Crystal structure of 2-cyano-1-methylpyridinium perchlorate
Nguyen, Vu D.; McCormick, Cameron A.; Mague, Joel T.; Koplitz, Lynn V.; Acta Crystallographica Section E 71 (2015) o852–o853; doi:10.1107/S2056989015019155

data_2241244
_publ_section_title
;
 Crystal structure of 2-cyano-1-methylpyridinium perchlorate
;
_journal_coeditor_code           TK5395
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o852
_journal_page_last               o853
_journal_paper_doi               10.1107/S2056989015019155
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C7 H7 N2 +, Cl O4 -'
_chemical_formula_moiety         'C7 H7 N2 +, Cl O4 -'
_chemical_formula_sum            'C7 H7 Cl N2 O4'
_chemical_formula_weight         218.60
_chemical_name_systematic
;
2-Cyano-1-methylpyridinium perchlorate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.982(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0112(12)
_cell_length_b                   7.7011(12)
_cell_length_c                   14.742(2)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1731
_cell_measurement_theta_min      2.5428
_cell_volume                     909.4(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2014) and <i>CELL_NOW</i> (Sheldrick,
2008a)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008b)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22843
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         29.173
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.341
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1908 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         22843
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0531P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                20913
_reflns_number_total             22843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk5395sup1.cif
_cod_data_source_block           I
_cod_database_code               2241244
_cod_database_fobs_code          2241244
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.949
_shelx_hkl_checksum              58730
_shelx_res_checksum              82566
_shelxl_version_number           2.014