#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/72/2217210.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2217210
loop_
_publ_author_name
'Pospieszna, Izabela'
'Radecka-Paryzek, Wanda'
'Kubicki, Maciej'
_publ_section_title
;
 Bis(pyridinium) trans-tetrachloridodioxidouranate(VI) dioxane
 solvate
;
_journal_coeditor_code           NC2081
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m239
_journal_page_last               m239
_journal_paper_doi               10.1107/S1600536807066949
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C5 H6 N)2 [U Cl4 O2], C4 H8 O2'
_chemical_formula_moiety         '2(C5 H6 N +), Cl4 O2 U 2-, C4 H8 O2'
_chemical_formula_sum            'C14 H20 Cl4 N2 O4 U'
_chemical_formula_weight         660.15
_chemical_name_systematic
;
bis(pyridinium) uranyl tetrachloridodioxidouranium(VI)
dioxane solvate]
;
_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                63.57(3)
_cell_angle_beta                 67.08(2)
_cell_angle_gamma                81.96(2)
_cell_formula_units_Z            1
_cell_length_a                   7.766(2)
_cell_length_b                   8.666(2)
_cell_length_c                   9.202(2)
_cell_measurement_reflns_used    2368
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     510.4(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics    'XP (Siemens, 1989)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Kuma KM-4-CCD four-circle'
_diffrn_measurement_method       ω
_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  0.097
_diffrn_reflns_av_sigmaI/netI    0.2510
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    8.495
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.800
_refine_diff_density_min         -2.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1770
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0556
_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)+(0.02P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                1142
_reflns_number_total             1770
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            nc2081.cif
_cod_data_source_block           I
_cod_database_code               2217210
_cod_database_fobs_code          2217210
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
U U1 1.0000 1.0000 0.0000 0.0190(3) Uani d S 1
O O1 0.8449(10) 0.8196(8) 0.0864(8) 0.0147(18) Uani d U 1
Cl Cl1 1.1731(4) 0.8012(3) 0.2188(3) 0.0233(9) Uani d . 1
Cl Cl2 0.7746(4) 1.1044(3) 0.2426(3) 0.0220(9) Uani d . 1
O O1A 0.3181(10) 0.5610(8) 0.5613(8) 0.013(2) Uani d . 1
C C2A 0.4823(16) 0.6717(13) 0.4704(13) 0.017(3) Uani d U 1
H H2A2 0.4632 0.7624 0.5122 0.022 Uiso calc R 1
H H2A1 0.5058 0.7287 0.3439 0.022 Uiso calc R 1
C C3A 0.6456(17) 0.5718(14) 0.4994(13) 0.018(3) Uani d U 1
H H3A2 0.7573 0.6508 0.4375 0.023 Uiso calc R 1
H H3A1 0.6230 0.5183 0.6256 0.023 Uiso calc R 1
N N1B 0.9618(13) 0.6611(10) 0.6810(10) 0.016(2) Uani d U 1
H H1B 1.0681 0.6435 0.6087 0.019 Uiso calc R 1
C C2B 0.9005(17) 0.5495(14) 0.8497(13) 0.022(3) Uani d U 1
H H2B 0.9733 0.4548 0.8923 0.027 Uiso calc R 1
C C3B 0.7294(17) 0.5742(14) 0.9614(13) 0.020(3) Uani d U 1
H H3B 0.6810 0.4911 1.0796 0.024 Uiso calc R 1
C C4B 0.6257(18) 0.7202(14) 0.9030(13) 0.023(3) Uani d U 1
H H4B 0.5107 0.7412 0.9792 0.028 Uiso calc R 1
C C5B 0.7038(17) 0.8332(14) 0.7241(12) 0.018(3) Uani d U 1
H H5B 0.6409 0.9347 0.6777 0.022 Uiso calc R 1
C C6B 0.8639(17) 0.8001(14) 0.6192(14) 0.021(3) Uani d U 1
H H6B 0.9103 0.8759 0.4983 0.026 Uiso calc R 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
U1 0.0264(6) 0.0098(4) 0.0142(4) 0.0037(4) -0.0084(3) 0.0003(3)
O1 0.015(2) 0.015(2) 0.015(2) 0.0000(10) -0.0054(11) -0.0072(11)
Cl1 0.031(2) 0.0219(17) 0.0137(15) 0.0129(17) -0.0104(16) -0.0067(13)
Cl2 0.026(2) 0.0193(17) 0.0173(15) 0.0095(16) -0.0073(15) -0.0077(13)
O1A 0.005(5) 0.014(4) 0.020(4) 0.001(4) -0.004(4) -0.008(3)
C2A 0.017(3) 0.017(3) 0.017(3) 0.0005(10) -0.0060(14) -0.0072(15)
C3A 0.018(3) 0.018(3) 0.018(3) 0.0004(10) -0.0066(14) -0.0075(15)
N1B 0.016(2) 0.016(2) 0.016(2) 0.0006(10) -0.0053(13) -0.0073(13)
C2B 0.022(3) 0.022(3) 0.022(3) 0.0011(10) -0.0083(15) -0.0093(15)
C3B 0.020(3) 0.020(3) 0.020(3) 0.0009(10) -0.0076(14) -0.0082(15)
C4B 0.023(3) 0.023(3) 0.023(3) 0.0006(10) -0.0086(15) -0.0100(16)
C5B 0.018(3) 0.018(3) 0.018(3) 0.0008(10) -0.0067(14) -0.0078(15)
C6B 0.021(3) 0.021(3) 0.021(3) 0.0007(10) -0.0081(14) -0.0088(15)
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O1 . 2_775 180.0000(10) ?
O1 U1 Cl2 . 2_775 88.5(2) ?
O1 U1 Cl2 2_775 2_775 91.5(2) ?
O1 U1 Cl2 . . 91.5(2) y
O1 U1 Cl2 2_775 . 88.5(2) y
Cl2 U1 Cl2 2_775 . 180.0000(10) y
O1 U1 Cl1 . . 88.4(2) y
O1 U1 Cl1 2_775 . 91.6(2) y
Cl2 U1 Cl1 2_775 . 90.57(8) ?
Cl2 U1 Cl1 . . 89.43(8) y
O1 U1 Cl1 . 2_775 91.6(2) ?
O1 U1 Cl1 2_775 2_775 88.4(2) ?
Cl2 U1 Cl1 2_775 2_775 89.43(8) ?
Cl2 U1 Cl1 . 2_775 90.57(8) y
Cl1 U1 Cl1 . 2_775 180.0000(10) y
C2A O1A C3A . 2_666 107.7(8) ?
O1A C2A C3A . . 110.4(8) ?
O1A C2A H2A2 . . 109.6 ?
C3A C2A H2A2 . . 109.6 ?
O1A C2A H2A1 . . 109.6 ?
C3A C2A H2A1 . . 109.6 ?
H2A2 C2A H2A1 . . 108.1 ?
O1A C3A C2A 2_666 . 112.1(10) ?
O1A C3A H3A2 2_666 . 109.2 ?
C2A C3A H3A2 . . 109.2 ?
O1A C3A H3A1 2_666 . 109.2 ?
C2A C3A H3A1 . . 109.2 ?
H3A2 C3A H3A1 . . 107.9 ?
C2B N1B C6B . . 121.4(10) ?
C2B N1B H1B . . 119.3 ?
C6B N1B H1B . . 119.3 ?
N1B C2B C3B . . 119.0(10) ?
N1B C2B H2B . . 120.5 ?
C3B C2B H2B . . 120.5 ?
C2B C3B C4B . . 121.2(10) ?
C2B C3B H3B . . 119.4 ?
C4B C3B H3B . . 119.4 ?
C3B C4B C5B . . 115.7(11) ?
C3B C4B H4B . . 122.2 ?
C5B C4B H4B . . 122.2 ?
C6B C5B C4B . . 121.2(10) ?
C6B C5B H5B . . 119.4 ?
C4B C5B H5B . . 119.4 ?
C5B C6B N1B . . 121.4(10) ?
C5B C6B H6B . . 119.3 ?
N1B C6B H6B . . 119.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.789(7) y
U1 O1 2_775 1.789(7) ?
U1 Cl2 2_775 2.679(3) ?
U1 Cl2 . 2.679(3) y
U1 Cl1 . 2.684(3) y
U1 Cl1 2_775 2.684(3) ?
O1A C2A . 1.430(13) ?
O1A C3A 2_666 1.440(12) ?
C2A C3A . 1.477(13) ?
C2A H2A2 . 0.9900 ?
C2A H2A1 . 0.9900 ?
C3A O1A 2_666 1.440(12) ?
C3A H3A2 . 0.9900 ?
C3A H3A1 . 0.9900 ?
N1B C2B . 1.337(11) ?
N1B C6B . 1.350(12) ?
N1B H1B . 0.8800 ?
C2B C3B . 1.386(15) ?
C2B H2B . 0.9500 ?
C3B C4B . 1.409(13) ?
C3B H3B . 0.9500 ?
C4B C5B . 1.411(12) ?
C4B H4B . 0.9500 ?
C5B C6B . 1.331(14) ?
C5B H5B . 0.9500 ?
C6B H6B . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C6B H6B Cl1 . 0.95 2.87 3.525(12) 127.3
C2A H2A2 Cl2 2_676 0.99 2.88 3.754(12) 147.3
N1B H1B O1A 1_655 0.88 1.92 2.725(11) 150.7
C4B H4B Cl1 1_456 0.95 2.85 3.803(13) 177.4
