2_675 ?
O7 U1 O2 93.9(4) . 2_675 ?
O9 U1 O2 90.8(4) . . ?
O7 U1 O2 92.9(4) . . ?
O2 U1 O2 71.6(3) 2_675 . ?
O9 U1 O10 91.7(4) . . ?
O7 U1 O10 87.5(4) . . ?
O2 U1 O10 74.3(3) 2_675 . ?
O2 U1 O10 145.8(3) . . ?
O9 U1 O8 83.8(4) . . ?
O7 U1 O8 90.7(3) . . ?
O2 U1 O8 146.4(3) 2_675 . ?
O2 U1 O8 141.4(3) . . ?
O10 U1 O8 72.7(3) . . ?
O9 U1 O4 94.3(3) . . ?
O7 U1 O4 83.4(3) . . ?
O2 U1 O4 138.4(3) 2_675 . ?
O2 U1 O4 67.1(3) . . ?
O10 U1 O4 146.5(3) . . ?
O8 U1 O4 75.2(3) . . ?
O9 U1 U1 91.2(3) . 2_675 ?
O7 U1 U1 94.2(3) . 2_675 ?
O2 U1 U1 35.8(2) 2_675 2_675 ?
O2 U1 U1 35.8(2) . 2_675 ?
O10 U1 U1 110.1(2) . 2_675 ?
O8 U1 U1 174.45(19) . 2_675 ?
O4 U1 U1 102.77(19) . 2_675 ?
O9 U1 U2 93.6(3) . . ?
O7 U1 U2 87.7(3) . . ?
O2 U1 U2 100.2(2) 2_675 . ?
O2 U1 U2 28.8(2) . . ?
O10 U1 U2 172.4(2) . . ?
O8 U1 U2 113.3(2) . . ?
O4 U1 U2 38.36(18) . . ?
U1 U1 U2 64.425(16) 2_675 . ?
O9 U1 U2 87.6(3) . 2_675 ?
O7 U1 U2 96.1(3) . 2_675 ?
O2 U1 U2 24.3(2) 2_675 2_675 ?
O2 U1 U2 95.7(2) . 2_675 ?
O10 U1 U2 50.5(2) . 2_675 ?
O8 U1 U2 122.1(2) . 2_675 ?
O4 U1 U2 162.67(19) . 2_675 ?
U1 U1 U2 59.936(14) 2_675 2_675 ?
U2 U1 U2 124.361(14) . 2_675 ?
O6 U2 O3 174.7(4) . . ?
O6 U2 O2 92.7(4) . . ?
O3 U2 O2 90.9(4) . . ?
O6 U2 O5 88.5(4) . 2_765 ?
O3 U2 O5 86.7(3) . 2_765 ?
O2 U2 O5 106.3(3) . 2_765 ?
O6 U2 O4 92.8(4) . . ?
O3 U2 O4 92.1(3) . . ?
O2 U2 O4 70.1(3) . . ?
O5 U2 O4 176.3(3) 2_765 . ?
O6 U2 O5 88.1(3) . . ?
O3 U2 O5 87.5(3) . . ?
O2 U2 O5 165.2(3) . . ?
O5 U2 O5 58.9(3) 2_765 . ?
O4 U2 O5 124.6(3) . . ?
O6 U2 N1 90.8(4) . . ?
O3 U2 N1 89.6(4) . . ?
O2 U2 N1 133.1(3) . . ?
O5 U2 N1 120.5(3) 2_765 . ?
O4 U2 N1 63.0(3) . . ?
O5 U2 N1 61.6(3) . . ?
O6 U2 U1 94.2(3) . . ?
O3 U2 U1 90.9(3) . . ?
O2 U2 U1 30.3(2) . . ?
O5 U2 U1 136.54(19) 2_765 . ?
O4 U2 U1 39.87(18) . . ?
O5 U2 U1 164.34(19) . . ?
N1 U2 U1 102.8(2) . . ?
O6 U2 U1 94.5(3) . 2_675 ?
O3 U2 U1 87.0(3) . 2_675 ?
O2 U2 U1 25.5(2) . 2_675 ?
O5 U2 U1 80.90(19) 2_765 2_675 ?
O4 U2 U1 95.49(18) . 2_675 ?
O5 U2 U1 139.69(19) . 2_675 ?
N1 U2 U1 158.1(2) . 2_675 ?
U1 U2 U1 55.639(14) . 2_675 ?
U2 O2 U1 130.2(4) . 2_675 ?
U2 O2 U1 120.9(4) . . ?
U1 O2 U1 108.4(3) 2_675 . ?
C1 O4 U2 126.4(8) . . ?
C1 O4 U1 131.5(8) . . ?
U2 O4 U1 101.8(3) . . ?
C2 O5 U2 113.6(8) . 2_765 ?
C2 O5 U2 125.3(8) . . ?
U2 O5 U2 121.1(3) 2_765 . ?
C2 O10 U1 168.5(9) 1_465 . ?
C6 N1 C5 117.0(10) . . ?
C6 N1 U2 120.6(8) . . ?
C5 N1 U2 122.3(7) . . ?
O1 C1 O4 127.6(12) . . ?
O1 C1 C6 117.3(11) . . ?
O4 C1 C6 115.1(11) . . ?
O10 C2 O5 121.3(12) 1_645 . ?
O10 C2 C5 121.1(11) 1_645 . ?
O5 C2 C5 117.7(11) . . ?
C4 C3 C6 118.1(12) . . ?
C4 C3 H3 121.0 . . ?
C6 C3 H3 121.0 . . ?
C3 C4 C7 120.4(12) . . ?
C3 C4 H4 119.8 . . ?
C7 C4 H4 119.8 . . ?
N1 C5 C7 124.3(11) . . ?
N1 C5 C2 112.9(10) . . ?
C7 C5 C2 122.7(11) . . ?
N1 C6 C3 123.7(11) . . ?
N1 C6 C1 114.6(11) . . ?
C3 C6 C1 121.7(11) . . ?
C4 C7 C5 116.4(12) . . ?
C4 C7 H7 121.8 . . ?
C5 C7 H7 121.8 . . ?
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 O9 1.760(9) . ?
U1 O7 1.766(9) . ?
U1 O2 2.284(9) 2_675 ?
U1 O2 2.286(9) . ?
U1 O10 2.434(9) . ?
U1 O8 2.507(9) . ?
U1 O4 2.545(8) . ?
U1 U1 3.7067(10) 2_675 ?
U1 U2 3.8862(7) . ?
U1 U2 4.0503(7) 2_675 ?
U2 O6 1.783(8) . ?
U2 O3 1.794(9) . ?
U2 O2 2.181(8) . ?
U2 O5 2.456(8) 2_765 ?
U2 O4 2.464(8) . ?
U2 O5 2.520(8) . ?
U2 N1 2.575(10) . ?
U2 U1 4.0503(7) 2_675 ?
O1 C1 1.225(15) . ?
O2 U1 2.284(9) 2_675 ?
O4 C1 1.286(14) . ?
O5 C2 1.260(14) . ?
O5 U2 2.456(8) 2_765 ?
O10 C2 1.260(14) 1_465 ?
N1 C6 1.336(15) . ?
N1 C5 1.351(14) . ?
C1 C6 1.529(17) . ?
C2 O10 1.260(14) 1_645 ?
C2 C5 1.494(18) . ?
C3 C4 1.380(16) . ?
C3 C6 1.399(17) . ?
C3 H3 0.9300 . ?
C4 C7 1.399(17) . ?
C4 H4 0.9300 . ?
C5 C7 1.404(17) . ?
C7 H7 0.9300 . ?
