Efficient synthesis of functionalized spiro[indoline-3,4'-pyridines] and spiro[indene-2,4'-pyridines] via three-component reaction
Zhang, Jing; Sun, Jing; Yan, Chao Guo; RSC Adv.  (2015) –; doi:10.1039/C5RA15139B

data_7222293
_publ_section_title
;
 Efficient synthesis of functionalized spiro[indoline-3,4'-pyridines] and
 spiro[indene-2,4'-pyridines] via three-component reaction
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA15139B
_journal_year                    2015
_chemical_formula_moiety         'C34 H25 N3 O6'
_chemical_formula_sum            'C34 H25 N3 O6'
_chemical_formula_weight         571.57
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jhlf1
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-23 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                83.195(8)
_cell_angle_beta                 66.986(7)
_cell_angle_gamma                81.841(7)
_cell_formula_units_Z            2
_cell_length_a                   10.963(2)
_cell_length_b                   12.057(3)
_cell_length_c                   12.362(3)
_cell_measurement_reflns_used    4812
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.39
_cell_volume                     1485.2(6)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22725
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1735
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.3611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                3148
_reflns_number_total             6786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra15139b2.cif
_cod_data_source_block           zj150724
_cod_database_code               7222293