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_7712380
_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
'C47 H64 Au P3 Rh, C2 F6 N O4 S2, C6 H6'
_chemical_formula_sum            'C55 H70 Au F6 N O4 P3 Rh S2'
_chemical_formula_weight         1380.02
_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   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                85.692(4)
_cell_angle_beta                 88.744(4)
_cell_angle_gamma                86.622(4)
_cell_formula_units_Z            4
_cell_length_a                   14.1319(13)
_cell_length_b                   17.4134(15)
_cell_length_c                   23.475(2)
_cell_measurement_reflns_used    115
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      3.03
_cell_volume                     5749.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1328
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28874
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         1.808
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.

Final HKLF 4 output contains 316790 reflections, Rint = 0.1526
 (71194 with I > 3sig(I), Rint = 0.0982)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prysm
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.781
_refine_diff_density_min         -2.192
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1337
_refine_ls_number_reflns         28874
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.0863
_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^)+89.7588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18490
_reflns_number_total             28874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00410d3.cif
_cod_data_source_block           7aCyp
_cod_depositor_comments
;

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C110 H140 Au2 F12 N2 O8 P6 Rh2 S4'
_cod_original_formula_weight         2760.04
_cod_original_formula_moiety
'2(C47 H64 Au P3 Rh), 2(C2 F6 N O4 S2), 2(C6 H6)'
_cod_original_formula_units_Z            2
_cod_database_code               7712380
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6865(13)
 0.3090(12) 0.0045(6)
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. Rigid bond restraints
 S2, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C37(H37), C42(H42), C88(H88), C93(H93)
4.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C18(H18A,H18B),
 C89(H89A,H89B), C90(H90A,H90B), C92(H92A,H92B), C94(H94A,H94B), C95(H95A,H95B),
  C96(H96A,H96B), C97(H97A,H97B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C1(H1), C6(H6), C7(H7), C8(H8), C9(H9), C17(H17), C19(H19),
 C23(H23), C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C91(H91), C50(H50),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C68(H68),
 C69(H69), C70(H70), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84),
  C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C111(H111)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C65(H65A,H65B,H65C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C86(H86A,
 H86B,H86C), C87(H87A,H87B,H87C)
;
_shelx_res_checksum              42869
_shelx_hkl_checksum              48160
_olex2_submission_special_instructions 'No special instructions were received'