34π Octaphyrin: First Structural Characterization of a Planar, Aromatic [1.0.1.0.1.0.1.0] Octaphyrin with Inverted Heterocyclic Rings
Venkataramanarao G. Anand; Simi K. Pushpan; Sundararaman Venkatraman; Abhishek Dey; Tavarekere K. Chandrashekar; Bhavani S. Joshi; Raja Roy; Weijie Teng; Karin Ruhlandt Senge; Journal of the American Chemical Society 123 (2001) 8620–8621; doi:10.1021/ja011265w

data_4115677
_publ_section_title
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 34\p Octaphyrin: First Structural Characterization of a Planar, Aromatic
 [1.0.1.0.1.0.1.0] Octaphyrin with Inverted Heterocyclic Rings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8620
_journal_page_last               8621
_journal_paper_doi               10.1021/ja011265w
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C74 H66.5 Cl N4 S4'
_chemical_formula_weight         1175.50
_chemical_name_systematic
;
 ?
;
_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                100.0340(10)
_cell_angle_beta                 100.7120(10)
_cell_angle_gamma                107.4260(10)
_cell_formula_units_Z            4
_cell_length_a                   15.3559(4)
_cell_length_b                   21.8104(6)
_cell_length_c                   23.3825(6)
_cell_measurement_temperature    90(2)
_cell_volume                     7117.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36771
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.91
_diffrn_standards_decay_%        no
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9013
_exptl_absorpt_correction_T_min  0.8519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'R. Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       block
_exptl_crystal_F_000             2478
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1492
_refine_ls_number_reflns         23793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1046P)^2^+2.8502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                16661
_reflns_number_total             23793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011265w.cif
_cod_data_source_block           sadp1
_cod_original_formula_sum        'C74 H66.50 Cl N4 S4'
_cod_database_code               4115677