The crystal structure of 1,2-bis(pyridinium-4-yl)ethane diperchlorate, C12H14N2·2ClO4 – a second polymorph
Qiu, Qi-Ming; Song, Jian-Biao; Yan, Li; Dong, Ai-Guo; Li, Chuan-Tao; Zheng, Zhi-Yuan; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 695–696; doi:10.1515/ncrs-2022-0190

data_8107191
_publ_section_title
;
 The crystal structure of 1,2-bis(pyridinium-4-yl)ethane diperchlorate,
 C12H14N2&#x00B7;2ClO4&#x00A0;-- a second polymorph
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              695
_journal_page_last               696
_journal_paper_doi               10.1515/ncrs-2022-0190
_journal_volume                  237
_journal_year                    2022
_chemical_formula_sum            'C12 H14 Cl2 N2 O8'
_chemical_formula_weight         385.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 100.888(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.3170(4)
_cell_length_b                   12.8711(8)
_cell_length_c                   11.6788(7)
_cell_measurement_reflns_used    1338
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      71.52
_cell_measurement_theta_min      3.381
_cell_volume                     784.86(9)
_computing_cell_refinement       'Bruker SMART [1]'
_computing_data_collection       'Bruker SMART [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'Bruker SHELXTL [2]'
_computing_publication_material  'Bruker SHELXTL [2]'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018) [3]'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018) [2]'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.493
_diffrn_reflns_theta_min         5.165
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.165
_exptl_absorpt_correction_T_max  0.7317
_exptl_absorpt_correction_T_min  0.4896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0127(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0582P)^2^+0.3593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1338
_reflns_number_total             1500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0190_suppl.cif
_cod_data_source_block           170222b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8107191
_shelx_estimated_absorpt_t_min   0.681
_shelx_estimated_absorpt_t_max   0.851
_diffrn_scan_mode                'continuous scan'
_shelx_res_checksum              32145
_shelx_hkl_checksum              90752