Enantioselective construction of dispirotriheterocycles featuring a 4-aminopyrazolone motif through a cascade Michael/cyclization process.
Wei, Shiqiang; Bao, Xiaoze; Wang, Wenyao; Nawaz, Shah; Dai, Qimin; Qu, Jingping; Wang, Baomin; Chemical communications (Cambridge, England) 56 (2020) 10690–10693; doi:10.1039/d0cc04215c

data_7127018
_publ_section_title
;
 Enantioselective construction of dispirotriheterocycles featuring a
 4-aminopyrazolone motif through a cascade Michael/cyclization process.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10690
_journal_page_last               10693
_journal_paper_doi               10.1039/d0cc04215c
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_sum            'C36 H29 Br N4 O4 S'
_chemical_formula_weight         693.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-04-13 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4627(13)
_cell_length_b                   10.6763(14)
_cell_length_c                   29.015(4)
_cell_measurement_reflns_used    5582
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.7135
_cell_measurement_theta_min      2.3674
_cell_volume                     3241.1(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17760
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.033
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.240
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5742
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 1857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0200P)^2^+2.5524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4930
_reflns_number_total             5728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04215c2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7127018.cif.'
_cod_original_cell_volume        3241.0(7)
_cod_database_code               7127018
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.667
_shelx_estimated_absorpt_t_max   0.733
_shelx_res_checksum              84673
_shelx_hkl_checksum              86341