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_7712376
_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         'C48 H70 Au P3 Rh'
_chemical_formula_sum            'C48 H70 Au P3 Rh'
_chemical_formula_weight         1039.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                104.345(3)
_cell_angle_beta                 98.054(3)
_cell_angle_gamma                90.238(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4923(10)
_cell_length_b                   17.2690(18)
_cell_length_c                   18.5760(18)
_cell_measurement_reflns_used    4229
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.30
_cell_volume                     2918.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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 0.998
_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  0.1604
_diffrn_reflns_av_unetI/netI     0.1210
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45966
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.169
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.900
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1330 before and 0.0868 after correction.
The Ratio of minimum to maximum transmission is 0.4731.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       needle
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.120
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6412
_reflns_number_total             10273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00410d3.cif
_cod_data_source_block           4bCyp
_cod_database_code               7712376
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.439
_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.a Ternary CH refined with riding coordinates:
 C39(H39), C44(H44)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B),
 C47(H47A,H47B), C48(H48A,H48B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C33(H33),
 C34(H34), C35(H35)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              72800
_shelx_hkl_checksum              9540
_shelx_fab_checksum              60495
_olex2_submission_special_instructions 'No special instructions were received'