Mechanism of Catalytic Nitrene Transfer Using Iron(I)‒Isocyanide Complexes
Cowley, Ryan E.; Golder, Matthew R.; Eckert, Nathan A.; Al-Afyouni, Malik H.; Holland, Patrick L.; Organometallics 32 (2013) 5289–; doi:10.1021/om400379p

data_4089536
_publ_section_title
;
 Mechanism of Catalytic Nitrene Transfer Using Iron(I)--Isocyanide
 Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5289
_journal_paper_doi               10.1021/om400379p
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C48 H75 Fe N4'
_chemical_formula_sum            'C48 H75 Fe N4'
_chemical_formula_weight         763.97
_chemical_name_common            HOLRC10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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                 97.234(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.549(5)
_cell_length_b                   34.799(15)
_cell_length_c                   12.236(5)
_cell_measurement_reflns_used    4080
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.40
_cell_volume                     4456(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1494
_diffrn_reflns_av_sigmaI/netI    0.1069
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52756
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.417
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         9108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1050P)^2^+5.1324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.2190
_reflns_number_gt                5468
_reflns_number_total             9108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400379p_si_002.cif
_cod_data_source_block           holrc10
_cod_database_code               4089536