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_4348536
_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         'C38 H44 Au2 Cl2 Fe O4 P2, C H2 Cl2'
_chemical_formula_sum            'C39 H46 Au2 Cl4 Fe O4 P2'
_chemical_formula_weight         1232.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-04-26
_audit_creation_method           'WinGX-Routine IMPORT-KappaCCD'
_cell_angle_alpha                90
_cell_angle_beta                 112.3795(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7292(4)
_cell_length_b                   11.8179(3)
_cell_length_c                   22.1518(6)
_cell_measurement_reflns_used    4844
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4291.72(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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 9
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.30797E-2
_diffrn_orient_matrix_UB_12      0.422437E-1
_diffrn_orient_matrix_UB_13      -0.381109E-1
_diffrn_orient_matrix_UB_21      -0.171242E-1
_diffrn_orient_matrix_UB_22      -0.697345E-1
_diffrn_orient_matrix_UB_23      -0.274293E-1
_diffrn_orient_matrix_UB_31      -0.584643E-1
_diffrn_orient_matrix_UB_32      0.226504E-1
_diffrn_orient_matrix_UB_33      -0.133694E-1
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.338732E-1
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19210
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.523
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    7.515
_exptl_absorpt_correction_T_max  0.3439
_exptl_absorpt_correction_T_min  0.1686
_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    1.907
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00047(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.374
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.374
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0411
_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^)+80.8585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4769
_reflns_number_total             4901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01318_si_002.cif
_cod_data_source_block           9
_cod_database_code               4348536
_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. Others
 Fixed Sof: C100(0.5) H10A(0.5) H10B(0.5) Cl2(0.5) Cl3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B)
3.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C11(H11), C12(H12), C16(H16), C17(H17)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C)
;
_olex2_submission_original_sample_id v350
_olex2_submission_special_instructions 'No special instructions were received'