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_1542594
_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_sum            'C74 H77 N4 Ni O P'
_chemical_formula_weight         1128.07
_chemical_name_systematic
'doubly 10,12- and 18,20-phenylene-fused meso-diphenylphosphinylporphyrin'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-27 deposited with the CCDC.
2016-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.168(4)
_cell_angle_gamma                90
_cell_formula_units_Z            9
_cell_length_a                   12.3714(16)
_cell_length_b                   28.233(3)
_cell_length_c                   41.360(6)
_cell_measurement_reflns_used    5527
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      31.2
_cell_volume                     14363(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            94969
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.336
_diffrn_reflns_theta_min         6.558
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1732
_refine_ls_number_reflns         26005
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0739
_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^)+(0.1185P)^2^+18.8594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18452
_reflns_number_total             26005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04748j2.cif
_cod_data_source_block           40426FU
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 1542591--1542594.cif.
;
_cod_database_code               1542594
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              10761