Palladium-Catalyzed Stereospecific Oxidative Cascade Reaction of Allenes for the Construction of Pyrrole Rings: Control of Reactivity and Selectivity
Li, Man-Bo; Grape, Erik Svensson; Bäckvall, Jan-E.; ACS Catalysis 9 (2019) 5184–; doi:10.1021/acscatal.9b01041

data_4514784
_publ_section_title
;
 Palladium-Catalyzed Stereospecific Oxidative Cascade Reaction of Allenes
 for the Construction of Pyrrole Rings: Control of Reactivity and
 Selectivity
;
_journal_issue                   6
_journal_name_full               'ACS Catalysis'
_journal_page_first              5184
_journal_paper_doi               10.1021/acscatal.9b01041
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C28 H27 N O2 S'
_chemical_formula_weight         441.56
_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   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 109.7140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0088(3)
_cell_length_b                   9.6520(2)
_cell_length_c                   19.0811(4)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.54
_cell_measurement_theta_min      2.46
_cell_volume                     2428.79(9)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            88468
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.567
_diffrn_reflns_theta_min         3.351
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (1996). SADABS. University of G&#x00C3;&#x00B6;ttingen, Germany.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       stubby
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0578P)^2^+0.5495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3860
_reflns_number_total             4816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b01041_si_003.cif
_cod_data_source_block           manbo_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4514784
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              8675
_shelx_hkl_checksum              34919