Stereoselective synthesis of cyclopentanone-fused benzosultams through Tomita zipper cyclization.
Ramachary, Dhevalapally B.; Krishna, Patoju M.; Reddy, T. Prabhakar; Organic & biomolecular chemistry 14 (2016) 6413–6416; doi:10.1039/c6ob01096b

data_7155148
_publ_section_title
;
 Stereoselective synthesis of cyclopentanone-fused benzosultams through
 Tomita zipper cyclization.
;
_journal_issue                   27
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6413
_journal_page_last               6416
_journal_paper_doi               10.1039/c6ob01096b
_journal_volume                  14
_journal_year                    2016
_chemical_formula_sum            'C22 H21 N O5 S'
_chemical_formula_weight         411.47
_space_group_IT_number           14
_symmetry_cell_setting           Monoclinic'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-05-16 deposited with the CCDC.
2016-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.263(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7273(11)
_cell_length_b                   13.2654(14)
_cell_length_c                   15.7765(15)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.80
_cell_volume                     2019.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46124
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.194
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.7369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                2956
_reflns_number_total             3549
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ob01096b3.cif
_cod_data_source_block           dbr2vr_a
_cod_depositor_comments
;
     Adding full bibliography for 7155148.cif.

2018-02-03
Z value and formula changed from orginal absurd values
                 miguel
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C3.38 H3.23 N0.15 O0.77 S0.15'
_cod_original_formula_units_Z    26
_cod_original_formula_weight     63.30
_cod_database_code               7155148