Palladium-Catalyzed Asymmetric [3+2] Cycloaddition to Construct 1,3-Indandione and Oxindole-Fused Spiropyrazolidine Scaffolds
Shi, Min; Cao, Bo; Mei, Liangyong; Li, Xiaoge; RSC Adv.  (2015) –; doi:10.1039/C5RA19838K

data_7223007
_publ_section_title
;
 Palladium-Catalyzed Asymmetric [3+2] Cycloaddition to Construct
 1,3-Indandione and Oxindole-Fused Spiropyrazolidine Scaffolds
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA19838K
_journal_year                    2015
_chemical_formula_sum            'C45 H35 N5 O4 S'
_chemical_formula_weight         741.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-23 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.295(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.457(3)
_cell_length_b                   17.435(3)
_cell_length_c                   22.102(3)
_cell_measurement_reflns_used    1432
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      37.275
_cell_measurement_theta_min      4.526
_cell_volume                     8108(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0941
_diffrn_reflns_av_unetI/netI     0.1113
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29136
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.681
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;
;
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.00012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3570
_reflns_number_total             7959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra19838k2.cif
_cod_data_source_block           mo_dm15591_0m
_cod_database_code               7223007
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2013-4
_shelx_res_checksum              45810