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_1573906
_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         'C41 H47 Au N2 O4, C7 H8'
_chemical_formula_sum            'C48 H55 Au N2 O4'
_chemical_formula_weight         920.90
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.094(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4242(9)
_cell_length_b                   13.8027(7)
_cell_length_c                   18.9461(10)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      30.017
_cell_measurement_theta_min      2.391
_cell_volume                     4553.0(4)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            164776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.532
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.273
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0741 after correction.
The Ratio of minimum to maximum transmission is 0.6960.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         13925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0130P)^2^+9.2867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10708
_reflns_number_total             13925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08227c6.cif
_cod_data_source_block           pr0124a_0m
_cod_depositor_comments
'Adding full bibliography for 1573902--1573910.cif.'
_cod_database_code               1573906
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.440
_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.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C13(H13), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C20(H20), C19(H19),
 C18(H18), C3(H3), C2(H2), C8(H8), C7(H7), C6(H6), C45(H45), C44(H44), C43(H43),
  C46(H46), C47(H47)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C24(H24A,H24B,H24C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              45518
_olex2_submission_special_instructions 'No special instructions were received'