Efficient synthesis of novel cyclic fused-phenothiazines via domino cyclization of 2-(benzo[b][1,4]thiazin-3-ylidene)acetate, aromatic aldehydes and cyclic 1,3-diketones
Sun, Jing; Sun, Quan-Shun; Yan, Chao-Guo; Organic Chemistry Frontiers 6 (2019) 3555–; doi:10.1039/C9QO00951E

data_1555145
_publ_section_title
;
 Efficient synthesis of novel cyclic fused-phenothiazines via domino
 cyclization of 2-(benzo[b][1,4]thiazin-3-ylidene)acetate, aromatic
 aldehydes and cyclic 1,3-diketones
;
_journal_issue                   20
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              3555
_journal_paper_doi               10.1039/C9QO00951E
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C31 H26 N2 O4 S2'
_chemical_formula_sum            'C31 H26 N2 O4 S2'
_chemical_formula_weight         554.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-26 deposited with the CCDC.	2019-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.263(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   22.343(2)
_cell_measurement_reflns_used    3891
_cell_measurement_temperature    273(2)
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_cell_measurement_theta_min      2.33
_cell_volume                     2793.1(4)
_computing_cell_refinement       'Bruker SAINT'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
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_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.331
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_description       block
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_refine_diff_density_max         0.952
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.2165
_refine_ls_R_factor_gt           0.0930
_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^)+(0.1209P)^2^+1.1685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2271
_refine_ls_wR_factor_ref         0.2662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2410
_reflns_number_total             5473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00951e2.cif
_cod_data_source_block           9c
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1555145
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              62472
_shelx_hkl_checksum              90081