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_7118660
_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            'C45 H39.5 Br1.5 Cl2 N5 Ni'
_chemical_formula_weight         899.79
_chemical_name_systematic        2-bromo-10-azacorrole
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_update_record
;
2015-04-14 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.783(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.489(2)
_cell_length_b                   20.454(3)
_cell_length_c                   12.894(2)
_cell_measurement_reflns_used    3562
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.39
_cell_volume                     4038.2(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0765
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23120
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    2.136
_exptl_absorpt_correction_T_max  0.9007
_exptl_absorpt_correction_T_min  0.4820
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1836
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dichloroethane'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.645
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1924P)^2^+23.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2854
_refine_ls_wR_factor_ref         0.3347
_reflns_number_gt                4220
_reflns_number_total             7118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc10247b2.cif
_cod_data_source_block           13620ho
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7118659--7118660.cif.
;
_cod_original_cell_volume        4038.3(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C45 H39.50 Br1.50 Cl2 N5 Ni'
_cod_database_code               7118660