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_4128765
_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            'C42 H52 Fe N4'
_chemical_formula_weight         668.73
_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
;
2017-08-13 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 115.941(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2598(4)
_cell_length_b                   20.1582(7)
_cell_length_c                   14.9573(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.86
_cell_measurement_theta_min      3.95
_cell_volume                     3595.2(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.992
_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  0.1576
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47387
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.990
_diffrn_reflns_theta_min         3.707
_exptl_absorpt_coefficient_mu    3.616
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.3688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.122
_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     425
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.1114
_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^)+49.9580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2260
_refine_ls_wR_factor_ref         0.2487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4313
_reflns_number_total             6343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02443_si_001.cif
_cod_data_source_block           (MesPI)2Fe(isoprene)
_cod_depositor_comments
;

2020-10-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C28 H34.67 Fe0.67 N2.67'
_cod_original_formula_units_Z    6
_cod_original_formula_weight     445.82
_cod_database_code               4128765
_shelxl_version_number           2014-3
_shelx_res_checksum              35782
_shelx_hkl_checksum              86674