Facile Preparation of β-Haloporphyrins as Useful Precursors of β-Substituted Porphyrins.
Fujimoto, Keisuke; Yorimitsu, Hideki; Osuka, Atsuhiro; Organic letters 16 (2014) 972–975; doi:10.1021/ol4037049

data_1513467
_publ_section_title
;
 Facile Preparation of \b-Haloporphyrins as Useful Precursors of
 \b-Substituted Porphyrins.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              972
_journal_page_last               975
_journal_paper_doi               10.1021/ol4037049
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C64 H70 N6 Zn'
_chemical_formula_sum            'C69 H79 Cl3 N7 O Zn'
_chemical_formula_weight         1194.11
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                111.7558(8)
_cell_angle_beta                 102.8420(8)
_cell_angle_gamma                97.3951(11)
_cell_formula_units_Z            2
_cell_length_a                   9.4123(2)
_cell_length_b                   18.6641(3)
_cell_length_c                   20.8623(4)
_cell_measurement_reflns_used    26718
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.27
_cell_measurement_theta_min      4.21
_cell_volume                     3227.30(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II'
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33685
_diffrn_reflns_theta_full        64.00
_diffrn_reflns_theta_max         64.00
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    2.031
_exptl_absorpt_correction_T_max  0.9052
_exptl_absorpt_correction_T_min  0.4299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Higashi, T. (1995). Program for 
 Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         10471
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2106
_reflns_number_gt                7241
_reflns_number_total             10471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4037049_si_004.cif
_cod_data_source_block           fk0425
_cod_database_code               1513467