Palladium-Catalyzed Double-Isocyanide Insertion via Oxidative N-O Cleavage of Acetyl Oximes: Syntheses of 2H-Pyrrol-2-imines.
Senadi, Gopal Chandru; Lu, Ting-Yi; Dhandabani, Ganesh Kumar; Wang, Jeh-Jeng; Organic letters 19 (2017) 1172–1175; doi:10.1021/acs.orglett.7b00208

data_1545439
_publ_section_title
;
 Palladium-Catalyzed Double-Isocyanide Insertion via Oxidative N-O
 Cleavage of Acetyl Oximes: Syntheses of 2H-Pyrrol-2-imines.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1172
_journal_page_last               1175
_journal_paper_doi               10.1021/acs.orglett.7b00208
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C20 H27 N3 O2'
_chemical_formula_sum            'C20 H27 N3 O2'
_chemical_formula_weight         341.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.724(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5287(7)
_cell_length_b                   13.0679(8)
_cell_length_c                   14.2874(8)
_cell_measurement_reflns_used    5787
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.248
_cell_measurement_theta_min      2.970
_cell_volume                     1956.0(2)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         3.118
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+1.0326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2628
_reflns_number_total             3997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00208_si_002.cif
_cod_data_source_block           rp2167
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1545439
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              17115
_shelx_hkl_checksum              5685