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_4086629
_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         'C27 H32 Au Cl Fe N4, C H Cl3'
_chemical_formula_sum            'C28 H33 Au Cl4 Fe N4'
_chemical_formula_weight         820.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                81.906(5)
_cell_angle_beta                 75.409(4)
_cell_angle_gamma                69.238(6)
_cell_formula_units_Z            2
_cell_length_a                   10.7513(6)
_cell_length_b                   10.7753(9)
_cell_length_c                   14.3647(4)
_cell_measurement_reflns_used    13313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5280
_cell_measurement_theta_min      3.8490
_cell_volume                     1503.44(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.8527
_diffrn_measurement_details
;
  1 omega  -57.00   70.40   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   19.0000 -120.0000 182

  2 omega  -86.00   15.50   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -37.0000   60.0000 145

  3 omega  -20.00   31.10   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000   60.0000 73

  4 omega  -99.00  -55.60   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000  120.0000 62

  5 omega  -19.00   54.50   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  -99.0000   90.0000 105

  6 omega  -86.00   15.50   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -37.0000  -90.0000 145

  7 omega  -86.00   15.50   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -37.0000 -180.0000 145

  8 omega  -73.00  -26.80   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  132.0000  138.8956 66

  9 omega  -61.00   41.90   0.7000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  -57.0000  -30.0000 147
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0000600000
_diffrn_orient_matrix_UB_12      -0.0661140000
_diffrn_orient_matrix_UB_13      0.0016031000
_diffrn_orient_matrix_UB_21      0.0118425000
_diffrn_orient_matrix_UB_22      -0.0109682000
_diffrn_orient_matrix_UB_23      0.0473487000
_diffrn_orient_matrix_UB_31      -0.0713213000
_diffrn_orient_matrix_UB_32      0.0219243000
_diffrn_orient_matrix_UB_33      0.0191681000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29958
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.403
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.737
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description
;
;
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.3362
_exptl_crystal_size_mid          0.2256
_exptl_crystal_size_min          0.1826
_refine_diff_density_max         2.703
_refine_diff_density_min         -1.852
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         7573
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0600P)^2^+2.8391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6690
_reflns_number_total             7573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00517_si_003.cif
_cod_data_source_block           str1822
_cod_depositor_comments
'Adding full bibliography for 4086627--4086629.cif.'
_cod_original_cell_volume        1503.42(17)
_cod_database_code               4086629
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C27 H32 N4 Fe Au Cl'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H16A(0.056) H16B(0.056) H16C(0.056) H7A(0.061) H7B(0.061)
 H12(0.041) H20(0.051) H6A(0.045) H6B(0.045) H15(0.035) H19(0.049) H8A(0.069)
 H8B(0.069) H21(0.052) H22(0.045) H28(0.072) H2A(0.057) H2B(0.057) H23(0.103)
 H27(0.102) H3A(0.1) H3B(0.1) H26(0.117) H24(0.121) H9A(0.106) H9B(0.106)
 H9C(0.106) H5A(0.153) H5B(0.153) H5C(0.153) H4A(0.123) H4B(0.123) H25(0.123)
 Fixed X: H16A(0.1519) H16B(0.1318) H16C(0.2225) H7A(0.3894) H7B(0.5081) H12(-
 0.2284) H20(-0.3863) H6A(0.3478) H6B(0.3367) H15(0.2242) H19(-0.3501)
 H8A(0.3223) H8B(0.4435) H21(-0.1814) H22(-0.0171) H28(0.5843) H2A(-0.2242)
 H2B(-0.1268) H23(0.0496) H27(0.1408) H3A(-0.0858) H3B(-0.1964) H26(-0.0379)
 H24(-0.1766) H9A(0.4898) H9B(0.6015) H9C(0.4912) H5A(-0.2442) H5B(-0.3783)
 H5C(-0.3695) H4A(-0.2275) H4B(-0.3431) H25(-0.2274)
 Fixed Y: H16A(0.5211) H16B(0.6678) H16C(0.6057) H7A(0.6104) H7B(0.5076)
 H12(0.7834) H20(0.9207) H6A(0.4476) H6B(0.4192) H15(0.5448) H19(0.913)
 H8A(0.7316) H8B(0.6295) H21(0.7419) H22(0.6238) H28(0.7868) H2A(0.7299)
 H2B(0.7042) H23(0.9343) H27(0.8399) H3A(0.9047) H3B(0.9122) H26(0.9709)
 H24(1.1206) H9A(0.826) H9B(0.6937) H9C(0.7761) H5A(1.1576) H5B(1.1769)
 H5C(1.1344) H4A(0.9741) H4B(0.9476) H25(1.1389)
 Fixed Z: H16A(1.1016) H16B(1.1197) H16C(1.0227) H7A(0.7186) H7B(0.6523)
 H12(0.8231) H20(1.3483) H6A(0.6002) H6B(0.7115) H15(0.8665) H19(1.1654)
 H8A(0.5853) H8B(0.5196) H21(1.4018) H22(1.2539) H28(0.0242) H2A(0.6569)
 H2B(0.5549) H23(1.0754) H27(1.226) H3A(0.5881) H3B(0.5334) H26(1.3718)
 H24(1.1169) H9A(0.5396) H9B(0.5643) H9C(0.6474) H5A(0.5954) H5B(0.6752)
 H5C(0.5731) H4A(0.7118) H4B(0.6791) H25(1.2958)
;
_olex2_submission_special_instructions 'No special instructions were received'