#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:08:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179441 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/38/4333890.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_4333890
loop_
_publ_author_name
'Sonia G. Thangavelu'
'Michael B. Andrews'
'Simon J.A. Pope'
'Christopher L. Cahill'
_publ_contact_author_address
;The George Washington University
Department of Chemistry
725 21st Street, NW
Washington, DC, 20052
;
_publ_contact_author_email       cahill@gwu.edu
_publ_contact_author_fax         202-994-5873
_publ_contact_author_name        'Christopher L. Cahill'
_publ_contact_author_phone       202-994-6959
_publ_section_title
;
 Synthesis, Structures, and Luminescent Properties of Uranyl Terpyridine
 Aromatic Carboxylate Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2060
_journal_page_last               2069
_journal_paper_doi               10.1021/ic3024698
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H13 N3 O6 S U'
_chemical_formula_sum            'C21 H13 N3 O6 S U'
_chemical_formula_weight         673.438
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.0320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5824(3)
_cell_length_b                   13.5216(5)
_cell_length_c                   16.2164(5)
_cell_measurement_reflns_used    5938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      1.98
_cell_volume                     2054.99(12)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40347
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX CCD'
_exptl_absorpt_coefficient_mu    8.046
_exptl_absorpt_correction_T_max  0.2730
_exptl_absorpt_correction_T_min  0.2422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.170
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.689
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0359
_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)+(0.0464P)²+3.1924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                5251
_reflns_number_total             5938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3024698_si_002_2.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
U1 U 0.674982(14) 0.141521(9) 0.071158(8) 0.02058(6) Uani 1 1 d .
O1 O 0.8465(3) 0.1658(2) 0.13509(19) 0.0272(6) Uani 1 1 d .
O2 O 0.5048(3) 0.1142(2) 0.00975(19) 0.0281(6) Uani 1 1 d .
O3 O 0.6861(3) 0.2785(2) -0.00905(18) 0.0303(6) Uani 1 1 d .
O4 O 0.8859(4) 0.3594(2) -0.0205(2) 0.0318(7) Uani 1 1 d .
O5 O 0.5751(3) 0.2556(2) 0.14547(18) 0.0247(5) Uani 1 1 d .
O6 O 0.3389(3) 0.2426(2) 0.13756(19) 0.0296(6) Uani 1 1 d .
S1 S 0.73451(10) 0.55434(7) -0.06897(6) 0.02406(19) Uani 1 1 d .
N1 N 0.6164(4) 0.0332(2) 0.1911(2) 0.0236(6) Uani 1 1 d .
N2 N 0.7568(3) -0.0410(2) 0.0760(2) 0.0222(6) Uani 1 1 d .
N3 N 0.7687(4) 0.0770(2) -0.0567(2) 0.0250(6) Uani 1 1 d .
C12 C 0.8687(4) -0.0523(3) -0.1282(3) 0.0274(8) Uani 1 1 d .
H12 H 0.9055 -0.1176 -0.1278 0.033 Uiso 1 1 calc R
C11 C 0.8216(4) -0.0158(3) -0.0580(2) 0.0231(7) Uani 1 1 d .
C2 C 0.5054(5) 0.0157(3) 0.3110(3) 0.0293(8) Uani 1 1 d .
H2 H 0.4558 0.0453 0.3496 0.035 Uiso 1 1 calc R
C4 C 0.6203(5) -0.1219(3) 0.2626(3) 0.0274(8) Uani 1 1 d .
H4 H 0.6467 -0.1897 0.2662 0.033 Uiso 1 1 calc R
C14 C 0.8039(5) 0.1015(3) -0.1979(3) 0.0305(8) Uani 1 1 d .
H14 H 0.7957 0.1435 -0.2456 0.037 Uiso 1 1 calc R
C5 C 0.6578(4) -0.0621(3) 0.2005(2) 0.0234(7) Uani 1 1 d .
C13 C 0.8611(5) 0.0076(3) -0.1984(3) 0.0290(8) Uani 1 1 d .
H13 H 0.8946 -0.0155 -0.2461 0.035 Uiso 1 1 calc R
C15 C 0.7590(6) 0.1327(3) -0.1269(3) 0.0324(10) Uani 1 1 d .
H15 H 0.7189 0.1970 -0.1273 0.039 Uiso 1 1 calc R
C8 C 0.8776(5) -0.2297(3) 0.0928(3) 0.0307(9) Uani 1 1 d .
H8 H 0.9219 -0.2929 0.0997 0.037 Uiso 1 1 calc R
C1 C 0.5398(5) 0.0701(3) 0.2458(3) 0.0277(8) Uani 1 1 d .
H1 H 0.5082 0.1367 0.2389 0.033 Uiso 1 1 calc R
C9 C 0.8864(5) -0.1716(3) 0.0244(3) 0.0281(8) Uani 1 1 d .
H9 H 0.9344 -0.1950 -0.0174 0.034 Uiso 1 1 calc R
C6 C 0.7429(4) -0.1005(3) 0.1412(2) 0.0244(7) Uani 1 1 d .
C10 C 0.8244(4) -0.0781(3) 0.0172(2) 0.0228(7) Uani 1 1 d .
C3 C 0.5453(4) -0.0830(3) 0.3187(3) 0.0273(8) Uani 1 1 d .
H3 H 0.5212 -0.1230 0.3618 0.033 Uiso 1 1 calc R
C7 C 0.8034(5) -0.1949(3) 0.1515(3) 0.0311(9) Uani 1 1 d .
H7 H 0.7936 -0.2347 0.1982 0.037 Uiso 1 1 calc R
C20 C 0.5685(4) 0.6034(3) -0.1085(2) 0.0246(7) Uani 1 1 d .
C16 C 0.7564(5) 0.3538(3) -0.0272(3) 0.0266(8) Uani 1 1 d .
C17 C 0.6620(4) 0.4387(3) -0.0619(2) 0.0248(7) Uani 1 1 d .
C18 C 0.5174(5) 0.4388(3) -0.0891(2) 0.0257(8) Uani 1 1 d .
H18 H 0.4595 0.3815 -0.0901 0.031 Uiso 1 1 calc R
C19 C 0.4632(4) 0.5330(3) -0.1155(2) 0.0254(8) Uani 1 1 d .
H19 H 0.3647 0.5464 -0.1359 0.030 Uiso 1 1 calc R
C21 C 0.4447(4) 0.2902(3) 0.1313(2) 0.0252(8) 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'
S S 0.1246 0.1234 '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
O2 U1 O1 178.23(13) . .
O2 U1 O3 89.77(13) . .
O1 U1 O3 92.01(13) . .
O2 U1 O5 89.99(12) . .
O1 U1 O5 90.31(12) . .
O3 U1 O5 80.04(10) . .
O2 U1 N3 84.90(13) . .
O1 U1 N3 95.54(12) . .
O3 U1 N3 75.55(10) . .
O5 U1 N3 155.06(10) . .
O2 U1 N2 93.21(12) . .
O1 U1 N2 85.47(12) . .
O3 U1 N2 138.01(11) . .
O5 U1 N2 141.75(10) . .
N3 U1 N2 63.06(10) . .
O2 U1 N1 89.18(12) . .
O1 U1 N1 89.17(12) . .
O3 U1 N1 158.80(10) . .
O5 U1 N1 78.79(10) . .
N3 U1 N1 125.40(10) . .
N2 U1 N1 63.18(10) . .
C16 O3 U1 149.5(3) . .
C21 O5 U1 129.6(2) . .
C20 S1 C17 91.1(2) . .
C5 N1 C1 117.6(3) . .
C5 N1 U1 121.4(3) . .
C1 N1 U1 120.9(3) . .
C10 N2 C6 117.9(3) . .
C10 N2 U1 121.2(2) . .
C6 N2 U1 120.7(3) . .
C15 N3 C11 117.5(4) . .
C15 N3 U1 120.9(3) . .
C11 N3 U1 121.4(3) . .
C13 C12 C11 119.4(4) . .
C13 C12 H12 120.3 . .
C11 C12 H12 120.3 . .
N3 C11 C12 121.7(4) . .
N3 C11 C10 117.2(3) . .
C12 C11 C10 121.1(4) . .
C1 C2 C3 118.3(4) . .
C1 C2 H2 120.8 . .
C3 C2 H2 120.8 . .
C3 C4 C5 120.3(4) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
C15 C14 C13 118.7(4) . .
C15 C14 H14 120.7 . .
C13 C14 H14 120.7 . .
N1 C5 C4 121.4(4) . .
N1 C5 C6 116.8(3) . .
C4 C5 C6 121.7(4) . .
C14 C13 C12 119.0(4) . .
C14 C13 H13 120.5 . .
C12 C13 H13 120.5 . .
N3 C15 C14 123.7(4) . .
N3 C15 H15 118.2 . .
C14 C15 H15 118.2 . .
C9 C8 C7 119.1(4) . .
C9 C8 H8 120.5 . .
C7 C8 H8 120.5 . .
N1 C1 C2 123.5(4) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C8 C9 C10 119.3(4) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N2 C6 C7 121.9(4) . .
N2 C6 C5 117.1(3) . .
C7 C6 C5 121.0(4) . .
N2 C10 C9 122.4(4) . .
N2 C10 C11 116.1(3) . .
C9 C10 C11 121.4(4) . .
C4 C3 C2 118.8(4) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
C8 C7 C6 119.3(4) . .
C8 C7 H7 120.4 . .
C6 C7 H7 120.4 . .
C19 C20 C21 128.8(4) . 3_665
C19 C20 S1 111.7(3) . .
C21 C20 S1 119.4(3) 3_665 .
O4 C16 O3 126.6(4) . .
O4 C16 C17 120.5(4) . .
O3 C16 C17 112.8(4) . .
C18 C17 C16 128.0(4) . .
C18 C17 S1 112.0(3) . .
C16 C17 S1 120.0(3) . .
C17 C18 C19 112.6(4) . .
C17 C18 H18 123.7 . .
C19 C18 H18 123.7 . .
C20 C19 C18 112.5(4) . .
C20 C19 H19 123.7 . .
C18 C19 H19 123.7 . .
O6 C21 O5 125.2(4) . .
O6 C21 C20 120.1(4) . 3_665
O5 C21 C20 114.8(3) . 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.764(3) .
U1 O1 1.781(3) .
U1 O3 2.278(3) .
U1 O5 2.286(3) .
U1 N3 2.577(3) .
U1 N2 2.586(3) .
U1 N1 2.588(3) .
O3 C16 1.289(5) .
O4 C16 1.225(6) .
O5 C21 1.309(5) .
O6 C21 1.223(5) .
S1 C20 1.719(4) .
S1 C17 1.724(4) .
N1 C5 1.347(5) .
N1 C1 1.358(5) .
N2 C10 1.356(5) .
N2 C6 1.357(5) .
N3 C15 1.353(6) .
N3 C11 1.354(5) .
C12 C13 1.386(6) .
C12 C11 1.399(5) .
C12 H12 0.9500 .
C11 C10 1.479(5) .
C2 C1 1.383(6) .
C2 C3 1.387(6) .
C2 H2 0.9500 .
C4 C3 1.375(6) .
C4 C5 1.396(6) .
C4 H4 0.9500 .
C14 C15 1.377(6) .
C14 C13 1.384(6) .
C14 H14 0.9500 .
C5 C6 1.479(6) .
C13 H13 0.9500 .
C15 H15 0.9500 .
C8 C9 1.376(6) .
C8 C7 1.384(6) .
C8 H8 0.9500 .
C1 H1 0.9500 .
C9 C10 1.391(5) .
C9 H9 0.9500 .
C6 C7 1.398(6) .
C3 H3 0.9500 .
C7 H7 0.9500 .
C20 C19 1.375(6) .
C20 C21 1.485(5) 3_665
C16 C17 1.497(5) .
C17 C18 1.364(6) .
C18 C19 1.408(5) .
C18 H18 0.9500 .
C19 H19 0.9500 .
C21 C20 1.485(5) 3_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 U1 O3 C16 -176.2(5) . .
O1 U1 O3 C16 3.8(5) . .
O5 U1 O3 C16 93.8(5) . .
N3 U1 O3 C16 -91.4(5) . .
N2 U1 O3 C16 -81.7(6) . .
N1 U1 O3 C16 96.7(6) . .
O2 U1 O5 C21 -9.1(3) . .
O1 U1 O5 C21 172.6(3) . .
O3 U1 O5 C21 80.7(3) . .
N3 U1 O5 C21 68.7(4) . .
N2 U1 O5 C21 -104.3(3) . .
N1 U1 O5 C21 -98.3(3) . .
O2 U1 N1 C5 95.8(3) . .
O1 U1 N1 C5 -83.5(3) . .
O3 U1 N1 C5 -176.9(3) . .
O5 U1 N1 C5 -174.0(3) . .
N3 U1 N1 C5 12.7(3) . .
N2 U1 N1 C5 1.8(3) . .
O2 U1 N1 C1 -82.7(3) . .
O1 U1 N1 C1 97.9(3) . .
O3 U1 N1 C1 4.5(5) . .
O5 U1 N1 C1 7.4(3) . .
N3 U1 N1 C1 -165.9(3) . .
N2 U1 N1 C1 -176.7(3) . .
O2 U1 N2 C10 91.1(3) . .
O1 U1 N2 C10 -90.0(3) . .
O3 U1 N2 C10 -2.1(4) . .
O5 U1 N2 C10 -174.8(2) . .
N3 U1 N2 C10 8.5(3) . .
N1 U1 N2 C10 178.6(3) . .
O2 U1 N2 C6 -93.9(3) . .
O1 U1 N2 C6 85.0(3) . .
O3 U1 N2 C6 172.9(3) . .
O5 U1 N2 C6 0.2(4) . .
N3 U1 N2 C6 -176.5(3) . .
N1 U1 N2 C6 -6.4(3) . .
O2 U1 N3 C15 76.0(3) . .
O1 U1 N3 C15 -105.7(3) . .
O3 U1 N3 C15 -15.0(3) . .
O5 U1 N3 C15 -2.9(5) . .
N2 U1 N3 C15 172.3(4) . .
N1 U1 N3 C15 161.4(3) . .
O2 U1 N3 C11 -100.1(3) . .
O1 U1 N3 C11 78.2(3) . .
O3 U1 N3 C11 168.9(3) . .
O5 U1 N3 C11 -179.0(3) . .
N2 U1 N3 C11 -3.8(3) . .
N1 U1 N3 C11 -14.7(3) . .
C15 N3 C11 C12 1.8(6) . .
U1 N3 C11 C12 178.0(3) . .
C15 N3 C11 C10 -176.7(4) . .
U1 N3 C11 C10 -0.4(5) . .
C13 C12 C11 N3 0.0(6) . .
C13 C12 C11 C10 178.4(4) . .
C1 N1 C5 C4 1.8(6) . .
U1 N1 C5 C4 -176.9(3) . .
C1 N1 C5 C6 -179.1(3) . .
U1 N1 C5 C6 2.3(4) . .
C3 C4 C5 N1 -3.1(6) . .
C3 C4 C5 C6 177.7(4) . .
C15 C14 C13 C12 1.2(7) . .
C11 C12 C13 C14 -1.5(6) . .
C11 N3 C15 C14 -2.1(7) . .
U1 N3 C15 C14 -178.4(4) . .
C13 C14 C15 N3 0.6(7) . .
C5 N1 C1 C2 1.4(6) . .
U1 N1 C1 C2 -180.0(3) . .
C3 C2 C1 N1 -3.2(6) . .
C7 C8 C9 C10 2.0(6) . .
C10 N2 C6 C7 4.0(6) . .
U1 N2 C6 C7 -171.2(3) . .
C10 N2 C6 C5 -174.6(3) . .
U1 N2 C6 C5 10.2(4) . .
N1 C5 C6 N2 -8.1(5) . .
C4 C5 C6 N2 171.0(4) . .
N1 C5 C6 C7 173.2(4) . .
C4 C5 C6 C7 -7.6(6) . .
C6 N2 C10 C9 -4.0(6) . .
U1 N2 C10 C9 171.2(3) . .
C6 N2 C10 C11 172.7(3) . .
U1 N2 C10 C11 -12.2(4) . .
C8 C9 C10 N2 1.0(6) . .
C8 C9 C10 C11 -175.5(4) . .
N3 C11 C10 N2 8.2(5) . .
C12 C11 C10 N2 -170.3(4) . .
N3 C11 C10 C9 -175.1(4) . .
C12 C11 C10 C9 6.4(6) . .
C5 C4 C3 C2 1.3(6) . .
C1 C2 C3 C4 1.7(6) . .
C9 C8 C7 C6 -1.9(7) . .
N2 C6 C7 C8 -1.1(6) . .
C5 C6 C7 C8 177.5(4) . .
C17 S1 C20 C19 0.0(3) . .
C17 S1 C20 C21 -179.0(3) . 3_665
U1 O3 C16 O4 31.3(8) . .
U1 O3 C16 C17 -150.5(4) . .
O4 C16 C17 C18 165.8(4) . .
O3 C16 C17 C18 -12.6(6) . .
O4 C16 C17 S1 -15.5(6) . .
O3 C16 C17 S1 166.1(3) . .
C20 S1 C17 C18 0.3(3) . .
C20 S1 C17 C16 -178.6(3) . .
C16 C17 C18 C19 178.3(4) . .
S1 C17 C18 C19 -0.5(4) . .
C21 C20 C19 C18 178.6(4) 3_665 .
S1 C20 C19 C18 -0.2(4) . .
C17 C18 C19 C20 0.5(5) . .
U1 O5 C21 O6 68.3(5) . .
U1 O5 C21 C20 -113.5(3) . 3_665
