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_1543842
_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 H45 N5 O2 Zn'
_chemical_formula_weight         753.23
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1814(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5138(6)
_cell_length_b                   7.8297(2)
_cell_length_c                   25.5113(8)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.0122
_cell_measurement_theta_min      2.3539
_cell_volume                     3761.77(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25251
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.9209
_exptl_absorpt_correction_T_min  0.7533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+5.8225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                5641
_reflns_number_total             6606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b01323_si_002.cif
_cod_data_source_block           shino140515oh1_0m
_cod_database_code               1543842