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_4348532
_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 Au Cl Fe P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H66 Au Cl5 Fe P4'
_chemical_formula_weight         1437.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                73.2620(10)
_cell_angle_beta                 85.8130(10)
_cell_angle_gamma                86.0190(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9199(3)
_cell_length_b                   15.0009(4)
_cell_length_c                   17.2749(4)
_cell_measurement_reflns_used    12498
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3193.53(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '\k-geometry diffractometer'
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23803
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.651
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    2.871
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.237
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         14509
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0159P)^2^+20.2706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12443
_reflns_number_total             14509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01318_si_003.cif
_cod_data_source_block           12
_cod_database_code               4348532
_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(Cl2) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(Cl5) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.05 and sigma for terminal
atoms of 0.2
3. Rigid body (RIGU) restrains
 AuB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(AuB)=1-FVAR(1)
 Sof(Au)=FVAR(1)
5.a Free rotating group:
 Cl2(Cl3,C1A)
5.b Secondary CH2 refined with riding coordinates:
 C1A(H1AB,H1AC), C1B(H1BA,H1BB)
5.c 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)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), 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),
 C37(H37), 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), C1AA(H1AA), C63(H63), C64(H64), C65(H65), C66(H66)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'