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_7107680
_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 H35 N3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C54.5 H36 Cl N3'
_chemical_formula_weight         767.45
_chemical_name_common            5,10,15,20-tetraphenyl-meso-anthriporphyrin
_chemical_name_systematic        5,10,15,20-tetraphenyl-meso-anthriporphyrin
_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                92.09(3)
_cell_angle_beta                 101.98(4)
_cell_angle_gamma                106.41(4)
_cell_formula_units_Z            2
_cell_length_a                   9.779(3)
_cell_length_b                   13.499(6)
_cell_length_c                   16.963(6)
_cell_measurement_reflns_used    8295
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.9002
_cell_measurement_theta_min      2.7878
_cell_volume                     2090.4(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.828
_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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.1989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40404
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.92
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The residual electron-density count was assessed as 41.4 electrons per unit cell, which is approximately consistent with nearly one molecule of dichloromethane per unit cell which yields 0.5 dichloromethane per formula unit.
;
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         17492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.774
_refine_ls_R_factor_all          0.1838
_refine_ls_R_factor_gt           0.0764
_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^)+(0.0953P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                6447
_reflns_number_total             17492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30362k.txt
_cod_data_source_block           bs10
_cod_original_formula_sum        'C54.5 H36 Cl1 N3'
_cod_database_code               7107680