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_7158245
_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_formula_moiety         'C34 H28 I2 O4'
_chemical_formula_sum            'C34 H28 I2 O4'
_chemical_formula_weight         754.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90.0000
_cell_angle_beta                 103.830(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.4916(3)
_cell_length_b                   14.1803(3)
_cell_length_c                   18.3463(5)
_cell_measurement_reflns_used    31495
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.36
_cell_measurement_theta_min      3.12
_cell_volume                     3155.55(16)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1702
_diffrn_reflns_av_unetI/netI     0.1029
_diffrn_reflns_Laue_measured_fraction_full 0.987
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_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34209
_diffrn_reflns_point_group_measured_fraction_full 0.987
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_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.888
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.930
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1480.00
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.35
_refine_diff_density_min         -1.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         5690
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0978P)^2^+5.3489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4413
_reflns_number_total             5690
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1ob01270c2.cif
_cod_data_source_block           yasuda20200115
_cod_depositor_comments
'Adding full bibliography for 7158245--7158249.cif.'
_cod_original_cell_volume        3155.55(17)
_cod_database_code               7158245
_shelx_res_checksum              45344
_shelx_hkl_checksum              48598
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