#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:52:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179544 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/13/4501383.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_4501383
loop_
_publ_author_name
'Kerr, Andrew T.'
'Cahill, Christopher L.'
_publ_section_title
;
 Crystal Engineering with the Uranyl Cation III. Mixed Aliphatic
 Dicarboxylate/Aromatic Dipyridyl Coordination Polymers: Synthesis,
 Structures, and Speciation
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5634
_journal_paper_doi               10.1021/cg2011869
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C15 H19 N O6 U'
_chemical_formula_weight         547.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                108.60
_cell_angle_beta                 96.0540(10)
_cell_angle_gamma                100.7710(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1535(3)
_cell_length_b                   9.4052(3)
_cell_length_c                   12.3338(4)
_cell_measurement_reflns_used    17084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.603
_cell_measurement_theta_min      4.680
_cell_volume                     866.68(5)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Gualardi, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Siemens SMART, Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17076
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens SMART'
_exptl_absorpt_coefficient_mu    9.392
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5243
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             512
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.60
_refine_diff_density_max         2.304
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0116P)²+1.1806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0414
_reflns_number_gt                4483
_reflns_number_total             4783
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            cg2011869_si_001.cif
_cod_data_source_block           Compound5
_cod_original_cell_volume        866.67(5)
_cod_database_code               4501383
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
C1 C 0.0705(4) 1.1046(3) 0.7887(3) 0.0350(6) Uani 1 1 d .
C2 C -0.0800(4) 1.1524(4) 0.8383(3) 0.0426(7) Uani 1 1 d .
H2A H -0.0713 1.1483 0.9162 0.051 Uiso 1 1 calc R
H2B H -0.1820 1.0772 0.7918 0.051 Uiso 1 1 calc R
C3 C -0.1009(4) 1.3127(4) 0.8442(3) 0.0402(7) Uani 1 1 d .
H3A H -0.1866 1.3389 0.8910 0.048 Uiso 1 1 calc R
H3B H 0.0052 1.3868 0.8838 0.048 Uiso 1 1 calc R
C4 C -0.1506(4) 1.3301(3) 0.7274(3) 0.0385(6) Uani 1 1 d .
H4A H -0.0589 1.3174 0.6838 0.046 Uiso 1 1 calc R
H4B H -0.2498 1.2492 0.6834 0.046 Uiso 1 1 calc R
C5 C -0.1894(5) 1.4863(4) 0.7404(3) 0.0469(8) Uani 1 1 d .
H5A H -0.2911 1.4926 0.7743 0.056 Uiso 1 1 calc R
H5B H -0.0968 1.5667 0.7940 0.056 Uiso 1 1 calc R
C6 C 0.6202(4) 0.8259(3) 0.5270(2) 0.0322(6) Uani 1 1 d .
C7 C 0.7114(4) 0.7008(4) 0.5271(3) 0.0390(7) Uani 1 1 d .
H7A H 0.8242 0.7304 0.5110 0.047 Uiso 1 1 calc R
H7B H 0.6518 0.6071 0.4641 0.047 Uiso 1 1 calc R
C8 C 0.7283(5) 0.6653(4) 0.6389(3) 0.0434(7) Uani 1 1 d .
H8A H 0.6197 0.6580 0.6647 0.052 Uiso 1 1 calc R
H8B H 0.8096 0.7502 0.6983 0.052 Uiso 1 1 calc R
C9 C 0.7849(4) 0.5167(4) 0.6265(3) 0.0399(7) Uani 1 1 d .
H9A H 0.8905 0.5217 0.5967 0.048 Uiso 1 1 calc R
H9B H 0.7005 0.4309 0.5702 0.048 Uiso 1 1 calc R
C10 C 0.2792(4) 0.6633(4) 0.7469(3) 0.0471(8) Uani 1 1 d .
H10 H 0.1924 0.6329 0.6832 0.057 Uiso 1 1 calc R
C11 C 0.4986(5) 0.8480(3) 0.8743(3) 0.0413(7) Uani 1 1 d .
H11 H 0.5678 0.9471 0.8998 0.050 Uiso 1 1 calc R
C12 C 0.3047(5) 0.5564(4) 0.7982(3) 0.0497(8) Uani 1 1 d .
H12 H 0.2380 0.4561 0.7679 0.060 Uiso 1 1 calc R
C13 C 0.5309(5) 0.7487(4) 0.9316(3) 0.0436(7) Uani 1 1 d .
H13 H 0.6197 0.7814 0.9944 0.052 Uiso 1 1 calc R
C14 C 0.4298(4) 0.5995(3) 0.8946(3) 0.0385(7) Uani 1 1 d .
C15 C 0.4513(5) 0.4851(4) 0.9504(3) 0.0431(7) Uani 1 1 d .
H15 H 0.3905 0.3837 0.9117 0.052 Uiso 1 1 calc R
N1 N 0.3725(3) 0.8080(3) 0.7840(2) 0.0340(5) Uani 1 1 d .
O1 O 0.4864(3) 1.1334(3) 0.7900(2) 0.0462(5) Uani 1 1 d .
O2 O 0.1738(4) 0.8461(3) 0.5719(2) 0.0600(7) Uani 1 1 d .
O3 O 0.1390(3) 1.1649(3) 0.7215(2) 0.0458(5) Uani 1 1 d .
O4 O 0.1293(3) 1.0017(3) 0.8133(2) 0.0443(5) Uani 1 1 d .
O5 O 0.5448(4) 0.8769(3) 0.6061(2) 0.0579(7) Uani 1 1 d .
O6 O 0.3815(4) 1.1308(4) 0.5581(3) 0.0733(9) Uani 1 1 d .
U1 U 0.328880(14) 0.993421(12) 0.677918(9) 0.03276(4) Uani 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
O4 C1 O3 118.9(3) . .
O4 C1 C2 119.8(2) . .
O3 C1 C2 121.3(2) . .
O4 C1 U1 60.20(15) . .
O3 C1 U1 58.91(14) . .
C2 C1 U1 174.5(2) . .
C1 C2 C3 115.9(3) . .
C1 C2 H2A 108.3 . .
C3 C2 H2A 108.3 . .
C1 C2 H2B 108.3 . .
C3 C2 H2B 108.3 . .
H2A C2 H2B 107.4 . .
C4 C3 C2 115.4(3) . .
C4 C3 H3A 108.4 . .
C2 C3 H3A 108.4 . .
C4 C3 H3B 108.4 . .
C2 C3 H3B 108.4 . .
H3A C3 H3B 107.5 . .
C5 C4 C3 112.4(3) . .
C5 C4 H4A 109.1 . .
C3 C4 H4A 109.1 . .
C5 C4 H4B 109.1 . .
C3 C4 H4B 109.1 . .
H4A C4 H4B 107.9 . .
C9 C5 C4 113.8(3) 1_465 .
C9 C5 H5A 108.8 1_465 .
C4 C5 H5A 108.8 . .
C9 C5 H5B 108.8 1_465 .
C4 C5 H5B 108.8 . .
H5A C5 H5B 107.7 . .
O5 C6 O6 122.0(3) . 2_676
O5 C6 C7 120.5(2) . .
O6 C6 C7 117.5(3) 2_676 .
C6 C7 C8 115.5(2) . .
C6 C7 H7A 108.4 . .
C8 C7 H7A 108.4 . .
C6 C7 H7B 108.4 . .
C8 C7 H7B 108.4 . .
H7A C7 H7B 107.5 . .
C7 C8 C9 113.5(3) . .
C7 C8 H8A 108.9 . .
C9 C8 H8A 108.9 . .
C7 C8 H8B 108.9 . .
C9 C8 H8B 108.9 . .
H8A C8 H8B 107.7 . .
C8 C9 C5 113.1(3) . 1_645
C8 C9 H9A 109.0 . .
C5 C9 H9A 109.0 1_645 .
C8 C9 H9B 109.0 . .
C5 C9 H9B 109.0 1_645 .
H9A C9 H9B 107.8 . .
N1 C10 C12 123.5(3) . .
N1 C10 H10 118.2 . .
C12 C10 H10 118.2 . .
N1 C11 C13 123.0(3) . .
N1 C11 H11 118.5 . .
C13 C11 H11 118.5 . .
C14 C12 C10 119.4(3) . .
C14 C12 H12 120.3 . .
C10 C12 H12 120.3 . .
C11 C13 C14 119.5(3) . .
C11 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
C12 C14 C13 117.3(3) . .
C12 C14 C15 118.6(3) . .
C13 C14 C15 124.1(3) . .
C15 C15 C14 125.1(4) 2_667 .
C15 C15 H15 117.4 2_667 .
C14 C15 H15 117.4 . .
C10 N1 C11 117.1(2) . .
C10 N1 U1 121.6(2) . .
C11 N1 U1 121.11(19) . .
C1 O3 U1 94.48(16) . .
C1 O4 U1 93.22(17) . .
C6 O5 U1 151.2(2) . .
C6 O6 U1 163.8(3) 2_676 .
O2 U1 O1 176.16(11) . .
O2 U1 O6 93.38(13) . .
O1 U1 O6 90.26(12) . .
O2 U1 O5 91.06(12) . .
O1 U1 O5 88.03(11) . .
O6 U1 O5 84.91(8) . .
O2 U1 O3 93.13(11) . .
O1 U1 O3 88.84(10) . .
O6 U1 O3 78.02(8) . .
O5 U1 O3 162.63(7) . .
O2 U1 O4 88.25(11) . .
O1 U1 O4 90.30(10) . .
O6 U1 O4 131.10(8) . .
O5 U1 O4 143.97(7) . .
O3 U1 O4 53.10(6) . .
O2 U1 N1 89.88(10) . .
O1 U1 N1 86.28(9) . .
O6 U1 N1 157.40(9) . .
O5 U1 N1 72.67(7) . .
O3 U1 N1 124.15(7) . .
O4 U1 N1 71.31(7) . .
O2 U1 C1 89.28(11) . .
O1 U1 C1 91.00(10) . .
O6 U1 C1 104.53(8) . .
O5 U1 C1 170.52(8) . .
O3 U1 C1 26.61(7) . .
O4 U1 C1 26.57(7) . .
N1 U1 C1 97.86(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O4 1.261(3) .
C1 O3 1.264(3) .
C1 C2 1.507(4) .
C1 U1 2.814(3) .
C2 C3 1.529(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.523(4) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.523(4) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C9 1.522(4) 1_465
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 O5 1.224(3) .
C6 O6 1.241(3) 2_676
C6 C7 1.505(4) .
C7 C8 1.517(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.520(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C5 1.522(4) 1_645
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 N1 1.335(4) .
C10 C12 1.382(4) .
C10 H10 0.9300 .
C11 N1 1.336(4) .
C11 C13 1.384(4) .
C11 H11 0.9300 .
C12 C14 1.379(5) .
C12 H12 0.9300 .
C13 C14 1.391(5) .
C13 H13 0.9300 .
C14 C15 1.477(4) .
C15 C15 1.304(6) 2_667
C15 H15 0.9300 .
N1 U1 2.544(2) .
O1 U1 1.768(2) .
O2 U1 1.752(3) .
O3 U1 2.417(2) .
O4 U1 2.446(2) .
O5 U1 2.348(2) .
O6 C6 1.241(3) 2_676
O6 U1 2.277(2) .
