Regioselective phenylene-fusion reactions of Ni(ii)-porphyrins controlled by an electron-withdrawing meso-substituent
Fukui, Norihito; Lee, Seung-Kyu; Kato, Kenichi; Shimizu, Daiki; Tanaka, Takayuki; Lee, Sangsu; Yorimitsu, Hideki; Kim, Dongho; Osuka, Atsuhiro; Chem. Sci. 7 (2016) 4059–; doi:10.1039/C5SC04748J

data_1542593
_publ_section_title
;
 Regioselective phenylene-fusion reactions of Ni(ii)-porphyrins controlled
 by an electron-withdrawing meso-substituent
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4059
_journal_paper_doi               10.1039/C5SC04748J
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C62 H69 N5 Ni O2, C7 H8'
_chemical_formula_sum            'C69 H77 N5 Ni O2'
_chemical_formula_weight         1067.06
_chemical_name_systematic        '13,15-phenylene-fused meso-nitroporphyrin'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-27 deposited with the CCDC.
2016-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.073(8)
_cell_angle_beta                 103.209(15)
_cell_angle_gamma                109.518(5)
_cell_formula_units_Z            4
_cell_length_a                   14.734(6)
_cell_length_b                   20.554(8)
_cell_length_c                   20.788(9)
_cell_measurement_reflns_used    2590
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.0
_cell_measurement_theta_min      25.3
_cell_volume                     5756(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1359
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68526
_diffrn_reflns_theta_full        63.50
_diffrn_reflns_theta_max         63.50
_diffrn_reflns_theta_min         6.53
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.9914
_exptl_absorpt_correction_T_min  0.8123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1387
_refine_ls_number_reflns         18297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1832
_refine_ls_R_factor_gt           0.1419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+135.7153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3453
_refine_ls_wR_factor_ref         0.3713
_reflns_number_gt                12239
_reflns_number_total             18297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04748j2.cif
_cod_data_source_block           41001fu
_cod_depositor_comments
'Adding full bibliography for 1542591--1542594.cif.'
_cod_database_code               1542593