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_4128762
_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            'C30 H40 Fe N2'
_chemical_formula_weight         484.49
_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
_audit_update_record
;
2018-07-01 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 96.802(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7415(3)
_cell_length_b                   30.1238(8)
_cell_length_c                   8.1904(2)
_cell_measurement_reflns_used    8409
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.51
_cell_measurement_theta_min      2.93
_cell_volume                     2631.55(12)
_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 0.871
_diffrn_measured_fraction_theta_max 0.982
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.871
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14255
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.536
_diffrn_reflns_theta_min         2.934
_exptl_absorpt_coefficient_mu    4.723
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5086
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.1418
_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^)+37.3446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2395
_refine_ls_wR_factor_ref         0.2583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2857
_reflns_number_total             4144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02443_si_001.cif
_cod_data_source_block           '[(Mes)DI]FeCOD'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128762
_shelxl_version_number           2014-3
_shelx_res_checksum              35120
_shelx_hkl_checksum              63231