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_7712384
_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         'C68 H70 Au N P2 Rh, C3 H3.5'
_chemical_formula_sum            'C71 H73.5 Au N P2 Rh'
_chemical_formula_weight         1302.62
_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     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                 112.8643(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0998(7)
_cell_length_b                   24.7705(8)
_cell_length_c                   28.1675(9)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      24.986
_cell_measurement_theta_min      2.258
_cell_volume                     15493.8(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            146359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.037
_diffrn_reflns_theta_max         25.037
_diffrn_reflns_theta_min         2.258
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.179
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0707 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.8704.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_description       cube
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         13710
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0617P)^2^+72.4961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11500
_reflns_number_total             13710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00410d3.cif
_cod_data_source_block           '[(C9H7)(PPh3)(XylNC)RhAu(PCyp2ArXyl2)](NTf2)'
_cod_original_formula_sum        'C71 H73.50 Au N P2 Rh'
_cod_database_code               7712384
_shelx_shelxl_version_number     2018/3
_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. Rigid bond restraints
 C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Fixed Sof: H71A(0.5) H71B(0.5)
4.a Ternary CH refined with riding coordinates:
 C59(H59), C64(H64)
4.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,
 H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C71(H71A,H71B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C2(H2), 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), C31(H31), C32(H32),
 C33(H33), C39(H39), C40(H40), C41(H41), C45(H45), C46(H46), C47(H47), C53(H53),
  C54(H54), C55(H55), C72(H72), C73(H73), C74(H74)
4.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1514
_shelx_hkl_checksum              48007
_shelx_fab_checksum              44937
_olex2_submission_special_instructions 'No special instructions were received'