Generation of a High-Valent Iron Imido Corrolazine Complex and NR Group Transfer Reactivity
Pannee Leeladee; Guy N. L. Jameson; Maxime A. Siegler; Devesh Kumar; Sam P. de Visser; David P. Goldberg; Inorganic Chemistry 52 (2013) 4668–4682; doi:10.1021/ic400280x

data_4334526
_publ_contact_author_address
;Johns Hopkins University
Department of Chemistry
3400 N. Charles Street
Baltimore, MD 21218
USA
;
_publ_contact_author_email       dpg@jhu.edu
_publ_contact_author_name        'David P. Goldberg'
_publ_contact_author_phone       '(410) 516-6658'
_publ_section_title
;
 Generation of a High-Valent Iron Imido Corrolazine Complex and NR Group
 Transfer Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4668
_journal_page_last               4682
_journal_paper_doi               10.1021/ic400280x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C114 H119 Fe N8 P, 4(C H2 Cl2), C2 H3 N'
_chemical_formula_sum            'C120 H130 Cl8 Fe N9 P'
_chemical_formula_weight         2068.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.6307(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2124(2)
_cell_length_b                   33.4786(5)
_cell_length_c                   19.9855(2)
_cell_measurement_reflns_used    27289
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      1.60
_cell_volume                     11237.9(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65453
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             4360
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         19786
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1186P)^2^+5.0794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2026
_reflns_number_gt                13559
_reflns_number_total             19786
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic400280x_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334526