Auto-Tandem Palladium Catalysis: From Isoxazole to 2-Azafluorenone.
Das, Sajal; Hong, Dongsub; Chen, Zhiwei; She, Zhigang; Hersh, William H.; Subramaniam, Gopal; Chen, Yu; Organic letters 17 (2015) 5578–5581; doi:10.1021/acs.orglett.5b02731

data_1540624
_publ_section_title
;
 Auto-Tandem Palladium Catalysis: From Isoxazole to 2-Azafluorenone.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5578
_journal_page_last               5581
_journal_paper_doi               10.1021/acs.orglett.5b02731
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C17 H19 N O2'
_chemical_formula_sum            'C17 H19 N O2'
_chemical_formula_weight         269.33
_chemical_name_common            'o-(t-Bu isoxazole) MVK benzene'
_chemical_name_systematic
(E)-4-(2-(3-(tert-butyl)isoxazol-5-yl)phenyl)but-3-en-2-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'APEX2 v2014.11-0'
_cell_angle_alpha                90
_cell_angle_beta                 90.554(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5944(18)
_cell_length_b                   19.750(4)
_cell_length_c                   7.9170(15)
_cell_measurement_reflns_used    6104
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.36
_cell_volume                     1500.1(5)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V7.68A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Farrugia ORTEP-3/v2.02'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Breeze CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17411
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.222
_diffrn_reflns_theta_min         2.062
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear white'
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.677
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.295
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6958
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.4948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2832
_reflns_number_total             3345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b02731_si_002.cif
_cod_data_source_block           YC_13_46_1_3_p282_a
_cod_database_code               1540624
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              81102
_shelx_hkl_checksum              32458