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_1575997
_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         'C64 H92 Au4 S8'
_chemical_formula_sum            'C64 H92 Au4 S8'
_chemical_formula_weight         1905.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1z0w95
_audit_creation_date             2016-11-30
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.431(3)
_cell_length_b                   37.714(4)
_cell_length_c                   13.8529(10)
_cell_measurement_reflns_used    12667
_cell_measurement_temperature    99.91(19)
_cell_measurement_theta_max      75.3710
_cell_measurement_theta_min      3.1300
_cell_volume                     14331(2)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.91(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_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    -64.00  27.00   1.00   20.00    --  -38.50  57.00 -90.00   91
  2  \w   -115.00  -6.00   1.00   20.00    --  -38.50 -19.00-180.00  109
  3  \w    -58.00  23.00   1.00   20.00    --  -38.50  37.00-150.00   81
  4  \w     13.00  80.00   1.00   20.00    --   43.20  77.00 -30.00   67
  5  \w     78.00 114.00   1.00   20.00    --   43.20  77.00 -90.00   36
  6  \w     13.00  94.00   1.00   20.00    --   43.20  77.00-150.00   81
  7  \w     15.00  43.00   1.00   20.00    --   43.20  77.00 -90.00   28
  8  \w     58.00 126.00   1.00   20.00    --   43.20 178.00  90.00   68
  9  \w     55.00 127.00   1.00   20.00    --   43.20-178.00-180.00   72
 10  \w     65.00 115.00   1.00   20.00    --   43.20  77.00 150.00   50
 11  \w     16.00  70.00   1.00   20.00    --   43.20  77.00  30.00   54
 12  \w     24.00  96.00   1.00   20.00    --   43.20  57.00 -60.00   72
 13  \w     13.00  48.00   1.00   20.00    --   43.20  77.00  90.00   35
 14  \w     25.00  60.00   1.00   20.00    --   43.20  37.00  90.00   35
 15  \w     62.00  88.00   1.00   20.00    --   43.20  37.00  90.00   26
 16  \w     18.00 112.00   1.00   20.00    --   43.20  57.00 120.00   94
 17  \w     13.00  62.00   1.00   20.00    --   43.20  77.00 150.00   49
 18  \w     81.00 173.00   1.00   80.00    --  111.00  77.00 -65.50   92
 19  \w    127.00 168.00   1.00   80.00    --  111.00  65.00 127.57   41
 20  \w     82.00 107.00   1.00   80.00    --  111.00  76.00 141.61   25
 21  \w     84.00 123.00   1.00   80.00    --  111.00  65.00 127.57   39
 22  \w     81.00 177.00   1.00   80.00    --  111.00  77.00  90.00   96
 23  \w     45.00  98.00   1.00   80.00    --  111.00 -94.00  90.00   53
 24  \w     82.00 153.00   1.00   80.00    --  111.00  72.00 -13.15   71
 25  \w     81.00 107.00   1.00   80.00    --  111.00  77.00 -90.00   26
 26  \w     43.00  88.00   1.00   80.00    --  111.00 -61.00-120.00   45
 27  \w    101.00 136.00   1.00   80.00    --  111.00 -61.00-120.00   35
 28  \w     82.00 108.00   1.00   80.00    --  111.00  73.00-129.82   26
 29  \w     85.00 111.00   1.00   80.00    --  111.00  61.00 120.00   26
 30  \w     85.00 176.00   1.00   80.00    --  111.00  61.00 -90.00   91
 31  \w     88.00 115.00   1.00   80.00    --  111.00  49.00  83.68   27
 32  \w     81.00 107.00   1.00   80.00    --  111.00  77.00 120.00   26
 33  \w    116.00 174.00   1.00   80.00    --  111.00  77.00  60.00   58
 34  \w    126.00 178.00   1.00   80.00    --  111.00  75.00-163.33   52
 35  \w     38.00 108.00   1.00   80.00    --  111.00 -94.00  30.00   70
 36  \w     40.00 141.00   1.00   80.00    --  111.00 -77.00 120.00  101
 37  \w     81.00 107.00   1.00   80.00    --  111.00  75.00-163.33   26
 38  \w     87.00 113.00   1.00   80.00    --  111.00  52.00  53.04   26
 39  \w     81.00 177.00   1.00   80.00    --  111.00  77.00   0.00   96
 40  \w     81.00 107.00   1.00   80.00    --  111.00  77.00  30.00   26
 41  \w    114.00 172.00   1.00   80.00    --  111.00  77.00  30.00   58
 42  \w     81.00 107.00   1.00   80.00    --  111.00  77.00  60.00   26
 43  \w     85.00 111.00   1.00   80.00    --  111.00  61.00 -60.00   26
 44  \w     85.00 121.00   1.00   80.00    --  111.00  61.00 -30.00   36
 45  \w    152.00 178.00   1.00   80.00    --  111.00  77.00 -60.00   26
 46  \w     85.00 154.00   1.00   80.00    --  111.00  61.00 150.00   69
 47  \w     81.00 113.00   1.00   80.00    --  111.00  77.00 -30.00   32
 48  \w     81.00 166.00   1.00   80.00    --  111.00  77.00 150.00   85
 49  \w     81.00 108.00   1.00   80.00    --  111.00  77.00 -60.00   27
 50  \w     85.00 111.00   1.00   80.00    --  111.00  61.00  60.00   26
 51  \w     82.00 108.00   1.00   80.00    --  111.00  72.00 170.40   26
 52  \w     81.00 107.00   1.00   80.00    --  111.00  77.00-120.00   26
 53  \w     85.00 129.00   1.00   80.00    --  111.00  61.00  90.00   44
;
_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      -0.0040530000
_diffrn_orient_matrix_UB_12      0.0070377000
_diffrn_orient_matrix_UB_13      -0.1093881000
_diffrn_orient_matrix_UB_21      -0.0057168000
_diffrn_orient_matrix_UB_22      0.0399490000
_diffrn_orient_matrix_UB_23      0.0197434000
_diffrn_orient_matrix_UB_31      0.0557689000
_diffrn_orient_matrix_UB_32      0.0046413000
_diffrn_orient_matrix_UB_33      -0.0039885000
_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  0.1783
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            159865
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.180
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.482
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.319
_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    1.767
_exptl_crystal_description       needle
_exptl_crystal_F_000             7360
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.008
_refine_diff_density_max         6.938
_refine_diff_density_min         -2.810
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         13974
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7608
_reflns_number_total             13974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06444a2.cif
_cod_data_source_block           glatthor42
_cod_database_code               1575997
_chemical_oxdiff_formula         C64H89Au4S8
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_exptl_crystal_mounting_method mounted
_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 1.643
_oxdiff_exptl_absorpt_empirical_full_min 0.645
_shelx_res_checksum              99872
_shelx_shelxl_version_number     2014/7