The different modes of chiral [1,2,3]triazolo[5,1-<i>b</i>][1,3,4]thiadiazines: crystal packing, conformation investigation and cellular activity
Obydennov, Konstantin L'vovich; Kalinina, Tatiana Andreevna; Vysokova, Olga Alexandrovna; Slepukhin, Pavel Alexandrovich; Pozdina, Varvara Alexandrovna; Ulitko, Maria Valer'evna; Glukhareva, Tatiana Vladimirovna; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620009328

data_2022203
_publ_section_title
;
 The different modes of chiral
 [1,2,3]triazolo[5,1-<i>b</i>][1,3,4]thiadiazines: crystal packing,
 conformation investigation and cellular activity
;
_journal_coeditor_code           FM3064
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620009328
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C20 H24 N4 O4 S'
_chemical_formula_moiety         'C20 H24 N4 O4 S'
_chemical_formula_sum            'C20 H24 N4 O4 S'
_chemical_formula_weight         416.49
_chemical_name_systematic
'Ethyl 5'-(4-methoxybenzoyl)-5'<i>H</i>,7'<i>H</i>-spiro[cyclohexane-1,6'-[1,2,3]triazolo[5,1-<i>b</i>][1,3,4]thiadiazine]-3'-carboxylate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.5394(14)
_cell_length_b                   8.0288(3)
_cell_length_c                   9.1435(4)
_cell_measurement_reflns_used    2233
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.9970
_cell_measurement_theta_min      2.6510
_cell_volume                     2095.12(16)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009), PLATON (Spek, 2020) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur 3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6492
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.537
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.82157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.186
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 735 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3439
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                2926
_reflns_number_total             3439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fm3064sup1.cif
_cod_data_source_block           IV
_cod_database_code               2022203
_cod_database_fobs_code          2022203
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.972
_shelx_hkl_checksum              9062
_shelx_res_checksum              15185