A new synthetic approach to benzoporphyrins and Krohnke type porphyrin-2-ylpyridines
Nuno M. M. Moura; Maria A. F. Faustino; Maria G. P. M. S. Neves; Filipe A. Almeida Paz; Artur M. S. Silva; Augusto C. Tome; Jose A. S. Cavaleiro; Chem.Commun. 48 (2012) 6142–; doi:10.1039/c2cc30727h

data_7107842
_publ_section_title
;
 A new synthetic approach to benzoporphyrins and Krohnke type
 porphyrin-2-ylpyridines
;
_journal_name_full               Chem.Commun.
_journal_page_first              6142
_journal_paper_doi               10.1039/c2cc30727h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C59 H39 N7'
_chemical_formula_sum            'C59 H39 N7'
_chemical_formula_weight         845.97
_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_date             '22 December 2011'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                76.355(8)
_cell_angle_beta                 78.393(8)
_cell_angle_gamma                71.138(7)
_cell_formula_units_Z            2
_cell_length_a                   10.6667(14)
_cell_length_b                   13.6339(17)
_cell_length_c                   18.488(3)
_cell_measurement_reflns_used    1440
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.30
_cell_measurement_theta_min      2.73
_cell_volume                     2449.6(6)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1369
_diffrn_reflns_av_sigmaI/netI    0.2630
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30441
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_correction_T_min  0.9939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0054(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.2447
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1162P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2542
_reflns_number_gt                2983
_reflns_number_total             8820
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc30727h.txt
_cod_data_source_block           3e
_cod_database_code               7107842