Experimental evidence of 3-centre, 2-electron covalent bond character of the central O-H-O fragment on the Zundel cation in crystals of Zundel nitranilate tetrahydrate
Molcanov, Kresimir; Jelsch, Christian; Wenger, Emmanuel; Stare, Jernej; Madsen, Anders Østergaard; Kojic-Prodic, Biserka; CrystEngComm  (2017) –; doi:10.1039/C7CE00501F

data_7228489
_publ_section_title
;
 Experimental evidence of 3-centre, 2-electron covalent bond character of
 the central O-H-O fragment on the Zundel cation in crystals of Zundel
 nitranilate tetrahydrate
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00501F
_journal_year                    2017
_chemical_absolute_configuration -
_chemical_formula_moiety         'C3 H7 N O7'
_chemical_formula_sum            'C3 H7 N O7'
_chemical_formula_weight         169.085
_chemical_name_common            'nitranilic acid'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'MoPro v15.10   rev. 1113 '
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.
_cell_angle_beta                 93.645(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   3.5787(3)
_cell_length_b                   19.23520(10)
_cell_length_c                   9.1906(8)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.13
_cell_measurement_theta_min      4.92
_cell_volume                     631.37(8)
_computing_structure_refinement  'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'microfocus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.02927
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            66115
_diffrn_reflns_theta_full        39.76
_diffrn_reflns_theta_max         39.76
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_correction_T_min  0.9750
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: conc. nitric acid'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         3810
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0301
_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/[2.5*\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0274
_refine_ls_wR_factor_ref         0.0295
_reflns_number_gt                3234
_reflns_number_total             3810
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            c7ce00501f2.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7228489