Stepwise alkyne insertion in Au(i) acetylides: influence of the nuclearity.
Cayuela-Castillo, Juan; Fernández-de-Córdova, Francisco J; See, Matthew S.; Fernández, Israel; Ríos, Pablo; Chemical science 16 (2025) 4684–4694; doi:10.1039/d4sc08227c

data_1573909
_publ_section_title
;
 Stepwise alkyne insertion in Au(i) acetylides: influence of the
 nuclearity.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              4684
_journal_page_last               4694
_journal_paper_doi               10.1039/d4sc08227c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C62 H78 Au2 N4 O4'
_chemical_formula_sum            'C62 H78 Au2 N4 O4'
_chemical_formula_weight         1337.21
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.539(2)
_cell_length_b                   12.2149(7)
_cell_length_c                   29.5810(16)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      26.315
_cell_measurement_theta_min      2.433
_cell_volume                     13202.6(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            313267
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.399
_diffrn_reflns_theta_min         2.120
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.482
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0842 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.8263.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       prism
_exptl_crystal_F_000             5344
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene - Pentane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.066
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         13529
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0167P)^2^+104.6856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11555
_reflns_number_total             13529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08227c6.cif
_cod_data_source_block           pr1323b_0ma_a
_cod_depositor_comments
'Adding full bibliography for 1573902--1573910.cif.'
_cod_database_code               1573909
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.663
_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. Rigid bond restraints
 C11, C15, C2, C63
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C37, C50, C58, C51
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C11 \\sim C15 \\sim C2 \\sim C63: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C37 \\sim C58 \\sim C51 \\sim C50: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 C13(H13), C15(H15), C32(H32), C34(H34), C50(H50), C52(H52), C54(H54), C56(H56)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C8(H8), C9(H9), C10(H10), C17(H17), C24(H24), C25(H25),
 C26(H26), C31(H31), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45), C46(H46)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C29(H29A,H29B,
 H29C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C61(H61A,H61B,H61C), C2(H2A,H2B,H2C), C63(H63A,H63B,H63C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8981
_shelx_fab_checksum              72749
_olex2_submission_special_instructions 'No special instructions were received'