Synthesis of 3C-alkylated active methylene substituted 2H-indazole derivatives via sequential ring opening of donor–acceptor cyclopropanes and reductive cyclization reaction
Sahu, Archana Kumari; Biswas, Subhamoy; Bora, Surjya Kumar; Saikia, Anil K.; New Journal of Chemistry 46 (2022) 12456–12460; doi:10.1039/D2NJ01801B

data_7061596
_publ_section_title
;
 Synthesis of 3C-alkylated active methylene substituted 2H-indazole
 derivatives via sequential ring opening of donor--acceptor cyclopropanes
 and reductive cyclization reaction
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12456
_journal_page_last               12460
_journal_paper_doi               10.1039/D2NJ01801B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C20 H20 N2 O4 S'
_chemical_formula_weight         384.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.765(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.2570(8)
_cell_length_b                   13.741(2)
_cell_length_c                   13.614(2)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.35
_cell_measurement_theta_min      2.96
_cell_volume                     980.0(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17997
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        23.362
_diffrn_reflns_theta_max         23.362
_diffrn_reflns_theta_min         1.501
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 813 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.19(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.318
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0892
_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^)+(0.0535P)^2^+1.5625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2045
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                2332
_reflns_number_total             2731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01801b3.cif
_cod_data_source_block           AKS_0m_a
_cod_depositor_comments          'Adding full bibliography for 7061596.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7061596
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              99449