Ferrocenyl-Imidazolylidene Ligand for Redox-Switchable Gold-Based Catalysis. A Detailed Study on the Redox-Switching Abilities of the Ligand
Ibáñez, Susana; Poyatos, Macarena; Dawe, Louise N.; Gusev, Dmitry; Peris, Eduardo; Organometallics 35 (2016) 2747–; doi:10.1021/acs.organomet.6b00517

data_4086628
_publ_section_title
;
 Ferrocenyl-Imidazolylidene Ligand for Redox-Switchable Gold-Based
 Catalysis. A Detailed Study on the Redox-Switching Abilities of the
 Ligand
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2747
_journal_paper_doi               10.1021/acs.organomet.6b00517
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C36 H43 Fe I Ir N4, B F4'
_chemical_formula_sum            'C36 H43 B F4 Fe I Ir N4'
_chemical_formula_weight         993.50
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.285(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7844(7)
_cell_length_b                   10.9697(3)
_cell_length_c                   18.5044(6)
_cell_measurement_reflns_used    11664
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      27.6300
_cell_measurement_theta_min      3.7620
_cell_volume                     3695.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

--------------------------------------------------------------------------
  1  \w    -85.00 -37.40   0.70   40.00    --  -11.13 151.00 154.26   68
  2  \w    -20.00  29.70   0.70   40.00    --  -11.13 -99.00 -90.00   71
  3  \w    -69.00  57.70   0.70   40.00    --   12.06 -19.00-180.00  181
  4  \w    -77.00  99.40   0.70   40.00    --   12.06   0.00 120.00  252
  5  \w    -45.00  -6.50   0.70   40.00    --  -11.13  77.00   0.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.410
_diffrn_reflns_theta_min         2.908
_exptl_absorpt_coefficient_mu    4.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.492
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9203
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+18.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6452
_reflns_number_total             9203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00517_si_005.cif
_cod_data_source_block           str1837
_cod_depositor_comments
'Adding full bibliography for 4086627--4086629.cif.'
_cod_database_code               4086628
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C8 = C8-C9
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C8 \\sim C9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C9: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
5.a Ternary CH refined with riding coordinates:
 C33(H33), C19(H19), C22(H22), C21(H21), C27(H27), C20(H20), C24(H24),
 C26(H26), C23(H23), C32(H32), C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C2(H2A,H2B), C3(H3A,H3B), C31(H31A,H31B), C7(H7A,H7B), C6(H6A,
 H6B), C35(H35A,H35B), C34(H34A,H34B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15)
5.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C9(H9A,H9B,H9C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;