The synthesis of Ni(II) and Al(III) 10-azacorroles through coordination-induced cyclisation involving 1,2-migration.
Omori, Hiroto; Hiroto, Satoru; Shinokubo, Hiroshi; Chemical communications (Cambridge, England) 52 (2016) 3540–3543; doi:10.1039/c5cc10247b

data_7118659
_publ_section_title
;
 The synthesis of Ni(II) and Al(III) 10-azacorroles through
 coordination-induced cyclisation involving 1,2-migration.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3540
_journal_page_last               3543
_journal_paper_doi               10.1039/c5cc10247b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C49 H51 Br2 Cu N5'
_chemical_formula_weight         933.30
_chemical_name_systematic
'5-mesityl-N,N-bis(alpha-bromodipyrrinyl)amine Cu(II)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-04-14 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.4817(9)
_cell_length_b                   41.726(2)
_cell_length_c                   31.034(3)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    90.(2)
_cell_measurement_theta_max      23.9727
_cell_measurement_theta_min      2.4798
_cell_volume                     17458(2)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      90.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            102658
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7664
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.930
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.616
_refine_diff_density_min         -1.161
_refine_ls_abs_structure_details
;
Flack x determined using 7533 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.493(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2084
_refine_ls_number_reflns         27981
_refine_ls_number_restraints     2231
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0574P)^2^+238.8542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2080
_reflns_number_gt                19106
_reflns_number_total             27981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc10247b2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7118659--7118660.cif.'
_cod_original_cell_volume        17458.(2)
_cod_database_code               7118659
_shelx_res_checksum              14884
_shelx_hkl_checksum              55581