Synthesis of Aziridines from Alkenes and Aryl Azides with a Reusable Macrocyclic Tetracarbene Iron Catalyst
S. Alan Cramer; David M. Jenkins; Journal of the American Chemical Society 133 (2011) 19342–19345; doi:10.1021/ja2090965

data_4107186
_publ_section_title
;
 Synthesis of Aziridines from Alkenes and Aryl Azides with a Reusable
 Macrocyclic Tetracarbene Iron Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19342
_journal_page_last               19345
_journal_paper_doi               10.1021/ja2090965
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C78 H58 F12 Fe N11 O1.5 P2'
_chemical_formula_weight         1519.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.337(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.400(2)
_cell_length_b                   16.8402(18)
_cell_length_c                   21.336(2)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.49
_cell_volume                     7323.7(13)
_computing_molecular_graphics    'Diamond 3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            91579
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.208
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         17519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+10.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                13640
_reflns_number_total             17519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2090965_si_001.cif
_cod_data_source_block           dmj4a
_cod_original_cell_volume        7323.4(13)
_cod_original_formula_sum        'C78 H58 F12 Fe N11 O1.50 P2'
_cod_database_code               4107186