Reductive Coupling of Azides Mediated by an Iron(II) Bis(alkoxide) Complex
James A. Bellow; Philip D. Martin; Richard L. Lord; Stanislav Groysman; Inorganic Chemistry 52 (2013) 12335–12337; doi:10.1021/ic402517m

data_4336682
_publ_section_title
;
 Reductive Coupling of Azides Mediated by an Iron(II) Bis(alkoxide)
 Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12335
_journal_page_last               12337
_journal_paper_doi               10.1021/ic402517m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C45 H77 Fe N3 O2'
_chemical_formula_weight         747.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.360(2)
_cell_angle_beta                 93.147(2)
_cell_angle_gamma                115.750(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9324(6)
_cell_length_b                   12.9330(6)
_cell_length_c                   14.1689(7)
_cell_measurement_temperature    100(2)
_cell_volume                     2122.29(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65242
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.9254
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       prisms
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.086
_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     479
_refine_ls_number_reflns         9446
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0848P)^2^+2.6766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                7759
_reflns_number_total             9446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402517m_si_003_2.cif
_cod_data_source_block           sg108full
_cod_original_cell_volume        2122.29(17)
_cod_database_code               4336682