Knölker-Type Iron Complexes Bearing an N-Heterocyclic Carbene Ligand: Synthesis, Characterization, and Catalytic Dehydration of Primary Amides
Elangovan, Saravanakumar; Quintero-Duque, Samuel; Dorcet, Vincent; Roisnel, Thierry; Norel, Lucie; Darcel, Christophe; Sortais, Jean-Baptiste; Organometallics 34 (2015) 4521–; doi:10.1021/acs.organomet.5b00553

data_4086285
_publ_section_title
;
 Kn\"olker-Type Iron Complexes Bearing an N-Heterocyclic Carbene Ligand:
 Synthesis, Characterization, and Catalytic Dehydration of Primary Amides
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4521
_journal_paper_doi               10.1021/acs.organomet.5b00553
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C37 H48 Fe N2 O3 Si2'
_chemical_formula_sum            'C37 H48 Fe N2 O3 Si2'
_chemical_formula_weight         680.8
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.012(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.356(3)
_cell_length_b                   15.454(4)
_cell_length_c                   11.602(3)
_cell_measurement_reflns_used    2111
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.71
_cell_measurement_theta_min      2.42
_cell_measurement_wavelength     0.71073
_cell_volume                     1822.6(9)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.1384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12747
_diffrn_reflns_theta_full        26.89
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6839
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1611
_reflns_number_gt                5118
_reflns_number_total             6839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00553_si_002.cif
_cod_data_source_block           SR145
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4086285