Crystal structure of 1,3-dimethyl-2-(p-tolyl)-1H-perimidin-3-ium iodide 1.5 hydrate, C20H22IN2O1.5
Yuan, Lin; Li, Zhong-Yan; Yuan, Xian-You; Zhang, Min; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 1031–1032; doi:10.1515/ncrs-2018-0149

data_8106388
_publ_section_title
;
 Crystal structure of 1,3-dimethyl-2-(p-tolyl)-1H-perimidin-3-ium iodide
 1.5 hydrate, C20H22IN2O1.5
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1031
_journal_page_last               1032
_journal_paper_doi               10.1515/ncrs-2018-0149
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'I, 1.5(H2 O), C20 H19 N2'
_chemical_formula_sum            'C20 H22 I N2 O1.5'
_chemical_formula_weight         441.29
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 127.7190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   38.828(4)
_cell_length_b                   9.5689(9)
_cell_length_c                   26.186(2)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.23
_cell_volume                     7696.0(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0184
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35774
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.33
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.676
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0377 after correction.
The Ratio of minimum to maximum transmission is 0.7770.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3536
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+23.0625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                5614
_reflns_number_total             6781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2018-0149_suppl.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H44 I2 N4 O3'
_cod_original_formula_weight         882.59
_cod_original_formula_moiety         '2(I), 3(H2 O), 2(C20 H19 N2)'
_cod_original_formula_units_Z            8
_cod_database_code               8106388
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B), O1(H1A,H1B), O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C15(H15), C16(H16), C9(H9), C8(H8), C7(H7), C18(H18), C19(H19),
 C3(H3), C4(H4), C25(H25), C24(H24), C23(H23), C39(H39), C38(H38), C27(H27),
 C35(H35), C36(H36), C29(H29), C28(H28)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C40(H40A,H40B,
 H40C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'