Synthesis of spiroindolenine-cyclopentenedione skeletons and their chemical behaviours: the first example of a lactone-type spiroindolenine structure.
Tan Uygun, Meltem; Menges, Nurettin; Organic & biomolecular chemistry 20 (2022) 4161–4166; doi:10.1039/d2ob00396a

data_7158637
_publ_section_title
;
 Synthesis of spiroindolenine-cyclopentenedione skeletons and their
 chemical behaviours: the first example of a lactone-type spiroindolenine
 structure.
;
_journal_issue                   20
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4161
_journal_page_last               4166
_journal_paper_doi               10.1039/d2ob00396a
_journal_volume                  20
_journal_year                    2022
_chemical_formula_moiety         'C27 H19 N O4, C27 H17 N O4'
_chemical_formula_sum            'C27 H18 N O4'
_chemical_formula_weight         420.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-11-27 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                66.179(7)
_cell_angle_beta                 79.925(8)
_cell_angle_gamma                88.526(9)
_cell_formula_units_Z            4
_cell_length_a                   9.3467(10)
_cell_length_b                   15.2593(17)
_cell_length_c                   16.6257(18)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      17.9948
_cell_measurement_theta_min      2.5138
_cell_volume                     2133.1(4)
_computing_cell_refinement       'APEX2 v2014.9-0 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service v2013.12.0.0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material
'PLATON V1.16 (Spek, 2009), SHELXTL V6.14 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL V6.14 (Bruker AXS)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker APEX II QUAZAR three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer QUAZAR mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28845
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.36
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              ImuS
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.290
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.0946
_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^)+(0.1630P)^2^+0.3882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2608
_refine_ls_wR_factor_ref         0.3321
_reflns_number_gt                3305
_reflns_number_total             7498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob00396a2.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 7158637.cif.'
_cod_database_code               7158637
_shelx_res_checksum              43414