Single-molecule conductance studies on quasi- and metallaaromatic dibenzoylmethane coordination compounds and their aromatic analogs.
Mang, André; Rotthowe, Nils; Beltako, Katawoura; Linseis, Michael; Pauly, Fabian; Winter, Rainer F.; Nanoscale 15 (2023) 5305–5316; doi:10.1039/d2nr05670d

data_1568462
_publ_section_title
;
 Single-molecule conductance studies on quasi- and metallaaromatic
 dibenzoylmethane coordination compounds and their aromatic analogs.
;
_journal_issue                   11
_journal_name_full               Nanoscale
_journal_page_first              5305
_journal_page_last               5316
_journal_paper_doi               10.1039/d2nr05670d
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C25 H27 O2 Rh S2'
_chemical_formula_sum            'C25 H27 O2 Rh S2'
_chemical_formula_weight         526.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4517(3)
_cell_length_b                   23.2662(4)
_cell_length_c                   10.4808(7)
_cell_measurement_reflns_used    15216
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.90
_cell_volume                     2304.78(17)
_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  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_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 0.992
_diffrn_measurement_details
;
 128 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         2.131
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+5.0662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2384
_reflns_number_total             2723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05670d2.cif
_cod_data_source_block           am010
_cod_depositor_comments
'Adding full bibliography for 1568461--1568464.cif.'
_cod_database_code               1568462
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C11-C10 \\sim C13-C12
 with sigma of 0.01
 C16-C17 \\sim C14-C15
 with sigma of 0.01
 C17-C10 \\sim C14-C13
 with sigma of 0.01
 C12-C11 \\sim C15-C16
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) = Uanis(C17)
Uanis(C10) = Uanis(C13)
4. Others
 Fixed Sof: C10(0.5) H10(0.5) C17(0.5) H17(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 C16(0.5) H16A(0.5) H16B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C17(H17), C13(H13), C14(H14)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C16(H16A,H16B), C12(H12A,H12B), C15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C6(H6), C9(H9), C7(H7)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              25473
_olex2_submission_special_instructions 'No special instructions were received'