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_4128764
_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            'C34.5 H42 Fe N4'
_chemical_formula_weight         568.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.969(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2244(9)
_cell_length_b                   23.3339(12)
_cell_length_c                   14.9504(7)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.39
_cell_volume                     5950.7(5)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.769
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       plate
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0983
_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^)+(0.0001P)^2^+98.5894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5248
_reflns_number_total             7727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02443_si_001.cif
_cod_data_source_block           '[(Mes)PI]2Fe'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C34.50 H42 Fe N4'
_cod_database_code               4128764
_shelxl_version_number           2014-3
_shelx_res_checksum              63578
_shelx_hkl_checksum              44464