Synthesis of Free-Base 10-Azacorroles.
Omori, Hiroto; Hiroto, Satoru; Shinokubo, Hiroshi; Organic letters 18 (2016) 2978–2981; doi:10.1021/acs.orglett.6b01323

data_1543843
_publ_section_title
;
 Synthesis of Free-Base 10-Azacorroles.
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              2978
_journal_page_last               2981
_journal_paper_doi               10.1021/acs.orglett.6b01323
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C45 H40.84 Br0.16 Cl2 N5 Pd'
_chemical_formula_weight         841.86
_chemical_name_systematic
;
 ?
;
_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           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 112.282(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4227(16)
_cell_length_b                   20.557(2)
_cell_length_c                   12.5961(12)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.1372
_cell_measurement_theta_min      2.3922
_cell_volume                     3934.9(7)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18421
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.137
_diffrn_reflns_theta_min         2.392
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       prism
_exptl_crystal_F_000             1726
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.425
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+36.3833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5574
_reflns_number_total             6588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01323_si_004.cif
_cod_data_source_block           shino_160221_oh_0ma_a
_cod_database_code               1543843
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2014-3
_shelx_res_checksum              50989
_shelx_hkl_checksum              39659