Unprecedented formation of eta^46-(vinylketene)iron complexes from eta^4^-(diene)iron complexes and aromatic compounds in the presence of a Lewis acid
Tatsuo Okauchi; Naoki Sata; Akihiro Urakawa; Mitsuru Kitamura; Chem.Commun. 51 (2015) 8454–; doi:10.1039/C5cc00870K

data_7117142
_publ_section_title
;
 Unprecedented formation of eta^46-(vinylketene)iron complexes from
 eta^4^-(diene)iron complexes and aromatic compounds in the presence of a
 Lewis acid
;
_journal_name_full               Chem.Commun.
_journal_page_first              8454
_journal_paper_doi               10.1039/C5cc00870K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C23 H20 Fe O4'
_chemical_formula_weight         416.24
_chemical_properties_physical    Photo-sensitive
_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'
_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           'APEX2 v2009.11-0'
_audit_update_record
;
2015-01-15 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.68790(10)
_cell_length_b                   6.41630(10)
_cell_length_c                   34.7054(5)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    90.(2)
_cell_measurement_theta_max      35.8087
_cell_measurement_theta_min      2.4722
_cell_volume                     1927.91(5)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'Bruker Instrument Service v2009, 11, 1, 0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            29949
_diffrn_reflns_theta_full        36.46
_diffrn_reflns_theta_max         36.46
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'translucent pale yellow'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane, Ethyl acetate'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.909
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.394
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         8888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.394
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                7052
_reflns_number_total             8888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00870k2.cif
_cod_data_source_block           I
_cod_database_code               7117142