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_7712383
_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         'C67 H70 Au P3 Rh, C2 F6 N O4 S2'
_chemical_formula_sum            'C69 H70 Au F6 N O4 P3 Rh S2'
_chemical_formula_weight         1548.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0982(4)
_cell_length_b                   17.1018(4)
_cell_length_c                   30.9379(9)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.36
_cell_volume                     6930.2(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_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  0.1570
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            141225
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.690
_diffrn_reflns_theta_min         2.066
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.544
_exptl_absorpt_correction_T_max  0.7391
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1145 before and 0.1037 after correction.
The Ratio of minimum to maximum transmission is 0.8643.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       prism
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         13142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0297P)^2^+7.4929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10090
_reflns_number_total             13142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00410d3.cif
_cod_data_source_block           7cCyp
_cod_database_code               7712383
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.997(7)
 0.003(7)
2. 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
3.a Ternary CH refined with riding coordinates:
 C58(H58), C63(H63)
3.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C67(H67A,H67B), C11(H11A,H11B), C64(H64A,H64B), C62(H62A,
 H62B), C10(H10A,H10B), C66(H66A,H66B), C60(H60A,H60B), C65(H65A,H65B),
 C61(H61A,H61B)
3.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C5(H5), C25(H25), C29(H29), C4(H4), C31(H31), C9(H9), C2(H2),
 C54(H54), C26(H26), C52(H52), C32(H32), C33(H33), C22(H22), C23(H23), C34(H34),
  C40(H40), C21(H21), C19(H19), C46(H46), C6(H6), C13(H13), C53(H53), C38(H38),
 C28(H28), C1(H1), C14(H14), C45(H45), C17(H17), C27(H27), C44(H44), C39(H39),
 C20(H20), C7(H7), C16(H16), C15(H15)
3.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C56(H56A,H56B,H56C), C49(H49A,H49B,H49C), C48(H48A,H48B,
 H48C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              74349
_shelx_hkl_checksum              12926
_shelx_fab_checksum              35755
_olex2_submission_special_instructions 'No special instructions were received'