Tetraphenyl-p-benziporphyrin: A Carbaporphyrinoid with Two Linked Carbon Atoms in the Coordination Core
Marcin Stępień; Lechosław Latos-Grażyński; Journal of the American Chemical Society 124 (2002) 3838–3839; doi:10.1021/ja017852z

data_4114736
_publ_contact_author             'Marcin Stepien'
_publ_contact_author_email       ms@wchuwr.chem.uni.wroc.pl
_publ_section_title
;
 Tetraphenyl-p-benziporphyrin: A Carbaporphyrinoid with Two Linked Carbon
 Atoms in the Coordination Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3838
_journal_page_last               3839
_journal_paper_doi               10.1021/ja017852z
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C47.8 H36.6 Cl5.9 N3 O0.9'
_chemical_formula_weight         877.11
_chemical_name_systematic
; 
 5,10,15,20-tetraphenyl-para-benziporphyrin dication dichloride
 dichloromethane disolvate monohydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6690(10)
_cell_length_b                   15.6020(10)
_cell_length_c                   14.5830(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4247.6(5)
_computing_cell_refinement
'KM4CCD Software (Kuma Diffraction (1995--2001)'
_computing_data_collection
'KM4CCD Software (Kuma Diffraction (1995--2001)'
_computing_data_reduction
'KM4CCD Software (Kuma Diffraction (1995--2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'KUMA KM4CCD \k-geometry diffractometer'
_diffrn_measurement_method       2\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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27522
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'XPREP Ver. 5.1/NT (Bruker Analytical X-ray Systems, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1777
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+4.8559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                4523
_reflns_number_total             5271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017852z_2.cif
_cod_data_source_block           pbendc
_cod_original_formula_sum        'C47.8 H36.6 Cl5.9 N3.0 O0.90'
_cod_database_code               4114736