Systematic investigation of the influence of electronic substituents on dinuclear gold(i) amidinates: synthesis, characterisation and photoluminescence studies
Krätschmer, Frederic; Gui, Xin; Gamer, Michael T.; Klopper, Wim; Roesky, Peter W.; Dalton Transactions  (2022) –; doi:10.1039/D1DT03795A

data_7709720
_publ_section_title
;
 Systematic investigation of the influence of electronic substituents on
 dinuclear gold(i) amidinates: synthesis, characterisation and
 photoluminescence studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03795A
_journal_year                    2022
_chemical_formula_moiety
'C38 H46 Au2 N4 S4, 0.333[C7H8], 0.333[C4H8O]'
_chemical_formula_sum            'C38 H46 Au2 N4 S4'
_chemical_formula_weight         1080.96
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2022-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   32.8046(17)
_cell_length_b                   32.8046(17)
_cell_length_c                   20.4318(12)
_cell_measurement_reflns_used    36777
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.11
_cell_volume                     19041.7(18)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.161.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.0.0 (STOE, 2020)
X-Area LANA 1.78.0.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_details
;
 338 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_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  0.0904
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19962
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.850
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.153
_exptl_absorpt_correction_T_max  0.0008
_exptl_absorpt_correction_T_min  0.0001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens 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, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             9432
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1245P)^2^+60.7006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2172
_refine_ls_wR_factor_ref         0.2675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2844
_reflns_number_total             6132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03795a2.cif
_cod_data_source_block           fkm072tolsv
_cod_original_cell_volume        19042(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7709720
_shelx_shelxl_version_number     2018/3
_audit_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_audit_contact_letter
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C10
 2.82 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S1 \\sim C10: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N1 \\sim N2 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
4.a Me refined with riding coordinates:
 C10(H2A,H2B,H2C), C19(H14A,H14B,H14C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H5), C6(H6), C4(H1), C13(H8), C15(H9)
4.c Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3), C11(C12,C13,C14,C15,C16)
4.d Idealised Me refined as rotating group:
 C8(H00A,H00B,H00C), C9(H00D,H00E,H00F), C17(H12A,H12B,H12C), C18(H13A,H13B,
 H13C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 546 electrons were 
found in a volume of 2925A^3 in 1 void per unit cell. 
This is consistent with the presence of 0.333 molecules
of toluene and 0.333 molecules of THF per Formula Unit 
which account for 540 electrons per unit cell.
The solvent molecules are completely disordered along
channel like voids. Content was optimized based on
NMR studies.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55493
_shelx_hkl_checksum              74896
_shelx_fab_checksum              39131
_olex2_submission_special_instructions 'No special instructions were received'