Synthesis, electronic structure and reactivity of bis(imino)pyridine iron carbene complexes: evidence for a carbene radical
Russell, Sarah K.; Hoyt, Jordan M.; Bart, Suzanne C.; Milsmann, Carsten; Stieber, S. Chantal E.; Semproni, Scott P.; DeBeer, Serena; Chirik, Paul J.; Chemical Science 5 (2014) 1168–; doi:10.1039/c3sc52450g

data_1513662
_publ_section_title
;
 Synthesis, electronic structure and reactivity of bis(imino)pyridine iron
 carbene complexes: evidence for a carbene radical
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              1168
_journal_paper_doi               10.1039/c3sc52450g
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C40 H41 Fe N3'
_chemical_formula_weight         619.61
_chemical_name_systematic
;
 ?
;
_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                 116.242(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.344(5)
_cell_length_b                   14.623(5)
_cell_length_c                   23.427(5)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.33
_cell_measurement_theta_min      4.86
_cell_volume                     6558(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37599
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         65.85
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    3.921
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.5557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         10900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+3.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                9746
_reflns_number_total             10900
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52450g.txt
_cod_data_source_block           jmh35
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1513662