Metal ion independent conductance through bis-chelated metal complex molecular wires based on a bis(diphenylphosphino)aniline derivative
Gatto, Marco F.; Sangtarash, Sara; Jago, David; Abram, R. Tom; Barrett, Eleanor; Sil, Amit; Koutsantonis, George A.; Higgins, Simon J.; Robertson, Craig M.; Nichols, Richard J.; Sadeghi, Hatef; Vezzoli, Andrea; Dalton Transactions 54 (2025) 7874–7881; doi:10.1039/D5DT00292C

data_7719003
_publ_section_title
;
 Metal ion independent conductance through bis-chelated metal complex
 molecular wires based on a bis(diphenylphosphino)aniline derivative
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              7874
_journal_page_last               7881
_journal_paper_doi               10.1039/D5DT00292C
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C62 H54 Au N2 P4 S2), 2(F6 P)'
_chemical_formula_sum            'C124 H108 Au2 F12 N4 P10 S4'
_chemical_formula_weight         2714.01
_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
_audit_creation_date             2024-12-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-12-06 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                74.296(2)
_cell_angle_beta                 89.995(2)
_cell_angle_gamma                74.781(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2295(3)
_cell_length_b                   21.7084(6)
_cell_length_c                   24.2101(5)
_cell_measurement_reflns_used    25476
_cell_measurement_temperature    109(14)
_cell_measurement_theta_max      26.3440
_cell_measurement_theta_min      1.7320
_cell_volume                     5953.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 41.122a 64-bit (release 06-12-2021))'
_computing_data_reduction        'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -48.00  75.00   0.50    4.93    --  -12.10  57.00 -90.00  246
  2  \w    -69.00  26.00   0.50    4.93    --  -12.10 -68.00  90.00  190
  3  \w    -82.00  -3.00   0.50    4.93    --  -12.10 -57.00 150.00  158
  4  \w    -33.00  23.00   0.50    4.93    --  -12.10 -68.00 -60.00  112
  5  \w    -12.00  75.00   0.50    4.93    --  -12.10  68.00-150.00  174
  6  \w     -6.00  29.00   0.50    4.93    --  -12.10  68.00 -30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236033000
_diffrn_orient_matrix_UB_12      -0.0162723000
_diffrn_orient_matrix_UB_13      -0.0207544000
_diffrn_orient_matrix_UB_21      0.0553851000
_diffrn_orient_matrix_UB_22      -0.0052444000
_diffrn_orient_matrix_UB_23      0.0124149000
_diffrn_orient_matrix_UB_31      -0.0030688000
_diffrn_orient_matrix_UB_32      -0.0308580000
_diffrn_orient_matrix_UB_33      0.0186219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24260
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.731
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.107a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       needle
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         7.500
_refine_diff_density_min         -3.407
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1410
_refine_ls_number_reflns         24260
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0971
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2869
_refine_ls_wR_factor_ref         0.2983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21608
_reflns_number_total             24260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00292c2.cif
_cod_data_source_block           marco1
_cod_database_code               7719003
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20S2P3F6Au
_chemical_oxdiff_usercomment     'Marco 1 Au'
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.772
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6649(16)
 0.3351(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C106) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C113) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C19, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14, C20, C18, C17, C16, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C37, C38, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C113, C118, C117, C116, C115, C114
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C42(H42), C53(H53), C47(H47), C49(H49), C120(H120), C139(H139),
 C134(H134), C111(H111), C25(H25), C142(H142), C9(H9), C17(H17), C62(H62),
 C126(H126), C28(H28), C13(H13), C121(H121), C6(H6), C143(H143), C123(H123),
 C19(H19), C136(H136), C153(H153), C145(H145), C63(H63), C140(H140), C112(H112),
  C133(H133), C51(H51), C108(H108), C20(H20), C54(H54), C45(H45), C116(H116),
 C127(H127), C115(H115), C150(H150), C44(H44), C12(H12), C154(H154), C24(H24),
 C41(H41), C55(H55), C30(H30), C61(H61), C160(H160), C151(H151), C146(H146),
 C118(H118), C114(H114), C131(H131), C18(H18), C158(H158), C3(H3), C124(H124),
 C147(H147), C43(H43), C57(H57), C104(H104), C34(H34), C23(H23), C10(H10),
 C159(H159), C2(H2), C32(H32), C152(H152), C38(H38), C141(H141), C117(H117),
 C128(H128), C29(H29), C101(H101), C102(H102), C148(H148), C22(H22), C122(H122),
  C56(H56), C109(H109), C105(H105), C37(H37), C130(H130), C35(H35), C59(H59),
 C129(H129), C110(H110), C50(H50), C149(H149), C15(H15), C31(H31), C48(H48),
 C16(H16), C11(H11), C60(H60), C156(H156), C157(H157)
5.b Idealised Me refined as rotating group:
 C137(H13A,H13B,H13C), C39(H39A,H39B,H39C), C7(H7A,H7B,H7C), C106(H10A,H10B,
 H10C)
;
_shelx_res_checksum              90346
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.779