1,1′-Methylenebis(4-tert-butylpyridinium) dichloride hemihydrate
Bruekers, J.P.J.; Elemans, J.A.A.W.; Nolte, R.J.M.; Tinnemans, P.; IUCrData 6 (2021) x210768–; doi:10.1107/S2414314621007689

data_1564318
_publ_section_title
;
 1,1&#x2032;-Methylenebis(4-tert-butylpyridinium) dichloride hemihydrate
;
_journal_coeditor_code           BT4117
_journal_issue                   8
_journal_name_full               IUCrData
_journal_page_first              x210768
_journal_paper_doi               10.1107/S2414314621007689
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          'C19 H28 N2 2+, 2Cl -, 0.5H2 O'
_chemical_formula_moiety         'C19 H28 N2 2+, 2(Cl -), 0.5(H2 O)'
_chemical_formula_sum            'C19 H29 Cl2 N2 O0.5'
_chemical_formula_weight         364.34
_chemical_name_systematic
;
1,1'-Methylenebis(4-<i>tert</i>-butylpyridinium) dichloride hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 97.4152(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.7659(8)
_cell_length_b                   5.9001(2)
_cell_length_c                   23.9758(7)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.4
_cell_volume                     3894.9(2)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020) and <i>shelXle</i> (H\"ubschle <i>et al.</i>,
2011)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker D8 Quest APEX3'
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36472
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.198
_diffrn_reflns_theta_min         2.404
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       needle
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.546
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         7428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+4.7462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                5988
_reflns_number_total             7428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4117sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1564318
_cod_database_fobs_code          1564318
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.990
_shelx_hkl_checksum              24834
_shelx_res_checksum              1021