Synthesis, X-ray characterization, and DFT calculations of gold–nucleobase complexes: on the importance of regium bonds and anion–π interactions
Buils, Jordi; Terrón, Angel; Barceló-Oliver, Miquel; Fiol, Juan Jesús; García-Raso, Angel; Gomila, Rosa M.; Frontera, Antonio; CrystEngComm 27 (2025) 4081–4089; doi:10.1039/D5CE00363F

data_7250456
_publ_section_title
;
 Synthesis, X-ray characterization, and DFT calculations of
 gold--nucleobase complexes: on the importance of regium bonds and
 anion--\p interactions
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4081
_journal_page_last               4089
_journal_paper_doi               10.1039/D5CE00363F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Au Cl4, Cl, 2(C10 H18 N3 O)'
_chemical_formula_sum            'C20 H36 Au Cl5 N6 O2'
_chemical_formula_weight         766.76
_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             2025-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-26 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                84.708(6)
_cell_angle_beta                 86.889(6)
_cell_angle_gamma                72.364(5)
_cell_formula_units_Z            2
_cell_length_a                   6.8686(9)
_cell_length_b                   10.7183(14)
_cell_length_c                   20.600(3)
_cell_measurement_reflns_used    9507
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      4.31
_cell_volume                     1438.6(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78914
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.670
_diffrn_reflns_theta_min         4.312
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.120
_exptl_absorpt_correction_T_max  0.7298
_exptl_absorpt_correction_T_min  0.3307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1727 before and 0.1284 after correction.
The Ratio of minimum to maximum transmission is 0.4531.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         7.536
_refine_diff_density_min         -4.023
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.1083
_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^)+(0.1054P)^2^+69.6708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2842
_refine_ls_wR_factor_ref         0.2851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5008
_reflns_number_total             5198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00363f2.cif
_cod_data_source_block           1_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7250455--7250456.cif.'
_cod_database_code               7250456
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.539
_shelx_estimated_absorpt_t_min   0.110
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Restrained distances
 C9A-C10A = C11A-C12A
 1.5 with sigma of 0.02
 C10A-C11A
 1.5 with sigma of 0.02
 C7-C8A = C9A-C10A = C11A-C12A
 1.5 with sigma of 0.02
 C7-C8 = C9-C10 = C11-C12
 1.5 with sigma of 0.02
 C10A-C12A
 2.5 with sigma of 0.04
 C11A-C9A
 2.5 with sigma of 0.04
3. Rigid bond restraints
 C11A, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C12A \\sim C11A \\sim C10A \\sim C11 \\sim C12 \\sim C10 \\sim C9A \\sim C9
\\sim C8A \\sim C8 \\sim C7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
Uanis(C8') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N1', C7', C8', C9'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C12A, C11A, C10A, C9A, C8A, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C12, C11, C10, C9, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: H7BC(0.75) H7BD(0.75) H7AA(0.25) H7AB(0.25) C8(0.75) H8A(0.75)
 H8B(0.75) C9(0.75) H9A(0.75) H9B(0.75) C10(0.75) H10A(0.75) H10B(0.75)
 C11(0.75) H11A(0.75) H11B(0.75) C12(0.75) H12A(0.75) H12B(0.75) H12C(0.75)
 C9A(0.25) H9AA(0.25) H9AB(0.25) C8A(0.25) H8AA(0.25) H8AB(0.25) C10A(0.25)
 H10C(0.25) H10D(0.25) C11A(0.25) H11C(0.25) H11D(0.25) C12A(0.25) H12D(0.25)
 H12E(0.25) H12F(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C7'(H7'A,H7'B), C8'(H8'A,H8'B), C9'(H9'A,H9'B), C10'(H10E,H10F), C11'(H11E,
 H11F), C7(H7BC,H7BD), C7(H7AA,H7AB), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C9A(H9AA,H9AB), C8A(H8AA,H8AB), C10A(H10C,H10D), C11A(H11C,
 H11D)
7.b Me refined with riding coordinates:
 C12A(H12D,H12E,H12F)
7.c Aromatic/amide H refined with riding coordinates:
 N3'(H3'), C5'(H5'), C6'(H6'), N3(H3), C5(H5), C6(H6)
7.d X=CH2 refined with riding coordinates:
 N4'(H4'A,H4'B), N4(H00A,H00B)
7.e Idealised Me refined as rotating group:
 C12'(H12G,H12H,H12I), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              88378
_olex2_submission_special_instructions 'No special instructions were received'