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_1513465
_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         'C87 H89.48 N6 O Zn, C3.5, C H4 O'
_chemical_formula_sum            'C91.5 H93.48 N6 O2 Zn'
_chemical_formula_weight         1374.57
_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                98.501(2)
_cell_angle_beta                 92.026(2)
_cell_angle_gamma                92.976(3)
_cell_formula_units_Z            2
_cell_length_a                   14.6574(7)
_cell_length_b                   15.6368(7)
_cell_length_c                   17.2398(7)
_cell_measurement_reflns_used    18515
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.16
_cell_measurement_theta_min      3.02
_cell_volume                     3898.9(3)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1218
_diffrn_reflns_av_sigmaI/netI    0.1440
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47792
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.8512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Higashi, T. (1995). Program for 
 Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1461
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.443
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         11301
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1765
_refine_ls_R_factor_gt           0.1000
_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^)+(0.1507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.3082
_reflns_number_gt                5404
_reflns_number_total             11301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4037049_si_003.cif
_cod_data_source_block           0930fk
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C91.50 H93.48 N6 O2 Zn'
_cod_database_code               1513465