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_4134328
_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_moiety         '2(C45 H61 Fe N3), C5 H12'
_chemical_formula_sum            'C95 H134 Fe2 N6'
_chemical_formula_weight         1471.78
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.604(5)
_cell_length_b                   21.604(5)
_cell_length_c                   8.778(2)
_cell_measurement_reflns_used    7203
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.66
_cell_volume                     4097.0(16)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 2008)'
_computing_data_collection       'BRUKER APEX II software suite (Bruker AXS)'
_computing_data_reduction        'BRUKER APEX II software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP 3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Farrugia, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23299
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sababs 2008/2'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.393(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4800
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+2.8122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                4158
_reflns_number_total             4800
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja0c00250_si_002.cif
_cod_data_source_block           jmh19
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      P-42(1)m
_cod_database_code               4134328