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_7709722
_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         'C58 H54 Au2 N4, 2(C4 H8 O)'
_chemical_formula_sum            'C66 H70 Au2 N4 O2'
_chemical_formula_weight         1345.19
_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             2021-11-04
_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                 104.188(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3524(3)
_cell_length_b                   18.6578(6)
_cell_length_c                   9.9186(2)
_cell_measurement_reflns_used    46252
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      1.75
_cell_volume                     2754.44(12)
_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 1.71.0.0 (STOE, 2016) X-Area X-Red32 1.63.2.0 (STOE, 2017)'
_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      100.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34907
_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         29.572
_diffrn_reflns_theta_min         1.750
_exptl_absorpt_coefficient_mu    5.369
_exptl_absorpt_correction_T_max  0.5242
_exptl_absorpt_correction_T_min  0.1955
_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.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7686
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0392P)^2^+0.7992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6359
_reflns_number_total             7686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03795a2.cif
_cod_data_source_block           fkp014b
_cod_database_code               7709722
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.239
_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
 C33B-O1A \\sim O1A-C30A \\sim C30A-C31A
 with sigma of 0.02
 C32A-C33B \\sim C32A-C31A
 with sigma of 0.02
 C32A-O1A \\sim C32A-C30A
 with sigma of 0.04
 O1A-C31A \\sim C33B-C30A
 with sigma of 0.04
 C33A-C32B \\sim C32B-C31B \\sim C31B-C30B
 with sigma of 0.02
 O1B-C33A \\sim O1B-C30B
 with sigma of 0.02
 O1B-C32B \\sim O1B-C31B
 with sigma of 0.04
 C32B-C30B \\sim C33A-C31B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1A \\sim C30A \\sim C31A \\sim C32A \\sim C33B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O1B \\sim C30B \\sim C31B \\sim C32B \\sim C33A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1A, C30A, C31A, C32A, C33B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, C30B, C31B, C32B, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1A(0.5) C30A(0.5) H30a(0.5) H30b(0.5) C31A(0.5) H31a(0.5)
 H31b(0.5) C32A(0.5) H32a(0.5) H32b(0.5) C33B(0.5) H33a(0.5) H33b(0.5) O1B(0.5)
 C30B(0.5) H30c(0.5) H30d(0.5) C31B(0.5) H31c(0.5) H31d(0.5) C32B(0.5)
 H32c(0.5) H32d(0.5) C33A(0.5) H33c(0.5) H33d(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C30A(H30a,H30b), C31A(H31a,H31b), C32A(H32a,H32b), C33B(H33a,H33b), C30B(H30c,
 H30d), C31B(H31c,H31d), C32B(H32c,H32d), C33A(H33c,H33d)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C18(H18), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
6.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C22(H22a,H22b,H22c), C29(H29a,H29b,
 H29c)
;
_shelx_res_checksum              87221
_shelx_hkl_checksum              14736
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'