Synthesis of Bis(imino)pyridine Iron Amide and Ammonia Compounds from an N-H Transfer Agent
Amanda C. Bowman; Suzanne C. Bart; Frank W. Heinemann; Karsten Meyer; Paul J. Chirik; Inorganic Chemistry 48 (2009) 5587–5589; doi:10.1021/ic9003017

data_4302476
_publ_section_title
;
Synthesis of Bis(imino)pyridine Iron Amide and Ammonia Compounds from an
N-H Transfer Agent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5587
_journal_page_last               5589
_journal_paper_doi               10.1021/ic9003017
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C47 H53 Fe N4, 1.5(C7 H8)'
_chemical_formula_sum            'C57.5 H65 Fe N4'
_chemical_formula_weight         867.98
_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                71.594(9)
_cell_angle_beta                 76.764(10)
_cell_angle_gamma                78.316(8)
_cell_formula_units_Z            2
_cell_length_a                   11.4441(9)
_cell_length_b                   13.5081(18)
_cell_length_c                   16.9763(16)
_cell_measurement_reflns_used    255
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     2399.7(5)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 2.00 \% and 150 sec per frame
;
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60107
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         10567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0447P)^2^+2.5130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                8169
_reflns_number_total             10567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003017_si_002_1.cif
_cod_data_source_block           sd0712
_cod_original_sg_symbol_Hall     -P1
_cod_original_formula_sum        'C57.50 H65 Fe N4'
_cod_database_code               4302476