Break-junction studies on paddle-wheel complexes with four lateral anchor groups: small influence of metal-metal bond order.
Mang, André; Beltako, Katawoura; Kadriu, Besa; Linseis, Michael; Pauly, Fabian; Winter, Rainer F.; Nanoscale 17 (2025) 24226–24240; doi:10.1039/d5nr01695a

data_1575917
_publ_section_title
;
 Break-junction studies on paddle-wheel complexes with four lateral anchor
 groups: small influence of metal-metal bond order.
;
_journal_issue                   41
_journal_name_full               Nanoscale
_journal_page_first              24226
_journal_page_last               24240
_journal_paper_doi               10.1039/d5nr01695a
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C80 H68 Mo2 N8 S4, 2(C H2 Cl2)'
_chemical_formula_sum            'C82 H72 Cl4 Mo2 N8 S4'
_chemical_formula_weight         1631.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2255(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.97951(6)
_cell_length_b                   17.60118(8)
_cell_length_c                   15.10734(7)
_cell_measurement_reflns_used    55079
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6430
_cell_measurement_theta_min      3.8570
_cell_volume                     3983.13(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.71a 64-bit (release 17-04-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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    -81.00 -16.00   0.50    0.20    --  -59.18 125.00   0.00  130
  2  \w    -98.00 -32.00   0.50    0.20    --  -75.23 125.00 -30.00  132
  3  \w    -81.00 -16.00   0.50    0.20    --  -59.18 125.00 -60.00  130
  4  \w    -98.00 -32.00   0.50    0.20    --  -75.23 125.00 -60.00  132
  5  \w    -98.00 -32.00   0.50    0.20    --  -75.23 125.00 -90.00  132
  6  \w    -98.00 -32.00   0.50    0.20    --  -75.23 125.00-150.00  132
  7  \w    -95.00 -58.00   0.50    0.20    --  -72.85 125.00-180.00   74
  8  \w    -70.00 -18.00   0.50    0.20    --  -59.18 107.00 -24.00  104
  9  \w    -84.00 -32.00   0.50    0.20    --  -72.85 107.00 -24.00  104
 10  \w    -87.00 -34.00   0.50    0.20    --  -75.23 107.00 -24.00  106
 11  \w    -98.00 -32.00   0.50    0.20    --  -75.23 125.00  30.00  132
 12  \w    -98.00 -32.00   0.50    0.20    --  -75.23 125.00 120.00  132
 13  \w   -106.00 -27.00   0.50    0.20    --  -59.18 -15.00   0.00  158
 14  \w   -122.00 -43.00   0.50    0.20    --  -75.23 -15.00 120.00  158
 15  \w   -122.00 -43.00   0.50    0.20    --  -75.23 -15.00 -60.00  158
 16  \w   -122.00 -43.00   0.50    0.20    --  -75.23 -15.00-120.00  158
 17  \w   -122.00 -43.00   0.50    0.20    --  -75.23 -15.00-180.00  158
 18  \w     19.00  80.00   0.50    0.20    --   57.27-125.00-180.00  122
 19  \w     38.00 101.00   0.50    0.20    --   81.23-125.00 -30.00  126
 20  \w     38.00 101.00   0.50    0.20    --   81.23-125.00  90.00  126
 21  \w     19.00  80.00   0.50    0.20    --   57.27-125.00 150.00  122
 22  \w     38.00 101.00   0.50    0.20    --   81.23-125.00 150.00  126
 23  \w     28.00  94.00   0.50    0.20    --   71.00-125.00 120.00  132
 24  \w     19.00  80.00   0.50    0.20    --   57.27-125.00 -30.00  122
 25  \w     16.00  69.00   0.50    0.20    --   57.27-107.00-122.00  106
 26  \w     38.00 101.00   0.50    0.20    --   81.23-125.00-180.00  126
 27  \w     38.00 101.00   0.50    0.20    --   81.23-125.00-120.00  126
 28  \w     30.00  83.00   0.50    0.20    --   71.00-107.00-122.00  106
 29  \w     40.00  92.00   0.50    0.20    --   81.23-107.00-122.00  104
 30  \w     48.00 128.00   0.50    0.20    --   81.23  15.00-180.00  160
 31  \w     48.00 128.00   0.50    0.20    --   81.23  15.00-120.00  160
 32  \w     48.00 128.00   0.50    0.20    --   81.23  15.00 -90.00  160
 33  \w     48.00 128.00   0.50    0.20    --   81.23  15.00 -30.00  160
 34  \w     24.00 104.00   0.50    0.20    --   57.27  15.00  60.00  160
 35  \w     48.00 128.00   0.50    0.20    --   81.23  15.00  90.00  160
 36  \w     38.00 118.00   0.50    0.20    --   71.00  15.00 150.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0642767000
_diffrn_orient_matrix_UB_12      0.0638337000
_diffrn_orient_matrix_UB_13      -0.0281357000
_diffrn_orient_matrix_UB_21      -0.0018626000
_diffrn_orient_matrix_UB_22      0.0324036000
_diffrn_orient_matrix_UB_23      0.0947715000
_diffrn_orient_matrix_UB_31      0.0802866000
_diffrn_orient_matrix_UB_32      -0.0502773000
_diffrn_orient_matrix_UB_33      0.0251640000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79587
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.677
_diffrn_reflns_theta_min         3.856
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.71a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 6683 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         15367
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+2.1548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                14841
_reflns_number_total             15367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01695a2.cif
_cod_data_source_block           exp_484_auto
_cod_depositor_comments
'Adding full bibliography for 1575913--1575917.cif.'
_cod_database_code               1575917
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C166  H148  N16  S8  Cl12  Mo4  '
_chemical_oxdiff_usercomment     Mo-paddle-wheel
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.950
_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
 S3-C51 \\sim S3'-C51
 with sigma of 0.02
 S3-C54 \\sim S3'-C54'
 with sigma of 0.02
 C51-C54 \\sim C51-C54'
 with sigma of 0.04
 S4-C71 \\sim S4'-C71
 with sigma of 0.02
 S4-C74 \\sim S4'-C74'
 with sigma of 0.02
 C71-C74 \\sim C71-C74'
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C51, S3', C54'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S3, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S4', C74'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S4, C74
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S3')=Sof(C54')=Sof(H54d)=Sof(H54e)=Sof(H54f)=1-FVAR(1)
 Sof(S3)=Sof(C54)=Sof(H54a)=Sof(H54b)=Sof(H54c)=FVAR(1)
 Sof(S4')=Sof(C74')=Sof(H74d)=Sof(H74e)=Sof(H74f)=1-FVAR(2)
 Sof(S4)=Sof(C74)=Sof(H74a)=Sof(H74b)=Sof(H74c)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C81(H81a,H81b), C82(H82a,H82b)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45),
  C46(H46), C49(H49), C50(H50), C52(H52), C53(H53), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
  C69(H69), C70(H70), C72(H72), C73(H73), C76(H76), C77(H77), C78(H78),
 C79(H79), C80(H80)
5.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C34(H34a,H34b,H34c), C54(H54a,H54b,H54c), C74(H74a,H74b,
 H74c), C54'(H54d,H54e,H54f), C74'(H74d,H74e,H74f)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 86 electrons were 
found in a volume of 382\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C5H12] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87755
_shelx_fab_checksum              95768
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.796