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_1568464
_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         '2(C29 H15 B F10 O2 S2), C7 H16'
_chemical_formula_sum            'C65 H46 B2 F20 O4 S4'
_chemical_formula_weight         1420.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.172(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7932(6)
_cell_length_b                   21.5764(9)
_cell_length_c                   32.252(2)
_cell_measurement_reflns_used    21299
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      1.86
_cell_volume                     6094.1(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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 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
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
 360 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            53375
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.366
_diffrn_reflns_theta_min         1.888
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9769
_exptl_absorpt_correction_T_min  0.9112
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       needle
_exptl_crystal_F_000             2888
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: heptane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00137(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         15200
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6459
_reflns_number_total             15200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05670d2.cif
_cod_data_source_block           ambw03
_cod_depositor_comments
'Adding full bibliography for 1568461--1568464.cif.'
_cod_original_cell_volume        6094.1(7)
_cod_database_code               1568464
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.900
_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
 C66-C67 = C67-C68 = C68-C69 = C69-C70 = C70-C71 = C71-C72
 1.52 with sigma of 0.02
 C65-C64 = C64-C63 = C63-C62 = C62-C61 = C61-C60 = C60-C59
 1.52 with sigma of 0.02
 C67-C69 = C69-C71
 2.55 with sigma of 0.04
 C68-C70 = C70-C72
 2.54 with sigma of 0.04
 C66-C68
 2.53 with sigma of 0.04
 C64-C62 = C62-C60
 2.55 with sigma of 0.04
 C63-C61 = C61-C59
 2.54 with sigma of 0.04
 C65-C63
 2.53 with sigma of 0.04
 C66-C67 \\sim C67-C68 \\sim C68-C69 \\sim C69-C70 \\sim C70-C71 \\sim C71-C72
 with sigma of 0.02
 C66-C68 \\sim C68-C70 \\sim C67-C69 \\sim C69-C71 \\sim C70-C72
 with sigma of 0.02
 C65-C63 \\sim C63-C61 \\sim C64-C62 \\sim C62-C60 \\sim C61-C59
 with sigma of 0.02
 C65-C64 \\sim C64-C63 \\sim C63-C62 \\sim C62-C61 \\sim C61-C60 \\sim C60-C59
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C66, C67, C68, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C60, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.5)
 H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5)
 H65C(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) C67(0.5) H67A(0.5) H67B(0.5)
 C68(0.5) H68A(0.5) H68B(0.5) C69(0.5) H69A(0.5) H69B(0.5) C70(0.5) H70A(0.5)
 H70B(0.5) C71(0.5) H71A(0.5) H71B(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,
 H64B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
 C71(H71A,H71B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38), C41(H41), C42(H42),
  C44(H44), C45(H45)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C30(H30A,H30B,H30C), C46(H46A,H46B,
 H46C), C59(H59A,H59B,H59C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C72(H72A,
 H72B,H72C)
;
_shelx_res_checksum              49948
_olex2_submission_special_instructions 'No special instructions were received'