Aromatic Expanded Isophlorins: Stable 30π Annulene Analogues with Diverse Structural Features
J. Sreedhar Reddy; Venkataramanarao G. Anand; Journal of the American Chemical Society 131 (2009) 15433–15439; doi:10.1021/ja906290d

data_4105192
_publ_contact_author_address
;
Department of Chemistry 
Indian Institute of Science Education and Research 
900 NCL Innovation Park
Dr.Homi Bhabha Road
Pune 411 008
India.
;
_publ_contact_author_email       vg.anand@iiserpune.ac.in
_publ_contact_author_fax         '091 20 25898022'
_publ_contact_author_name        'Venkataramanarao G. Anand'
_publ_contact_author_phone       '091 20 25898021'
_publ_section_title
;
 Aromatic Expanded Isophlorins: Stable 30\p Annulene Analogues with
 Diverse Structural Features
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15433
_journal_page_last               15439
_journal_paper_doi               10.1021/ja906290d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C66 H12 F30 S3 Se3, 4(C H Cl3)'
_chemical_formula_sum            'C70 H16 Cl12 F30 S3 Se3'
_chemical_formula_weight         2185.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_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                101.927(2)
_cell_angle_beta                 92.695(2)
_cell_angle_gamma                94.785(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7036(4)
_cell_length_b                   12.8407(5)
_cell_length_c                   15.7989(6)
_cell_measurement_reflns_used    6478
_cell_measurement_temperature    248(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.5
_cell_volume                     1915.18(13)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP 32 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare etal., 1993)'
_diffrn_ambient_temperature      248(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker axs (Kappa apex2)'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47503
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_T_max  0.8206
_exptl_absorpt_correction_T_min  0.5772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_description       needle
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.548(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         19873
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0628P)^2^+2.2254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                12001
_reflns_number_total             19873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906290d_si_007.cif
_cod_data_source_block           s3se3a
_cod_original_cell_volume        1915.17(13)
_cod_database_code               4105192