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_4128763
_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            'C38 H48 Fe N4'
_chemical_formula_weight         616.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                88.863(2)
_cell_angle_beta                 80.655(2)
_cell_angle_gamma                77.495(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6392(6)
_cell_length_b                   9.8763(6)
_cell_length_c                   18.4278(12)
_cell_measurement_reflns_used    9166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.79
_cell_measurement_theta_min      2.70
_cell_volume                     1689.76(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.1378
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77737
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.816
_diffrn_reflns_theta_min         2.240
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       rod
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0947
_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^)+7.3417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5827
_reflns_number_total             8794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02443_si_001.cif
_cod_data_source_block           '[(iPr)PI]2Fe'
_cod_depositor_comments
;

2020-10-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C19 H24 Fe0.50 N2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     308.33
_cod_database_code               4128763
_shelxl_version_number           2014-3
_shelx_res_checksum              29887
_shelx_hkl_checksum              61882