Investigations into the Mechanism of Inter- and Intramolecular Iron-Catalyzed [2+2] Cycloaddition of Alkenes.
Joannou, Matthew V.; Hoyt, Jordan M.; Chirik, Paul J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00250

data_4134329
_publ_section_title
;
 Investigations into the Mechanism of Inter- and Intramolecular
 Iron-Catalyzed [2+2] Cycloaddition of Alkenes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00250
_journal_year                    2020
_chemical_formula_sum            'C49 H64.5 Fe N3'
_chemical_formula_weight         751.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 103.465(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8735(8)
_cell_length_b                   13.1302(9)
_cell_length_c                   24.7514(16)
_cell_measurement_reflns_used    9310
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.03
_cell_measurement_theta_min      2.53
_cell_volume                     4068.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            68075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.075
_diffrn_reflns_theta_min         2.248
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v 2014.2 (BRUKER ASX)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       shard
_exptl_crystal_F_000             1622
_exptl_crystal_size_max          0.894
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         17776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.6873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13208
_reflns_number_total             17776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00250_si_002.cif
_cod_data_source_block           jmh49
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C49 H64.50 Fe N3'
_cod_database_code               4134329
_shelxl_version_number           2014-3
_shelx_res_checksum              35452
_shelx_hkl_checksum              9379