Titanocene(III)-Mediated 5-exo-trig Radical Cyclization: En Route to Spirooxindole-Based Tetrahydrofuran and Bicyclic Lactone.
Nallasivam, Jothi Lakshmi; Chakraborty, Tushar Kanti; The Journal of organic chemistry 84 (2019) 16124–16138; doi:10.1021/acs.joc.9b02608

data_4037631
_publ_section_title
;
 Titanocene(III)-Mediated 5-exo-trig Radical Cyclization: En Route to
 Spirooxindole-Based Tetrahydrofuran and Bicyclic Lactone.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              16124
_journal_page_last               16138
_journal_paper_doi               10.1021/acs.joc.9b02608
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C24 H27 N O5'
_chemical_formula_sum            'C24 H27 N O5'
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_space_group_name_Hall           '-P 2yn'
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_cell_angle_alpha                90
_cell_angle_beta                 94.998(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2282(14)
_cell_length_b                   9.0871(9)
_cell_length_c                   16.8947(16)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.98
_cell_volume                     2176.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.1524
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46902
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.803
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.7214
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       TABULAR
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.065
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1987
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_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^)+(0.0662P)^2^+1.7987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.2108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2248
_reflns_number_total             5120
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4037631--4037632.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4037631
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              95798
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