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_4105190
_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_sum            'C66.5 H14 Cl F30 O4.5 S2'
_chemical_formula_weight         1554.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.115(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2195(8)
_cell_length_b                   33.928(2)
_cell_length_c                   16.4312(11)
_cell_measurement_reflns_used    4552
_cell_measurement_temperature    248(2)
_cell_measurement_theta_max      19.0
_cell_measurement_theta_min      2.5
_cell_volume                     5977.6(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1007
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29593
_diffrn_reflns_theta_full        19.18
_diffrn_reflns_theta_max         19.18
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.9121
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       needle
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00017(4)
_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   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         4920
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0973
_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^)+(0.1589P)^2^+40.4455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2476
_refine_ls_wR_factor_ref         0.2821
_reflns_number_gt                3307
_reflns_number_total             4920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906290d_si_005.cif
_cod_data_source_block           s2o4
_cod_original_formula_sum        'C66.50 H14 Cl F30 O4.50 S2'
_cod_database_code               4105190