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_4324760
_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         'C31 H39 N3, 0.5(C5 H12)'
_chemical_formula_sum            'C33.5 H45 N3'
_chemical_formula_weight         489.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 91.744(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.4772(12)
_cell_length_b                   29.510(4)
_cell_length_c                   24.084(3)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.600
_cell_measurement_theta_min      2.237
_cell_volume                     6022.1(14)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            95705
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.9981
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS 2008/1, Bruker AXS (2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         10934
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0495P)^2^+2.9538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                8653
_reflns_number_total             10934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102186q_si_001_1.cif
_cod_data_source_block           6996
_cod_original_formula_sum        'C33.50 H45 N3'
_cod_database_code               4324760