Synthesis and Structural Analysis of a Highly Curved Buckybowl Containing Corannulene and Sumanene Fragments
Tsun-Cheng Wu; Hsin-Ju Hsin; Ming-Yu Kuo; Ching-Hsiu Li; Yao-Ting Wu; Journal of the American Chemical Society 133 (2011) 16319–16321; doi:10.1021/ja2067725

data_4106961
_publ_section_title
;
 Synthesis and Structural Analysis of a Highly Curved Buckybowl Containing
 Corannulene and Sumanene Fragments
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16319
_journal_page_last               16321
_journal_paper_doi               10.1021/ja2067725
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C32 H12'
_chemical_formula_weight         396.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7727(8)
_cell_length_b                   12.6382(6)
_cell_length_c                   8.1349(4)
_cell_measurement_reflns_used    2114
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0830
_cell_measurement_theta_min      3.2238
_cell_volume                     1827.22(15)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6614
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       Lump
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.099
_refine_diff_density_rms         0.024
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1489
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0379P)^2^+0.4683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                1284
_reflns_number_total             1489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2067725_si_002.cif
_cod_data_source_block           110565
_cod_depositor_comments
;

2020-12-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H24'
_cod_original_formula_weight         792.83
_cod_original_formula_units_Z            2
_cod_database_code               4106961