Iron-Catalyzed [2π + 2π] Cycloaddition of α,ω-Dienes: The Importance of Redox-Active Supporting Ligands
Bouwkamp, Marco W.; Bowman, Amanda C.; Lobkovsky, Emil; Chirik, Paul J.; Journal of the American Chemical Society 128 (2006) 13340–13341; doi:10.1021/ja064711u

data_4110969
_publ_section_title
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 Iron-Catalyzed [2\p + 2\p] Cycloaddition of \a,\w-Dienes:
 The Importance of Redox-Active Supporting Ligands
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_journal_coden_ASTM              JACSAT
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13340
_journal_page_last               13341
_journal_paper_doi               10.1021/ja064711u
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C37 H49 Fe N3'
_chemical_formula_sum            'C37 H49 Fe N3'
_chemical_formula_weight         591.64
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 106.317(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9396(8)
_cell_length_b                   16.2602(10)
_cell_length_c                   13.6584(7)
_cell_measurement_reflns_used    7280
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.50
_cell_measurement_theta_min      2.51
_cell_volume                     3184.3(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
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_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59580
_diffrn_reflns_theta_full        37.57
_diffrn_reflns_theta_max         37.57
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.7870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.063
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         14401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.4630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                11360
_reflns_number_total             14401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064711usi20060703_113821.cif
_cod_data_source_block           mwb7
_cod_depositor_comments
;
 Updated bibliographical information.

 Antanas Vaitkus,
 2019-09-17
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_cod_database_code               4110969