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_1575915
_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
'C72 H56 Mo2 N12, C4 H8 O, 0.5(C5 H12), 1[C4H8O]'
_chemical_formula_sum            'C78.5 H70 Mo2 N12 O'
_chemical_formula_weight         1389.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 89.839(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1390(5)
_cell_length_b                   23.7263(3)
_cell_length_c                   12.3581(2)
_cell_measurement_reflns_used    49654
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.36
_cell_volume                     7371.0(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.86, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
 178 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46289
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.589
_diffrn_reflns_theta_min         2.361
_diffrn_source
'Sealed Mo X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.7392
_exptl_absorpt_correction_T_min  0.5421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00087(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         16900
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+6.8372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13397
_reflns_number_total             16900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01695a2.cif
_cod_data_source_block           am151_2
_cod_depositor_comments
'Adding full bibliography for 1575913--1575917.cif.'
_cod_original_formula_sum        'C78.50 H70 Mo2 N12 O'
_cod_database_code               1575915
_shelx_shelxl_version_number     2019/2
_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
 C73-C74 = C74-C75 = C75-C76 = C76-C77
 1.52 with sigma of 0.02
 C73-C75 = C74-C76 = C75-C77
 2.54 with sigma of 0.04
 C73-C74 \\sim C74-C75 \\sim C75-C76 \\sim C76-C77
 with sigma of 0.02
 C73-C75 \\sim C75-C77 \\sim C74-C76
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C73, C74, C75, C76, C77
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) C74(0.5) H74A(0.5)
 H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5) C76(0.5) H76A(0.5) H76B(0.5) C77(0.5)
 H77A(0.5) H77B(0.5) H77C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C74(H74A,
 H74B), C75(H75A,H75B), C76(H76A,H76B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41),
  C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60),
  C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72)
6.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C77(H77A,H77B,H77C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18450
_shelx_fab_checksum              21084
_olex2_submission_special_instructions 'No special instructions were received'