Syntheses and crystal structures of 2-(<i>p</i>-tolyl)-1<i>H</i>-perimidine hemihydrate and 1-methyl-2-(<i>p</i>-tolyl)-1<i>H</i>-perimidine
Kalle, Paulina; Tatarin, Sergei V.; Kiseleva, Marina A.; Zakharov, Alexander Yu.; Smirnov, Daniil E.; Bezzubov, Stanislav I.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022000287

data_2244009
_publ_section_title
;
 Syntheses and crystal structures of
 2-(<i>p</i>-tolyl)-1<i>H</i>-perimidine hemihydrate and
 1-methyl-2-(<i>p</i>-tolyl)-1<i>H</i>-perimidine
;
_journal_coeditor_code           WM5631
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022000287
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C18 H14 N2, 0.5H2 O'
_chemical_formula_moiety         'C18 H14 N2, 0.5(H2 O)'
_chemical_formula_sum            'C18 H15 N2 O0.5'
_chemical_formula_weight         267.32
_chemical_name_systematic
;
2-(4-Methylphenyl)-1<i>H</i>-perimidine hemihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   7.2131(2)
_cell_length_b                   13.8648(5)
_cell_length_c                   53.4532(18)
_cell_measurement_reflns_used    4300
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.45
_cell_measurement_theta_min      3.04
_cell_volume                     5345.8(3)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_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
;
SHELXL  (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS  (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON II'
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            14708
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.996
_diffrn_reflns_theta_min         3.036
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2138
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0761P)^2^+4.7998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                1630
_reflns_number_total             2138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5631sup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C18 H15 N2 O0.50'
_cod_database_code               2244009
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              65709
_shelx_res_checksum              77917
_cod_database_fobs_code 2244009