The influence of chalcogen atom on conformation and phase transition in chalcogenazinoquinolinium monoiodides
Yushina, Irina; Krylov, Alexander; Leonidov, Ivan I.; Batalov, Vladimir; Chen, Yu-Sheng; Wang, Suyin Grass; Stash, Adam; Bartashevich, Ekaterina; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520621004571

data_2108836
_publ_contact_author             'Adam Stash'
_publ_section_title
;
 The influence of chalcogen atom on conformation and phase transition in
 chalcogenazinoquinolinium monoiodides
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621004571
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C12 H11 I N S, I'
_chemical_formula_sum            'C12 H11 I2 N S'
_chemical_formula_weight         455.08
_chemical_name_systematic
;
3-(iodomethyl)-2,3-dihydro-[1,4]thiazino[2,3,4-ij]quinolin-4-ium monoiodide
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                88.1883(7)
_cell_angle_beta                 89.4720(6)
_cell_angle_gamma                73.9234(8)
_cell_formula_units_Z            4
_cell_length_a                   8.1178(2)
_cell_length_b                   12.0928(3)
_cell_length_c                   14.4689(3)
_cell_measurement_reflns_used    9143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.715
_cell_measurement_theta_min      3.070
_cell_volume                     1364.14(6)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type
;
Huber 3 circle diffractometer with PILATUS3 X CdTe 1M detector
;
_diffrn_measurement_method       \f-scan
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41426
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31252
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         16.723
_diffrn_reflns_theta_min         0.821
_diffrn_source                   'Advanced photon source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
Statistics for singles of twin component  1
 -------------------------------------------
 Scan 2-theta  R(int)   Total I>2sig(I)
    1    0.0  0.0423    14226   11834

 Statistics for singles of twin component  2
 -------------------------------------------
 Scan 2-theta  R(int)   Total I>2sig(I)
    1    0.0  0.0399    14401   11687

 Statistics for all composite reflections
 ----------------------------------------
 Scan 2-theta  R(int)   Total I>2sig(I)
    1    0.0  0.0367     2625    2473

 Statistics for all single and composite reflections
 ---------------------------------------------------
 Scan 2-theta  R(int)   Total I>2sig(I)
    1    0.0  0.0404    31252   25994

 HKLF 5 dataset constructed from all observations involving domains 1..2
   13686 Corrected reflections written to HKL file.

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.628
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0449P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5767
_reflns_number_total             6546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5079sup1.cif
_cod_data_source_block           KB02_100K
_cod_database_code               2108836
_publcif_datablock.id            {c729a655-eabd-4f8c-a5ec-06a1023ba6af}
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              11683
_shelx_hkl_checksum              26007
_cod_database_fobs_code 2108836