Structural polymorphism of pyrazinium hydrogen sulfate: extending chemistry of the pyrazinium salts with small anions
Budzianowski, Armand; Derzsi, Mariana; Leszczyński, Piotr J.; Cyrański, Michał K.; Grochala, Wojciech; Acta Crystallographica Section B 66 (2010) 451–457; doi:10.1107/S0108768110019580

data_2104781
_publ_section_title
;
 Structural polymorphism of pyrazinium hydrogen sulfate: extending
 chemistry of the pyrazinium salts with small anions
;
_journal_coeditor_code           EB5006
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              451
_journal_page_last               457
_journal_paper_doi               10.1107/S0108768110019580
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C4 H5 N2, H O4 S'
_chemical_formula_sum            'C4 H6 N2 O4 S'
_chemical_formula_weight         178.17
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
and SHELXL-97
;
_cell_angle_alpha                86.484(12)
_cell_angle_beta                 88.111(11)
_cell_angle_gamma                77.487(12)
_cell_formula_units_Z            4
_cell_length_a                   5.3552(7)
_cell_length_b                   7.4832(10)
_cell_length_c                   16.506(2)
_cell_measurement_reflns_used    2099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6598
_cell_measurement_theta_min      2.9775
_cell_volume                     644.40(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.6479
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scans'
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.2283
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12016
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.99
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED, Oxford Diffraction Ltd.'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.446
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0491
_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/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                1242
_reflns_number_total             3124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb5006.cif
_cod_data_source_block           PHSb-100K
_cod_original_cell_volume        644.38(15)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               2104781
_cod_database_fobs_code          2104781