Synthesis, Electronic Structure, and Catalytic Activity of Reduced Bis(aldimino)pyridine Iron Compounds: Experimental Evidence for Ligand Participation
Sarah K. Russell; Carsten Milsmann; Emil Lobkovsky; Thomas Weyhermüller; Paul J. Chirik; Inorganic Chemistry 50 (2011) 3159–3169; doi:10.1021/ic102186q

data_4324763
_publ_section_title
;
 Synthesis, Electronic Structure, and Catalytic Activity of Reduced
 Bis(aldimino)pyridine Iron Compounds: Experimental Evidence for Ligand
 Participation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3159
_journal_page_last               3169
_journal_paper_doi               10.1021/ic102186q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C35 H45 Fe N3, 0.5(C6 H14)'
_chemical_formula_sum            'C38 H52 Fe N3'
_chemical_formula_weight         606.68
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.958(2)
_cell_angle_beta                 104.666(2)
_cell_angle_gamma                109.051(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0851(4)
_cell_length_b                   12.1329(6)
_cell_length_c                   16.6443(7)
_cell_measurement_reflns_used    7776
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.40
_cell_volume                     1648.76(13)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23513
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.9529
_exptl_absorpt_correction_T_min  0.8289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       needle
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7429
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.109
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.5835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                5856
_reflns_number_total             7429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102186q_si_001_4.cif
_cod_data_source_block           sr13
_cod_database_code               4324763