Gold(I) Complexes of Ferrocenyl Polyphosphines: Aurophilic Gold Chloride Formation and Phosphine-Concerted Shuttling of a Dinuclear [ClAu···AuCl] Fragment.
Rampazzi, Vincent; Roger, Julien; Amardeil, Régine; Penouilh, Marie-José; Richard, Philippe; Fleurat-Lessard, Paul; Hierso, Jean-Cyrille; Inorganic chemistry 55 (2016) 10907–10921; doi:10.1021/acs.inorgchem.6b01318

data_4348535
_publ_section_title
;
 Gold(I) Complexes of Ferrocenyl Polyphosphines: Aurophilic Gold Chloride
 Formation and Phosphine-Concerted Shuttling of a Dinuclear
 [ClAu&#x00B7;&#x00B7;&#x00B7;AuCl] Fragment.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10907
_journal_page_last               10921
_journal_paper_doi               10.1021/acs.inorgchem.6b01318
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C42 H44 Au2 Cl2 Fe P2, 1.5(C1 H2 Cl2)'
_chemical_formula_sum            'C43.5 H47 Au2 Cl5 Fe P2'
_chemical_formula_weight         1258.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.8790(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6720(2)
_cell_length_b                   20.4470(4)
_cell_length_c                   16.5451(3)
_cell_measurement_temperature    115
_cell_volume                     4470.12(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38974
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.617
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    7.269
_exptl_absorpt_correction_T_max  0.6028
_exptl_absorpt_correction_T_min  0.4076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'c.f. r.h. blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       plate
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.073
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+20.7934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9580
_reflns_number_total             10186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01318_si_002.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C43.50 H47 Au2 Cl5 Fe P2'
_cod_database_code               4348535
_shelxl_version_number           2014-3
_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. Uiso/Uaniso restraints and constraints
Uanis(C43) = Uanis(C43A)
Uanis(Cl3) = Uanis(Cl3A)
Uanis(Cl4) = Uanis(Cl4A)
3. Others
 Sof(Cl3A)=Sof(Cl4A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1)
 Fixed Sof: Cl5(0.5) Cl6(0.5) C44(0.5) H44A(0.5) H44B(0.5)
4.a Free rotating group:
 Cl3(Cl4,C43), Cl3A(Cl4A,C43A), Cl5(Cl6,C44)
4.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C43A(H43C,H43D), C44(H44A,H44B)
4.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C11(H11), C13(H13), C14(H14), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_original_sample_id 262
_olex2_submission_special_instructions 'No special instructions were received'