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_7719005
_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
'1(C61.978 H53.935 Ag N2 P4 S2), F6 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C63.98 H58.95 Ag F6 N2 O0.5 P5 S2'
_chemical_formula_weight         1304.74
_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     dual
_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                87.876(6)
_cell_angle_beta                 78.360(5)
_cell_angle_gamma                82.975(4)
_cell_formula_units_Z            4
_cell_length_a                   13.5820(14)
_cell_length_b                   21.259(3)
_cell_length_c                   23.026(3)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.336
_cell_measurement_theta_min      2.374
_cell_volume                     6462.4(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.980
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            111867
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         0.252
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.8978.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       plate
_exptl_crystal_F_000             2675
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1493
_refine_ls_number_reflns         26074
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0576P)^2^+6.9332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18506
_reflns_number_total             26074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00292c2.cif
_cod_data_source_block           first_25
_cod_original_cell_volume        6462.2(14)
_cod_original_formula_sum        'C63.98 H58.95 Ag F6 N2 O0.50 P5 S2'
_cod_database_code               7719005
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.897
_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. Restrained distances
 C4AA-S4AA
 1.8 with sigma of 0.02
3. Others
 Sof(S4AA)=Sof(C2BA)=Sof(H2BA)=Sof(C1BA)=Sof(C0BA)=Sof(H0BA)=Sof(C5)=Sof(H5)=
 Sof(C3BA)=Sof(H3BA)=1-FVAR(1)
 Sof(S00F)=Sof(C02L)=Sof(H02L)=Sof(C03S)=Sof(H03S)=Sof(C041)=Sof(C047)=
 Sof(H047)=Sof(C04H)=Sof(H04H)=FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
 Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C02S(H02,H), C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C016(H016),
 C01A(H01A), C01D(H01D), C01F(H01F), C01H(H01H), C01J(H01J), C01K(H01K),
 C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01R(H01R),
 C01S(H01S), C01T(H01T), C01W(H01W), C01Z(H01Z), C021(H021), C022(H022),
 C023(H023), C024(H024), C025(H025), C027(H027), C029(H029), C02A(H02A),
 C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G),
 C02I(H02O), C02J(H02J), C02K(H02S), C02L(H02L), C02M(H02M), C02N(H02N),
 C02O(H02T), C02P(H02P), C02Q(H02Q), C02R(H02R), C02T(H02U), C02U(H02V),
 C02W(H02W), C02X(H02X), C02Y(H02Y), C02Z(H02Z), C030(H030), C031(H031),
 C034(H034), C036(H036), C038(H038), C039(H039), C03A(H03D), C03B(H03F),
 C03C(H03G), C03D(H03H), C03E(H03E), C03F(H03I), C03G(H03J), C03I(H03K),
 C03L(H03L), C03M(H03M), C03N(H03N), C03O(H03O), C03P(H03P), C03Q(H03Q),
 C03R(H03R), C03S(H03S), C03T(H03T), C03V(H03V), C03W(H03W), C03Z(H03Z),
 C040(H040), C042(H042), C043(H043), C044(H044), C046(H046), C047(H047),
 C049(H049), C04B(H04B), C04D(H04D), C04E(H04F), C04F(H04G), C04H(H04H), C8(H8),
  C10(H10), C4(H4), C9(H9), C1(H1), C0AA(H0AA), C2BA(H2BA), C0BA(H0BA), C5(H5),
 C3BA(H3BA)
4.c Idealised Me refined as rotating group:
 C02H(H02H,H02I,H02K), C037(H03A,H03B,H03C), C04C(H04A,H04C,H04E), C1AA(H1AA,
 H1AB,H1AC), C3AA(H3AA,H3AB,H3AC), C2(H2A,H2B,H2C), C4AA(H4AA,H4AB,H4AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77003
_shelx_fab_checksum              48385
_olex2_submission_special_instructions 'No special instructions were received'