Hydrogen-bonded network structures in dipyridinium, bis(2-methylpyridinium), bis(3-methylpyridinium) and bis(4-methylpyridinium) dioxidobis(oxydiacetato)uranate(VI)
Lennartson, Anders; Håkansson, Mikael; Acta Crystallographica Section C 66 (2010) m69–m74; doi:10.1107/S0108270109053839

data_2017564
_publ_section_title
;
 Hydrogen-bonded network structures in dipyridinium,
 bis(2-methylpyridinium), bis(3-methylpyridinium) and
 bis(4-methylpyridinium) dioxidobis(oxydiacetato)uranate(VI)
;
_journal_coeditor_code           GG3221
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m69
_journal_page_last               m74
_journal_paper_doi               10.1107/S0108270109053839
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C6 H8 N)2 [U (C4 H4 O5)2 O2]'
_chemical_formula_moiety         '2C6 H8 N + , C8 H8 O12 U 2-'
_chemical_formula_sum            'C20 H24 N2 O12 U'
_chemical_formula_weight         722.44
_chemical_name_systematic
;
bis(3-methylpyridinium) dioxidobis(oxydiacetato)uranate(VI)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.224(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.415(2)
_cell_length_b                   13.312(5)
_cell_length_c                   11.806(4)
_cell_measurement_reflns_used    7099
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.15
_cell_volume                     1165.1(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2000)'
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalClear (Rigaku, 2000)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 2009)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 105
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7099
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.034
_exptl_absorpt_correction_T_max  0.500
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.195
_refine_diff_density_min         -3.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         1885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0872P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                1544
_reflns_number_total             1885
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3221.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017564
_cod_database_fobs_code          2017564