Regioselective Amination of Carbaporpholactone and N-Confused Porphyrin
Norbert Grzegorzek; Miłosz Pawlicki; Lechosław Latos-Grażyński; Journal of Organic Chemistry 74 (2009) 8547–8553; doi:10.1021/jo901508v

data_4025023
_publ_section_title
;
Regioselective Amination of Carbaporpholactone and N-Confused Porphyrin
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8547
_journal_page_last               8553
_journal_paper_doi               10.1021/jo901508v
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C56 H55 N5'
_chemical_formula_weight         798.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                75.86(3)
_cell_angle_beta                 79.25(3)
_cell_angle_gamma                75.07(3)
_cell_formula_units_Z            2
_cell_length_a                   9.964(2)
_cell_length_b                   14.502(3)
_cell_length_c                   16.876(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2264.9(8)
_computing_cell_refinement
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction, 1995-2003)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_molecular_graphics    'XP (Bruker, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type
'Oxford Diffraction KM4 Xcalibur PX \k-geometry diffractometer'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23601
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         76.54
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         8677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                4513
_reflns_number_total             8677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901508v_si_001.cif
_cod_data_source_block           NGMPLLG
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4025023