Crystal structure and Hirshfeld surface analysis of a pyrrolo-thiazine complex
Sribala, R.; Srinivasan, N.; Rajalaksmi, P.; Indumathi, S.; Krishnakumar, R.V.; Acta Crystallographica Section E 77 (2021) 770–774; doi:10.1107/S2056989021006642

data_2243862
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of a pyrrolo-thiazine
 complex
;
_journal_coeditor_code           JY2008
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              770
_journal_page_last               774
_journal_paper_doi               10.1107/S2056989021006642
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C22 H28 N O6 S3'
_chemical_formula_moiety         'C22 H28 N O6 S3'
_chemical_formula_sum            'C22 H28 N O6 S3'
_chemical_formula_weight         498.66
_chemical_name_systematic
'Diethyl 2,2-dioxo-4-(thiophen-2-yl)-1-[(thiophen-2-yl)methyl]-3,4,6,7,8,8a-hexahydro-1<i>H</i>-pyrrolo[2,1-<i>c</i>][1,4]thiazine-1,3-dicarboxylate'
_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                76.0070(10)
_cell_angle_beta                 65.5840(10)
_cell_angle_gamma                63.2130(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6886(5)
_cell_length_b                   11.4878(5)
_cell_length_c                   11.8389(6)
_cell_measurement_reflns_used    6274
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.306
_cell_measurement_theta_min      4.796
_cell_volume                     1178.87(10)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
PLUTON (Spek, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2013/1</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.280
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2009)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_meas      1.40
_exptl_crystal_density_method    'floatation method'
_exptl_crystal_description       needle
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.563
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4375
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0758P)^2^+0.5387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                3774
_reflns_number_total             4375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jy2008sup1.cif
_cod_data_source_block           I
_cod_database_code               2243862
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.966
_shelx_hkl_checksum              4030
_shelx_res_checksum              98184
_cod_database_fobs_code 2243862