Coordination complexes of P<sup>III</sup>-doped heterobuckybowls and their applications in catalysis.
Feng, Lijun; Hua, Xinqiang; Shang, Jihai; Shao, Xiangfeng; Organic & biomolecular chemistry 23 (2025) 665–672; doi:10.1039/d4ob01737d

data_7160252
_publ_section_title
;
 Coordination complexes of P<sup>III</sup>-doped heterobuckybowls and
 their applications in catalysis.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              665
_journal_page_last               672
_journal_paper_doi               10.1039/d4ob01737d
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C48 H59 Au Cl O6 P S2'
_chemical_formula_sum            'C48 H59 Au Cl O6 P S2'
_chemical_formula_weight         1059.45
_chemical_name_common            4-AuCl
_chemical_name_systematic        4-AuCl
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                106.6663(17)
_cell_angle_beta                 102.9809(16)
_cell_angle_gamma                114.312(2)
_cell_formula_units_Z            4
_cell_length_a                   16.7310(3)
_cell_length_b                   17.9089(4)
_cell_length_c                   19.0611(3)
_cell_measurement_reflns_used    32370
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      76.0910
_cell_measurement_theta_min      2.6180
_cell_volume                     4586.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_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    102.00 169.50   0.75    0.40    --  104.25  45.00 -60.00   90
  2  \w     82.00 170.50   0.75    0.40    --  104.25 125.00  30.00  118
  3  \w     89.00 138.50   0.75    0.40    --  104.25 104.00 170.00   66
  4  \w    143.00 169.25   0.75    0.40    --  104.25  61.00 120.00   35
  5  \w     88.00 134.50   0.75    0.40    --  104.25  61.00 120.00   62
  6  \w    -23.00  23.50   0.75    0.12    --   46.32 -19.00 -90.00   62
  7  \w     32.00  60.50   0.75    0.40    --  104.25 -61.00-120.00   38
  8  \w     45.00  72.00   0.75    0.40    --  104.25 -61.00 -60.00   36
  9  \w     34.00  73.00   0.75    0.40    --  104.25 -61.00  30.00   52
 10  \w     34.00  67.00   0.75    0.40    --  104.25 -61.00  60.00   44
 11  \w     42.00  67.50   0.75    0.40    --  104.25 -61.00 120.00   34
 12  \w     36.00  73.50   0.75    0.40    --  104.25 -61.00 150.00   50
 13  \w     54.00 105.00   0.75    0.40    --  104.25 -94.00  90.00   68
 14  \w     33.00 101.25   0.75    0.40    --  104.25-125.00  90.00   91
 15  \w     41.00 111.50   0.75    0.40    --  104.25-125.00   0.00   94
 16  \w     87.00 112.50   0.75    0.40    --  104.25-125.00 120.00   34
 17  \w     59.00  92.00   0.75    0.40    --  104.25-125.00 -30.00   44
 18  \w     65.00 107.00   0.75    0.40    --  104.25-104.00  69.00   56
 19  \w     59.00 109.25   0.75    0.40    --  104.25-113.00-113.99   67
 20  \w     67.00 103.00   0.75    0.40    --  104.25 -94.00-150.00   48
 21  \w     19.00  93.25   0.75    0.12    --   46.32-125.00-180.00   99
 22  \w     32.00  82.25   0.75    0.40    --  104.25-125.00-150.00   67
 23  \w     40.00 102.25   0.75    0.40    --  104.25-125.00-120.00   83
 24  \w     18.00  43.50   0.75    0.12    --   46.32-104.00  69.00   34
 25  \w    -36.00  27.00   0.75    0.12    --  -46.32  37.00 -30.00   84
 26  \w    -68.00 -20.75   0.75    0.12    --  -46.32  77.00  90.00   63
 27  \w    -40.00  22.25   0.75    0.12    --  -46.32  37.00  90.00   83
 28  \w     -6.00  26.25   0.75    0.12    --  -46.32  77.00  90.00   43
 29  \w     -7.00  27.50   0.75    0.12    --  -46.32  37.00-150.00   46
 30  \w    -40.00 -10.00   0.75    0.12    --  -46.32  37.00-150.00   40
 31  \w   -112.00 -68.50   0.75    0.40    -- -102.00 125.00 -30.00   58
 32  \w   -109.00 -82.00   0.75    0.40    -- -102.00 116.00 -25.85   36
 33  \w    -67.00 -31.00   0.75    0.40    -- -102.00 116.00 -25.85   48
 34  \w    -67.00 -29.50   0.75    0.40    -- -102.00  61.00 -90.00   50
 35  \w    -69.00   0.00   0.75    0.12    --  -46.32 104.00 170.00   92
 36  \w   -106.00 -68.50   0.75    0.40    -- -102.00 104.00 170.00   50
 37  \w    -69.00 -39.75   0.75    0.40    -- -102.00  61.00 150.00   39
 38  \w   -171.00-144.75   0.75    0.40    -- -102.00 -61.00 150.00   35
 39  \w   -174.00 -97.50   0.75    0.40    -- -102.00 -45.00 120.00  102
 40  \w   -111.00 -85.50   0.75    0.40    -- -102.00 -61.00 150.00   34
 41  \w   -173.00-137.00   0.75    0.40    -- -102.00 -30.00 -90.00   48
 42  \w   -134.00 -89.75   0.75    0.40    -- -102.00 -30.00 -90.00   59
 43  \w   -174.00-141.00   0.75    0.40    -- -102.00 -94.00 -90.00   44
 44  \w   -165.00 -75.00   0.75    0.40    -- -102.00-125.00-120.00  120
 45  \w   -115.00 -85.75   0.75    0.12    --  -46.32-125.00-150.00   39
 46  \w   -119.00 -77.00   0.75    0.12    --  -46.32-125.00-180.00   56
 47  \w   -132.00-100.50   0.75    0.40    -- -102.00 -94.00 -90.00   42
 48  \w   -138.00 -88.50   0.75    0.40    -- -102.00-104.00  69.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0189507000
_diffrn_orient_matrix_UB_12      0.0735771000
_diffrn_orient_matrix_UB_13      0.0441732000
_diffrn_orient_matrix_UB_21      -0.0843668000
_diffrn_orient_matrix_UB_22      -0.0323558000
_diffrn_orient_matrix_UB_23      -0.0765451000
_diffrn_orient_matrix_UB_31      -0.0677607000
_diffrn_orient_matrix_UB_32      -0.0666147000
_diffrn_orient_matrix_UB_33      0.0245732000
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            66554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.445
_diffrn_reflns_theta_min         2.631
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       needle
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         18478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0533P)^2^+4.2056P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15360
_reflns_number_total             18478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01737d2.cif
_cod_data_source_block           4-AuCl
_cod_depositor_comments
'Adding full bibliography for 7160252--7160260.cif.'
_cod_original_cell_volume        4585.98(18)
_cod_database_code               7160252
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H01E(0.55) H01F(0.55) H01G(0.45) H01H(0.45) H02M(0.45) H02N(0.45)
 H02K(0.55) H02L(0.55) C033(0.55) H03H(0.55) H03I(0.55) H03J(0.55) C036(0.45)
 H03M(0.45) H03N(0.45) C3(0.55) H3A(0.55) H3B(0.55) C7(0.45) H7A(0.45)
 H7B(0.45) H7C(0.45)
3.a Secondary CH2 refined with riding coordinates:
 C012(HA,HB), C018(HD,HE), C01A(HF,HG), C01G(HH,HI), C01K(HK,HL), C01L(H01A,
 H01B), C01M(H01C,H01D), C01Q(HM,HN), C01T(H01E,H01F), C01T(H01G,H01H), C01W(HP,
 HQ), C020(HU,HV), C023(H02A,H02B), C024(HX,HY), C027(HZ,H1), C028(H2,H3),
 C02B(H02C,H02D), C02D(H02E,H02F), C02E(H7,H8), C02F(H02G,H02H), C02H(H02I,
 H02J), C02I(H12,H13), C02J(H02M,H02N), C02J(H02K,H02L), C02K(H14,H15),
 C02L(H02O,H02P), C02M(H16,H17), C02N(H18,H19), C02Q(H23,H24), C02T(H02T,H02U),
 C02W(H02Z,H27), C030(H03A,H03B), C032(H03F,H03G), C034(H31,H32), C035(H03K,
 H03L), C036(H03M,H03N), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C00Y(H), C017(HC), C01H(HJ), C01O(H01O), C01R(HO), C021(HW), C02P(H02Q),
 C02R(H02R), C02S(H02S), C02Y(H02)
3.c Idealised Me refined as rotating group:
 C01Y(HR,HS,HT), C02A(H4,H5,H6), C02G(H9,H10,H11), C02O(H20,H21,H22),
 C02U(H02V,H02W,H02X), C02V(H02Y,H25,H26), C02X(H28,H29,H30), C031(H03C,H03D,
 H03E), C033(H03H,H03I,H03J), C037(H33,H34,H35), C038(H03O,H03P,H03Q), C4(H4A,
 H4B,H4C), C7(H7A,H7B,H7C)
;
_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 1.983
_oxdiff_exptl_absorpt_empirical_full_min 0.686