Protonated nucleobases are not fully ionized in their chloride salt crystals and form metastable base pairs further stabilized by the surrounding anions
Kumar, Prashant; Cabaj, Malgorzata Katarzyna; Pazio, Aleksandra; Dominiak, Paulina Maria; IUCrJ 5 (2018) –; doi:10.1107/S2052252518006346

data_1549526
_publ_section_title
;
 Protonated nucleobases are not fully ionized in their chloride salt
 crystals and form metastable base pairs further stabilized by the
 surrounding anions
;
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252518006346
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C5 H6 N5, Cl, 0.5(H2 O)'
_chemical_formula_sum            'C5 H7 Cl N5 O0.5'
_chemical_formula_weight         180.60
_chemical_name_systematic        'adeninium chloride hemihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0
_cell_angle_beta                 93.526(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   8.6936(1)
_cell_length_b                   4.8189(1)
_cell_length_c                   17.6971(1)
_cell_measurement_reflns_used    35568
_cell_measurement_temperature    89.9(3)
_cell_measurement_theta_max      65.7090
_cell_measurement_theta_min      2.5400
_cell_volume                     739.992(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      89.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0013
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
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_diffrn_measurement_details
;
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omega____ theta____ kappa____ phi______ frames
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  2 omega   35.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -10.00   17.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701  103.0000 -165.7302 27

  4 omega   44.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   77.0000 -120.0000 26

  5 omega   44.00   74.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701  -99.0000   30.0000 30

  6 omega   36.00   78.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
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  7 omega    4.00   35.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
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  8 omega   39.00  100.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
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  9 omega  -27.00   63.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
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 10 omega   11.00   37.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   77.0000 -120.0000 26

 11 omega   20.00  102.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   37.0000  150.0000 82

 12 omega    4.00   49.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   77.0000    0.0000 45

 13 omega  -19.00   74.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701  -99.0000 -150.0000 93

 14 omega   13.00   77.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   37.0000   30.0000 64

 15 omega    4.00  102.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   77.0000  -90.0000 98

 16 omega  -20.00   16.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701  -99.0000   30.0000 36

 17 omega   13.00   92.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   37.0000  -90.0000 79

 18 omega   16.00   93.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       33.5701   37.0000   90.0000 77

 19 omega   75.00  101.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   68.0000  108.3264 26

 20 omega  108.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   75.0000  -55.0523 50

 21 omega   72.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   71.0000 -163.1496 86

 22 omega   70.00   96.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   75.0000  -55.0523 26

 23 omega   30.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -94.0000   90.0000 65

 24 omega   28.00   76.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -45.0000 -120.0000 48

 25 omega   29.00   57.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -45.0000   60.0000 28

 26 omega   69.00   94.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  150.0000 25

 27 omega  120.00  146.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  150.0000 26

 28 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000   90.0000 26

 29 omega   78.00  143.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000  120.0000 65

 30 omega   75.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   45.0000 -120.0000 83

 31 omega   70.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   75.0000 -132.9202 25

 32 omega   77.00  103.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   57.0000  -91.7021 26

 33 omega   70.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   74.0000  -66.6346 25

 34 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  -30.0000 26

 35 omega   56.00   91.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -94.0000  -90.0000 35

 36 omega   69.00   94.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   76.0000   71.7607 25

 37 omega   27.00  110.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342 -111.0000    0.0000 83

 38 omega  118.00  156.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000    0.0000 38

 39 omega   71.00  135.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   32.0000   92.1535 64

 40 omega   70.00  156.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   75.0000  -14.9019 86

 41 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000    0.0000 26

 42 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000   30.0000 26

 43 omega  122.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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 44 omega   77.00  103.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000   60.0000 26

 45 omega   69.00   94.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  120.0000 25

 46 omega   27.00  109.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -94.0000  150.0000 82

 47 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000 -150.0000 26

 48 omega   28.00   76.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -45.0000    0.0000 48

 49 omega   77.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000  -90.0000 81

 50 omega   77.00  103.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000  150.0000 26

 51 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000   60.0000 26

 52 omega   70.00   96.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   74.0000   28.1936 26

 53 omega   77.00  111.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000   30.0000 34

 54 omega   75.00  101.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   45.0000 -180.0000 26

 55 omega   77.00  149.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000 -180.0000 72

 56 omega  129.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   74.0000    8.6196 29

 57 omega   34.00  121.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -61.0000  150.0000 87

 58 omega   69.00   95.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000 -120.0000 26

 59 omega   70.00   96.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   74.0000  -31.7065 26

 60 omega   69.00   94.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  -90.0000 25

 61 omega   27.00   87.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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 62 omega   69.00   94.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000 -180.0000 25

 63 omega   71.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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 64 omega   70.00   97.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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 65 omega   75.00  101.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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 66 omega   76.00  119.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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 67 omega   71.00  158.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
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;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0383486000
_diffrn_orient_matrix_UB_12      -0.0212799000
_diffrn_orient_matrix_UB_13      0.0337655000
_diffrn_orient_matrix_UB_21      0.0661169000
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_diffrn_radiation_monochromator  mirror
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_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.462
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'transparent colorless'
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
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_refine_diff_density_max         0.29
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         11241
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.000
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          -0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0283
_refine_ls_wR_factor_ref         0.0283
_reflns_d_resolution_high        0.39
_reflns_d_resolution_low         8.83
_reflns_limit_h_max              22
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_reflns_limit_k_max              12
_reflns_limit_k_min              0
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_reflns_number_gt                11241
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_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            lc5097.cif
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_cod_original_sg_symbol_H-M      'P 1 2/c 1'
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