Convenient Synthesis of Triphenylphosphanylidene Spiro[cyclopentane-1,3'-indolines] and Spiro[cyclopent[2]ene-1,3'-indolines] via Three-Component Reactions.
Han, Ying; Sheng, Yin-Jian; Yan, Chao-Guo; Organic letters 16 (2014) 2654–2657; doi:10.1021/ol5008394

data_1514910
_publ_section_title
;
 Convenient Synthesis of Triphenylphosphanylidene
 Spiro[cyclopentane-1,3'-indolines] and
 Spiro[cyclopent[2]ene-1,3'-indolines] via Three-Component Reactions.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2654
_journal_page_last               2657
_journal_paper_doi               10.1021/ol5008394
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C42 H31 F N3 O5 P'
_chemical_formula_sum            'C42 H31 F N3 O5 P'
_chemical_formula_weight         707.67
_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_creation_method           SHELXL-97
_cell_angle_alpha                88.992(5)
_cell_angle_beta                 74.957(4)
_cell_angle_gamma                66.544(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3434(8)
_cell_length_b                   10.8351(9)
_cell_length_c                   17.8432(14)
_cell_measurement_reflns_used    6531
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.27
_cell_volume                     1763.3(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25785
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0504P)^2^+0.3307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                5045
_reflns_number_total             8188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5008394_si_003.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 1514910--1514912.cif.'
_cod_database_code               1514910