Toward aceneporphyrinoids: synthesis and transformations of palladium(II) meso-anthriporphyrin
Bartosz Szyszko; Lechoslaw Latos-Grazynski; Ludmila Szterenberg; Chem.Commun. 48 (2012) 5004–; doi:10.1039/c2cc30362k

data_7107679
_publ_section_title
;
 Toward aceneporphyrinoids: synthesis and transformations of palladium(II)
 meso-anthriporphyrin
;
_journal_name_full               Chem.Commun.
_journal_page_first              5004
_journal_paper_doi               10.1039/c2cc30362k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C54 H36 N3, C2 F3 O2, 0.5(C2 H F3 O2)'
_chemical_formula_sum            'C57 H36.5 F4.5 N3 O3'
_chemical_formula_weight         896.0
_chemical_name_common            'meso-anthriporphyrin monocation'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.924(5)
_cell_length_b                   24.465(8)
_cell_length_c                   11.989(3)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.48
_cell_measurement_theta_min      2.54
_cell_volume                     4959(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur PX with Onyx CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41162
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.09
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1854
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The residual electron-density count was assessed as 110.4 electrons per unit cell, which is approximately consistent with nearly two molecules of trifluoroacetic acid per unit cell which yields 0.5 trifluoroacetic acid per formula unit.
;
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         11387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                6041
_reflns_number_total             11387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30362k.txt
_cod_data_source_block           monokation
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7107679