Regio- and Diastereoselective Iron-Catalyzed [4+4]-Cycloaddition of 1,3-Dienes.
Kennedy, C. Rose; Zhong, Hongyu; Macaulay, Rachel L.; Chirik, Paul J.; Journal of the American Chemical Society 141 (2019) 8557–8573; doi:10.1021/jacs.9b02443

data_4128766
_publ_section_title
;
 Regio- and Diastereoselective Iron-Catalyzed [4+4]-Cycloaddition of
 1,3-Dienes.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8557
_journal_page_last               8573
_journal_paper_doi               10.1021/jacs.9b02443
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C27 H42 Fe N2 O Si2'
_chemical_formula_weight         522.65
_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-2014
_cell_angle_alpha                90
_cell_angle_beta                 117.879(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2160(8)
_cell_length_b                   11.9385(6)
_cell_length_c                   16.7276(9)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.76
_cell_volume                     2862.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'I\mS microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            142565
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.774
_diffrn_reflns_theta_min         2.193
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+6.8921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5928
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02443_si_001.cif
_cod_data_source_block           (iPrPI)Fe(MviMvi)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128766
_shelxl_version_number           2014-3
_shelx_res_checksum              77238
_shelx_hkl_checksum              64865