Novel Core-Modified Expanded Porphyrins with meso-Aryl Substituents: Synthesis, Spectral and Structural Characterization
Seenichamy Jeyaprakash Narayanan; Bashyam Sridevi; Tavarekere K. Chandrashekar; Ashwani Vij; Raja Roy; Journal of the American Chemical Society 121 (1999) 9053–9068; doi:10.1021/ja991472k

data_4116552
_publ_section_title
;
 Novel Core-Modified Expanded Porphyrins with meso-Aryl Substituents:
 Synthesis, Spectral and Structural Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9053
_journal_page_last               9068
_journal_paper_doi               10.1021/ja991472k
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C58 H36 F15 N3 O10 S2'
_chemical_formula_weight         1284.02
_chemical_name_common            S2N3-TFA
_chemical_name_systematic
;
    

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;
_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                104.4030(10)
_cell_angle_beta                 109.2780(10)
_cell_angle_gamma                107.0930(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7165(3)
_cell_length_b                   14.8857(2)
_cell_length_c                   16.5289(4)
_cell_measurement_temperature    298(2)
_cell_volume                     2812.42(11)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'Siemens CCD '
_diffrn_measurement_method       '\w oscillation, 0.3 deg'
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9469
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 'beginning & end'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.207
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0110(13)
_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   1.197
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         5680
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0732P)^2^+4.6115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                4579
_reflns_number_total             5680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991472k_1.cif
_cod_data_source_block           JA991472K-123
_cod_original_cell_volume        2812.42(10)
_cod_database_code               4116552