Trapping Carbon Suboxide with a Carbene and Isolation of the Carbene-stabilized Carbon Suboxide Dimer
George, Tanner; Johnson, Erin R.; Masuda, Jason Douglas; Chemical Science  (2025) –; doi:10.1039/D5SC06444A

data_1575996
_publ_section_title
;
 Trapping Carbon Suboxide with a Carbene and Isolation of the
 Carbene-stabilized Carbon Suboxide Dimer
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC06444A
_journal_year                    2025
_chemical_formula_moiety         'C24 H42 Au6 S12, C8 H14 Au2 S4'
_chemical_formula_sum            'C32 H56 Au8 S16'
_chemical_formula_weight         2529.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1z0w73
_audit_creation_date             2016-09-15
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2018-01-19 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.056(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9729(3)
_cell_length_b                   12.1142(2)
_cell_length_c                   16.6245(4)
_cell_measurement_reflns_used    8969
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.1970
_cell_measurement_theta_min      3.6030
_cell_volume                     2717.44(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -105.00 -47.00   1.00   10.00    --  -38.50-178.00-120.00   58
  2  \w   -110.00 -23.00   1.00   10.00    --  -38.50 -37.00 120.00   87
  3  \w    -71.00  37.00   1.00   10.00    --  -38.50  19.00 -60.00  108
  4  \w     79.00 122.00   1.00   10.00    --   42.95 178.00   0.00   43
  5  \w      1.00  82.00   1.00   10.00    --   42.95 -99.00  90.00   81
  6  \w    120.00 163.00   1.00   38.50    --  111.00  30.00 120.00   43
  7  \w     42.00  76.00   1.00   38.50    --  111.00-125.00   0.00   34
  8  \w     60.00 141.00   1.00   38.50    --  111.00 -77.00-150.00   81
  9  \w     46.00 132.00   1.00   38.50    --  111.00 -45.00  30.00   86
 10  \w    107.00 132.00   1.00   38.50    --  111.00 -45.00-150.00   25
 11  \w     41.00 122.00   1.00   38.50    --  111.00-125.00-120.00   81
 12  \w     46.00  77.00   1.00   38.50    --  111.00 -45.00 120.00   31
 13  \w     85.00 127.00   1.00   38.50    --  111.00 -45.00 120.00   42
 14  \w     41.00 131.00   1.00   38.50    --  111.00 -45.00 -60.00   90
 15  \w     42.00  75.00   1.00   38.50    --  111.00 -45.00-150.00   33
 16  \w     97.00 122.00   1.00   38.50    --  111.00-125.00 -30.00   25
 17  \w     41.00  70.00   1.00   38.50    --  111.00-125.00 -30.00   29
 18  \w     85.00 120.00   1.00   38.50    --  111.00-125.00-180.00   35
 19  \w     80.00 107.00   1.00   38.50    --  111.00 -94.00 -30.00   27
 20  \w     42.00  67.00   1.00   38.50    --  111.00-125.00  90.00   25
 21  \w     67.00  94.00   1.00   38.50    --  111.00 -94.00-180.00   27
 22  \w     48.00 119.00   1.00   38.50    --  111.00-125.00  60.00   71
 23  \w     28.00 178.00   1.00   38.50    --  111.00   0.00 -90.00  150
 24  \w     63.00 119.00   1.00   38.50    --  111.00 -77.00  30.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0116532000
_diffrn_orient_matrix_UB_12      0.1221371000
_diffrn_orient_matrix_UB_13      0.0263540000
_diffrn_orient_matrix_UB_21      -0.0105096000
_diffrn_orient_matrix_UB_22      0.0338958000
_diffrn_orient_matrix_UB_23      -0.0912423000
_diffrn_orient_matrix_UB_31      -0.1131024000
_diffrn_orient_matrix_UB_32      0.0095092000
_diffrn_orient_matrix_UB_33      -0.0139720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22206
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.347
_diffrn_reflns_theta_min         3.649
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    45.457
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.034
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0433P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4624
_reflns_number_total             5384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06444a2.cif
_cod_data_source_block           glatthor20
_cod_database_code               1575996
_chemical_oxdiff_formula         'C4 H6 Au S2'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_date_sample_data_collection 2016-09-12
_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:
 C2(H2), C6(H6), C10(H10), C14(H14)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.761
_oxdiff_exptl_absorpt_empirical_full_min 0.632
_shelx_res_checksum              49592
_shelxl_version_number           2013-2