Insertion of N-Tosylacetimidates/Acetimidamides onto Arynes via [2 + 2] Cycloaddition.
Kranthikumar, Ramagonolla; Chegondi, Rambabu; Chandrasekhar, Srivari; The Journal of organic chemistry 81 (2016) 2451–2459; doi:10.1021/acs.joc.5b02907

data_4036598
_publ_section_title
;
 Insertion of N-Tosylacetimidates/Acetimidamides onto Arynes via [2 + 2]
 Cycloaddition.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2451
_journal_page_last               2459
_journal_paper_doi               10.1021/acs.joc.5b02907
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C25 H26 Cl N O5 S'
_chemical_formula_weight         487.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.923(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7060(4)
_cell_length_b                   14.3230(6)
_cell_length_c                   9.7000(8)
_cell_measurement_temperature    294(2)
_cell_volume                     2377.0(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26482
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         1.190
_exptl_absorpt_coefficient_mu    0.285
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.8849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4532
_reflns_number_total             5704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b02907_si_002.cif
_cod_data_source_block           BB45
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4036598
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              29758
_shelx_hkl_checksum              58412