Unexpected formation of poly-functionalized fulvenes by the reaction of a tetraaryl[5]cumulene with iodine.
Hoshi, Keita; Yasuda, Masashi; Nakamura, Takumi; Yoshida, Yasushi; Ueta, Shoko; Minagawa, Keiji; Kawamura, Yasuhiko; Imada, Yasushi; Yagishita, Fumitoshi; Organic & biomolecular chemistry 19 (2021) 7594–7597; doi:10.1039/d1ob01270c

data_7158249
_publ_section_title
;
 Unexpected formation of poly-functionalized fulvenes by the reaction of a
 tetraaryl[5]cumulene with iodine.
;
_journal_issue                   35
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7594
_journal_page_last               7597
_journal_paper_doi               10.1039/d1ob01270c
_journal_volume                  19
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_sum            'C34 H28 O4'
_chemical_formula_weight         500.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-06-10 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.913(4)
_cell_length_b                   7.442(3)
_cell_length_c                   16.072(5)
_cell_measurement_reflns_used    384
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.3131
_cell_measurement_theta_min      4.1358
_cell_volume                     1278.5(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEXII Ultra CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1406
_diffrn_reflns_av_unetI/netI     0.2838
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5392
_diffrn_reflns_theta_full        66.605
_diffrn_reflns_theta_max         66.605
_diffrn_reflns_theta_min         2.807
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.509
_refine_ls_abs_structure_details
;
Flack x determined using 194 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3532
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.2178
_refine_ls_R_factor_gt           0.1184
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1.1678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2748
_refine_ls_wR_factor_ref         0.3523
_reflns_number_gt                1420
_reflns_number_total             3532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob01270c2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7158245--7158249.cif.'
_cod_database_code               7158249
_cod_duplicate_entry 7158247