Dictating the Reactivity of η<sup>3</sup>-Oxoallyl Pd-Intermediate toward 5- exo-trig Cyclization: Access to Indano-spirooxindoles.
Arunprasath, Dhanarajan; Devi Bala, Balasubramanian; Sekar, Govindasamy; The Journal of organic chemistry 83 (2018) 11298–11308; doi:10.1021/acs.joc.8b01891

data_4035631
_publ_section_title
;
 Dictating the Reactivity of \h<sup>3</sup>-Oxoallyl Pd-Intermediate
 toward 5- exo-trig Cyclization: Access to Indano-spirooxindoles.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11298
_journal_page_last               11308
_journal_paper_doi               10.1021/acs.joc.8b01891
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C32 H22 N2 O3, 0.5 (C H2 Cl2)'
_chemical_formula_sum            'C32.5 H23 Cl N2 O3'
_chemical_formula_weight         524.98
_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_creation_method           SHELXL-2014/7
_cell_angle_alpha                72.385(2)
_cell_angle_beta                 81.878(2)
_cell_angle_gamma                75.389(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5895(5)
_cell_length_b                   10.8126(6)
_cell_length_c                   14.9943(7)
_cell_measurement_reflns_used    4929
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.69
_cell_measurement_theta_min      2.45
_cell_volume                     1281.18(12)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0633
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24444
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.129
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4508
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0778P)^2^+0.8313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2573
_reflns_number_total             4508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01891_si_002.cif
_cod_data_source_block           ME
_cod_original_formula_sum        'C32.50 H23 Cl N2 O3'
_cod_database_code               4035631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              70858
_shelx_hkl_checksum              74320