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_7712382
_publ_section_title
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 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         'C45 H51 Au P2'
_chemical_formula_sum            'C45 H51 Au P2'
_chemical_formula_weight         850.76
_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             2022-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-21 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1697(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5273(5)
_cell_length_b                   20.7432(8)
_cell_length_c                   16.8019(7)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.31
_cell_volume                     4713.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0790
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         1.952
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.214
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.7882.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.677
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         11695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0391P)^2^+13.2344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8801
_reflns_number_total             11695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00410d3.cif
_cod_data_source_block           '[(PCyp2ArXyl2)Au2(dppe)](NTf2)2'
_cod_database_code               7712382
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.699
_shelx_estimated_absorpt_t_min   0.595
_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. Others
 Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Sof(Au2)=1-FVAR(2)
 Sof(Au1)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C23(H23), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C30(H30C,H30D), C31A(H31A,H31B), C31B(H31C,H31D),
 C32(H32A,H32B), C32(H32C,H32D), C45(H45A,H45B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31551
_shelx_hkl_checksum              54139
_shelx_fab_checksum              82263
_olex2_submission_special_instructions 'No special instructions were received'