Crystal structure of tris[(pyridin-1-ium-2-yl)methyl]amine trichloride‒methanol‒water (1/1.829/0.342)
Van Erdewyk, Martha L.; Oshin, Kayode D.; IUCrData 3 (2018) x180826–; doi:10.1107/S241431461800826X

data_1549529
_publ_section_title
;
 Crystal structure of tris[(pyridin-1-ium-2-yl)methyl]amine
 trichloride--methanol--water (1/1.829/0.342)
;
_journal_coeditor_code           LH4035
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x180826
_journal_paper_doi               10.1107/S241431461800826X
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac
'C18 H21 N4 3+, 3Cl -, 1.829C H4 O, 0.342H2 O'
_chemical_formula_moiety
'C18 H21 N4 3+, 3(Cl -), 1.829(C H4 O), 0.342(H2 O)'
_chemical_formula_sum            'C19.83 H29 Cl3 N4 O2.17'
_chemical_formula_weight         464.50
_chemical_name_systematic
;
Tris[(pyridin-1-ium-2-yl)methyl]amine trichloride--methanol--water
(1/1.829/0.342)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                66.009(4)
_cell_angle_beta                 67.120(4)
_cell_angle_gamma                66.057(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0118(10)
_cell_length_b                   11.7295(11)
_cell_length_c                   11.7453(11)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.1205
_cell_measurement_theta_min      4.2776
_cell_volume                     1220.4(2)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015) and
<i>SHELXLE</i>  (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31160
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.252
_diffrn_reflns_theta_min         4.276
_exptl_absorpt_coefficient_mu    3.585
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.3425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       plate
_exptl_crystal_F_000             489
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.504
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.6234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1857
_reflns_number_gt                4537
_reflns_number_total             5201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh4035sup1.cif
_cod_data_source_block           I
_cod_database_code               1549529
_shelx_hkl_checksum              72057
_shelx_res_checksum              90682
_cod_database_fobs_code 1549529