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_4116553
_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            'C66 H44 N6 S2'
_chemical_formula_weight         985.19
_chemical_name_common            'S2N4 Rubyrin'
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 105.8160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.0002(6)
_cell_length_b                   15.0991(4)
_cell_length_c                   11.9801(3)
_cell_measurement_temperature    213(2)
_cell_volume                     5047.2(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_method       '\w scans'
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10690
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'greenish bl'
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       Block
_exptl_crystal_F_000             2056
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00051(17)
_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   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                2793
_reflns_number_total             3601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991472k_2.cif
_cod_data_source_block           JA991472K-123
_cod_database_code               4116553