Iterative Reductive Aromatization/Ring-Closing Metathesis Strategy toward the Synthesis of Strained Aromatic Belts.
Golder, Matthew R.; Colwell, Curtis E.; Wong, Bryan M.; Zakharov, Lev N.; Zhen, Jingxin; Jasti, Ramesh; Journal of the American Chemical Society 138 (2016) 6577–6582; doi:10.1021/jacs.6b02240

data_4130320
_publ_section_title
;
 Iterative Reductive Aromatization/Ring-Closing Metathesis Strategy toward
 the Synthesis of Strained Aromatic Belts.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6577
_journal_page_last               6582
_journal_paper_doi               10.1021/jacs.6b02240
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C60 H48 O2'
_chemical_formula_weight         800.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.381(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3012(7)
_cell_length_b                   9.9339(5)
_cell_length_c                   17.0395(6)
_cell_measurement_reflns_used    1805
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      60.32
_cell_measurement_theta_min      3.54
_cell_volume                     2110.53(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11828
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.642
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.1024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3416
_refine_ls_wR_factor_ref         0.4100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2234
_reflns_number_total             3706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b02240_si_002.cif
_cod_data_source_block           cu_jasti32_0m_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130320
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-4
_shelx_res_checksum              94809
_shelx_hkl_checksum              12272