Polarized Au(I)/Rh(I) Bimetallic Pairs Cooperatively Trigger Ligand non-Innocence and Bond Activation
González Alférez, Macarena; Moreno, Juan J.; Maya, Celia; Campos, Jesús; Dalton Transactions  (2023) –; doi:10.1039/D3DT00410D

data_7712377
_publ_section_title
;
 Polarized Au(I)/Rh(I) Bimetallic Pairs Cooperatively Trigger Ligand
 non-Innocence and Bond Activation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00410D
_journal_year                    2023
_chemical_formula_moiety         '2(C39 H52 Au P3 Rh), 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C82 H104 Au2 F12 N2 O8 P6 Rh2 S4'
_chemical_formula_weight         2387.48
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-21 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4312(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.8321(8)
_cell_length_b                   8.9867(3)
_cell_length_c                   40.1396(18)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.40
_cell_volume                     9301.5(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            49516
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.696
_diffrn_reflns_theta_min         2.033
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1015 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.6562.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       needle
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         17159
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0656
_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^)+94.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12482
_reflns_number_total             17159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00410d3.cif
_cod_data_source_block           7aMe
_cod_database_code               7712377
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C40, C41, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C20(H20), C21(H21),
 C22(H22), C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C41(H41),
  C40(H40), C44(H44), C48(H48), C47(H47), C46(H46), C45(H45), C59(H59),
 C60(H60), C61(H61), C73(H73), C74(H74), C75(H75), C68(H68), C70(H70), C69(H69)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C63(H63A,H63B,H63C), C15(H15A,H15B,H15C),
 C10(H10A,H10B,H10C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              86176
_shelx_hkl_checksum              68353
_olex2_submission_special_instructions 'No special instructions were received'