Reactivity of Gold and Copper Acetylide with a Secondary Borane
Thornton, Ragene; French, Kirk; Shuford, Kevin; Martin, Caleb Daniel; Chemical Communications  (2026) –; doi:10.1039/D5CC06957B

data_7135332
_publ_section_title
;
 Reactivity of Gold and Copper Acetylide with a Secondary Borane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC06957B
_journal_year                    2026
_chemical_formula_moiety         'C32 H47 Au B21 P'
_chemical_formula_sum            'C32 H47 Au B21 P'
_chemical_formula_weight         886.979
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2025-07-31
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-25 deposited with the CCDC.	2025-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.988(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4148(1)
_cell_length_b                   16.6168(1)
_cell_length_c                   15.9182(1)
_cell_measurement_reflns_used    36348
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.5590
_cell_measurement_theta_min      2.6830
_cell_volume                     4037.80(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.133a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.133a 64-bit (release 07-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.133a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.9962
_diffrn_measured_fraction_theta_max 0.9917
_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    -21.00  23.00   0.50    3.00    --   42.75 -80.00 -43.00   88
  2  \w    -77.00 -10.00   0.50    3.00    --  -44.00  80.00  80.00  134
  3  \w   -159.00 -85.00   0.50    3.00    --  -88.62 -80.00 -43.00  148
  4  \w    120.00 146.00   0.50    3.00    --  114.01  80.00  80.00   52
  5  \w    114.00 140.00   0.50    3.00    --  114.01 -80.00 -43.00   52
  6  \w     55.00  81.00   0.50    3.00    --  114.01 -80.00 -43.00   52
  7  \w    -36.00 -10.00   0.50    3.00    --  -44.00  38.00-180.00   52
  8  \w   -122.00 -81.00   0.50    3.00    --  -44.00-125.00   0.00   82
  9  \w      0.00  31.00   0.50    3.00    --  -44.00  19.00-180.00   62
 10  \w      0.00  37.00   0.50    3.00    --  -44.00  38.00-180.00   74
 11  \w      2.00  27.00   0.50    3.00    --   50.00  97.00-142.04   50
 12  \w   -154.00 -75.00   0.50    3.00    --  -78.00 -71.00 -99.48  158
 13  \w    -71.00 -44.00   0.50    3.00    --  -78.00 -71.00 -99.48   54
 14  \w    -48.00 -13.00   0.50    3.00    --  -88.62  45.00 -90.00   70
 15  \w    -45.00  -4.00   0.50    3.00    --  -88.62  45.00  30.00   82
 16  \w   -122.00 -96.00   0.50    3.00    --  -88.62  80.00  80.00   52
 17  \w    -85.00 -39.00   0.50    3.00    --  -88.62  80.00  80.00   92
 18  \w     36.00  62.00   0.50    3.00    --  114.01 -94.00 -60.00   52
 19  \w     40.00  65.00   0.50    3.00    --  114.01 -61.00   0.00   50
 20  \w     77.00 102.00   0.50    3.00    --  114.01-111.00 -60.00   50
 21  \w     34.00  59.00   0.50    3.00    --  114.01 -61.00-120.00   50
 22  \w     52.00  99.00   0.50    3.00    --  114.01 -94.00-180.00   94
 23  \w     49.00  75.00   0.50    3.00    --  114.01 -61.00  60.00   52
 24  \w     34.00  59.00   0.50    3.00    --  114.01 -61.00-180.00   50
 25  \w     77.00 109.00   0.50    3.00    --  116.00 -71.00 176.24   64
 26  \w     49.00 158.00   0.50    3.00    --  116.00  25.00 118.49  218
 27  \w     50.00  76.00   0.50    3.00    --  116.00 -80.00  52.75   52
 28  \w     44.00  71.00   0.50    3.00    --  116.00 -80.00 -88.95   54
 29  \w    101.00 149.00   0.50    3.00    --  116.00 -74.00  86.17   96
 30  \w    126.00 155.00   0.50    3.00    --  116.00 -82.00  29.33   58
 31  \w    129.00 155.00   0.50    3.00    --  116.00  23.00-122.93   52
 32  \w     86.00 154.00   0.50    3.00    --  116.00 -80.00 -88.95  136
 33  \w     43.00 117.00   0.50    3.00    --  116.00  23.00-122.93  148
 34  \w     44.00  70.00   0.50    3.00    --  116.00 -71.00 176.24   52
 35  \w     59.00  85.00   0.50    3.00    --  116.00-130.00  94.62   52
 36  \w     57.00 104.00   0.50    3.00    --  116.00 -71.00-118.57   94
 37  \w     50.00  88.00   0.50    3.00    --  116.00 -75.00 -69.47   76
 38  \w     59.00  84.00   0.50    3.00    --  116.00  26.00 -98.61   50
 39  \w    108.00 134.00   0.50    3.00    --  116.00   7.00 115.41   52
 40  \w     40.00  66.00   0.50    3.00    --  116.00 -71.00 167.94   52
 41  \w     45.00  71.00   0.50    3.00    --  116.00   7.00 115.41   52
 42  \w     42.00 129.00   0.50    3.00    --  116.00 -76.00   0.88  174
 43  \w     83.00 114.00   0.50    3.00    --  116.00 -78.00  25.40   62
 44  \w     43.00  69.00   0.50    3.00    --  116.00 -78.00  25.40   52
 45  \w    145.00 177.00   0.50    3.00    --  116.00   4.00  19.67   64
 46  \w     40.00  70.00   0.50    3.00    --  116.00 -72.00  98.31   60
 47  \w     97.00 122.00   0.50    3.00    --  116.00  26.00 -98.61   50
 48  \w    130.00 164.00   0.50    3.00    --  116.00  26.00 -98.61   68
 49  \w     77.00 107.00   0.50    3.00    --  116.00   4.00  19.67   60
 50  \w    113.00 144.00   0.50    3.00    --  116.00  29.00  -1.84   62
 51  \w     47.00  73.00   0.50    3.00    --  116.00 -79.00 -10.65   52
 52  \w    113.00 139.00   0.50    3.00    --  116.00 -79.00 -10.65   52
 53  \w     64.00  89.00   0.50    3.00    --  116.00  29.00  -1.84   50
 54  \w     41.00 113.00   0.50    3.00    --  116.00  14.00  96.97  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148348000
_diffrn_orient_matrix_UB_12      -0.0751032000
_diffrn_orient_matrix_UB_13      0.0529259000
_diffrn_orient_matrix_UB_21      0.0959573000
_diffrn_orient_matrix_UB_22      -0.0253826000
_diffrn_orient_matrix_UB_23      -0.0009845000
_diffrn_orient_matrix_UB_31      0.0274337000
_diffrn_orient_matrix_UB_32      0.0481278000
_diffrn_orient_matrix_UB_33      0.0821425000
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.9962
_diffrn_reflns_Laue_measured_fraction_max 0.9917
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41997
_diffrn_reflns_point_group_measured_fraction_full 0.9962
_diffrn_reflns_point_group_measured_fraction_max 0.9917
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         78.36
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.133a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             1742.050
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.351
_refine_diff_density_max         2.4452
_refine_diff_density_min         -1.2693
_refine_diff_density_rms         0.1385
_refine_ls_d_res_high            0.7871
_refine_ls_d_res_low             15.2652
_refine_ls_goodness_of_fit_ref   1.0311
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0311
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+10.7471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8565
_reflns_number_total             8605
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc06957b2.cif
_cod_data_source_block           CDM922_RT_RG_auto
_cod_original_cell_volume        4037.80(5)
_cod_database_code               7135332
_chemical_oxdiff_formula         PAuB21C32H42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
2.b Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C6(H6a,H6b,H6c)
2.c Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8a), B9(H9), B10(H10a),
 B11(H11a), B12(H12a), B13(H13a), B14(H14a), B15(H15), B16(H16a), B17(H17a),
 B18(H18a), B19(H19a), B20(H20a), B21(H21)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 16.077
_oxdiff_exptl_absorpt_empirical_full_min 0.514