Unusually short unsupported Au(III)⋯Au(III) aurophilic contacts in emissive lanthanide tetracyanoaurate(III) complexes.
Karpiuk, Thomas E.; Mahato, Samyadeb; Storr, Tim; Leznoff, Daniel B.; Chemical communications (Cambridge, England) 60 (2024) 3914–3917; doi:10.1039/d4cc00468j

data_7132874
_publ_section_title
;
 Unusually short unsupported Au(III)&#x22ef;Au(III) aurophilic contacts in
 emissive lanthanide tetracyanoaurate(III) complexes.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3914
_journal_page_last               3917
_journal_paper_doi               10.1039/d4cc00468j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C40 H32 Ce N8 O8, 3(C4 Au N4), 1.199(H2 O)'
_chemical_formula_sum            'C52 H34.4 Au3 Ce N20 O9.2'
_chemical_formula_weight         1817.59
_chemical_name_systematic
'tetrakis(N,N'-dioxide-2,2'-bipyridyl)cerium(III) tetracyanoaurate(III) hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   isomor
_audit_creation_date             2023-09-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-10 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2203(7)
_cell_length_b                   23.8559(8)
_cell_length_c                   23.9799(9)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100.04
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      2.409
_cell_volume                     11567.3(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.04
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'Pinhole collimator'
_diffrn_radiation_detector
'Bruker Photon II 14 charge-integrating pixel array (CPAD) area detector'
_diffrn_radiation_monochromator  'Horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            107468
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.570
_diffrn_source                   'Sealed tube'
_diffrn_source_type
'Sealed X-ray tube with a TRIUMPH monochromator'
_exptl_absorpt_coefficient_mu    8.431
_exptl_absorpt_correction_T_max  0.1864
_exptl_absorpt_correction_T_min  0.1176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2022) was used for absorption correction.
wR2(int) was 0.0867 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.6309.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6840
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.085
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         13275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+11.1533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10110
_reflns_number_total             13275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00468j2.cif
_cod_data_source_block           Ce_4bipyO2_3AuCN4
_cod_depositor_comments
'Adding full bibliography for 7132871--7132874.cif.'
_cod_original_formula_sum        'C52 H34.40 Au3 Ce N20 O9.20'
_cod_database_code               7132874
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.270
_shelx_estimated_absorpt_t_min   0.159
_exptl_absorpt_special_details
;
Additional spherical absorption correction applied:
mu*crystal_size_min = 1.3
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O10)=Sof(H10A)=Sof(H10B)=FVAR(1)
3.a Free rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49), C50(H50),
  C51(H51), C52(H52)
;
_shelx_res_checksum              98836
_shelx_hkl_checksum              91729
_olex2_submission_special_instructions 'No special instructions were received'