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_7107678
_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 H34 Cl N3 Pd, 0.4(C6 H14), 0.1(H2 O), 1.15(C H2 Cl2)'
_chemical_formula_sum            'C57.55 H42.1 Cl3.3 N3 O0.1 Pd'
_chemical_formula_weight         1000.63
_chemical_name_common            'chloropalladium meso-anthriporphyrin'
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   50.222(15)
_cell_length_b                   50.222(15)
_cell_length_c                   9.718(3)
_cell_measurement_reflns_used    18056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.5506
_cell_measurement_theta_min      4.1050
_cell_volume                     21227(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            58940
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.22
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             9203
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         13715
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                8722
_reflns_number_total             13715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30362k.txt
_cod_data_source_block           bs2abs
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C57.55 H42.10 Cl3.30 N3 O0.10 Pd'
_cod_database_code               7107678