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_4348534
_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         'C66 H62 Au2.11 Cl2.11 Fe P4, 3(C H2 Cl2)'
_chemical_formula_sum            'C69 H68 Au2.11 Cl8.11 Fe P4'
_chemical_formula_weight         1779.48
_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
_audit_creation_date             2015-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2298(2)
_cell_length_b                   22.4425(4)
_cell_length_c                   23.1174(4)
_cell_measurement_reflns_used    15183
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6855.1(2)
_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    'ShelXT (Sheldrick, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0572
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70945
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.566
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    5.157
_exptl_absorpt_correction_T_max  0.5477
_exptl_absorpt_correction_T_min  0.3731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'c.f. r.h. blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       plate
_exptl_crystal_F_000             3489
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.299
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         15597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+32.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13156
_reflns_number_total             15597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01318_si_003.cif
_cod_data_source_block           14
_cod_database_code               4348534
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Cl8A, Cl9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C67B)=Sof(H67A)=Sof(H67B)=Sof(Cl4B)=Sof(Cl5B)=1-FVAR(1)
 Sof(C67)=Sof(H67C)=Sof(H67D)=Sof(Cl4)=Sof(Cl5)=FVAR(1)
 Sof(H68C)=Sof(H68D)=Sof(Cl6B)=1-FVAR(2)
 Sof(H68A)=Sof(H68B)=Sof(Cl7)=FVAR(2)
 Sof(Au3)=Sof(Cl3)=Sof(H69C)=Sof(H69D)=Sof(Cl9A)=Sof(Cl8A)=1-FVAR(3)
 Sof(H69A)=Sof(H69B)=Sof(Cl8)=Sof(Cl9)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C69(H69C,H69D), C68(H68A,H68B), C68(H68C,H68D), C67B(H67A,
 H67B), C67(H67C,H67D)
4.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
 C38(H38), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'