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_7709723
_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         'C42 H46 Au2 N4 O8, 1[C7H8]'
_chemical_formula_sum            'C42 H46 Au2 N4 O8'
_chemical_formula_weight         1128.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                83.032(4)
_cell_angle_beta                 78.583(4)
_cell_angle_gamma                83.304(4)
_cell_formula_units_Z            1
_cell_length_a                   7.1610(3)
_cell_length_b                   12.6256(6)
_cell_length_c                   12.9627(7)
_cell_measurement_reflns_used    20580
_cell_measurement_temperature    160
_cell_measurement_theta_max      31.75
_cell_measurement_theta_min      2.18
_cell_volume                     1135.13(10)
_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      160
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
 717 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optics'
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15857
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.709
_diffrn_reflns_theta_min         2.175
_diffrn_source                   'Mo GeniX 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.506
_exptl_absorpt_correction_T_max  0.0019
_exptl_absorpt_correction_T_min  0.0007
_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    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0227P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5763
_reflns_number_total             6716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03795a2.cif
_cod_data_source_block           fkp050a
_cod_database_code               7709723
_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. Uiso/Uaniso restraints and constraints
O3A \\sim O4A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A
\\sim C18A \\sim C19A \\sim C20A \\sim C21A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O3B \\sim O4B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C17B
\\sim C18B \\sim C19B \\sim C20B \\sim C21B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C21A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C12B) = Uanis(C12A)
Uanis(C13B) = Uanis(C13A)
3. Others
 Fixed Sof: O3B(0.5) O4B(0.5) C12B(0.5) C17B(0.5) C16B(0.5) H16B(0.5)
 C15B(0.5) C14B(0.5) H14B(0.5) C13B(0.5) C18B(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C19B(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20B(0.5) C21B(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) O3A(0.5) O4A(0.5) C12A(0.5) C17A(0.5) C16A(0.5)
 H16A(0.5) C15A(0.5) C14A(0.5) H14A(0.5) C13A(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20A(0.5)
 C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C16B(H16B), C14B(H14B), C16A(H16A), C14A(H14A)
4.b Fitted hexagon refined as free rotating group:
 C12B(C17B,C16B,C15B,C14B,C13B), C12A(C17A,C16A,C15A,C14A,C13A)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C18B(H18A,H18B,H18C),
 C19B(H19A,H19B,H19C), C21B(H21A,H21B,H21C), C18A(H18D,H18E,H18F), C19A(H19D,
 H19E,H19F), C21A(H21D,H21E,H21F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 43 electrons were 
found in a volume of 163 A^3 in 1 void per unit cell. 
This is consistent with the presence of a multiple 
disordered molecule of Toluene unit cell, which 
account for 50 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51496
_shelx_hkl_checksum              95558
_shelx_fab_checksum              4156
_olex2_submission_special_instructions 'No special instructions were received'