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_7160255
_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 Te2'
_chemical_formula_sum            'C48 H59 Au Cl O6 P Te2'
_chemical_formula_weight         1250.53
_chemical_name_common            6-AuCl
_chemical_name_systematic        6-AuCl
_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'
_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                90
_cell_angle_beta                 90.7583(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.95628(4)
_cell_length_b                   33.13649(19)
_cell_length_c                   29.23546(13)
_cell_measurement_reflns_used    36912
_cell_measurement_temperature    149.99(11)
_cell_measurement_theta_max      75.7870
_cell_measurement_theta_min      2.0110
_cell_volume                     9644.41(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.945
_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    -29.00  33.00   0.50    0.09    --  -43.05  19.00 -30.00  124
  2  \w    -34.00   3.00   0.50    0.09    --   43.05 -19.00 -90.00   74
  3  \w    -27.00  -2.00   0.50    0.09    --   43.05 -19.00 -30.00   50
  4  \w     36.00  86.00   0.50    0.38    --  109.26 -94.00  90.00  100
  5  \w     54.00  98.00   0.50    0.38    --  109.26-117.00  87.00   88
  6  \w     46.00 111.00   0.50    0.38    --  109.26-125.00 150.00  130
  7  \w     53.00  92.00   0.50    0.09    --   43.05-117.00  87.00   78
  8  \w     40.00  66.00   0.50    0.38    --  109.26 -61.00 120.00   52
  9  \w     35.00  68.00   0.50    0.38    --  109.26 -61.00 150.00   66
 10  \w     98.00 172.00   0.50    0.38    --  109.26  45.00 -30.00  148
 11  \w     74.00 154.00   0.50    0.38    --  109.26 160.00 -33.00  160
 12  \w     62.00  87.00   0.50    0.09    --   43.05 160.00 -33.00   50
 13  \w    104.00 129.00   0.50    0.38    --  109.26 117.00 174.00   50
 14  \w    -37.00  23.00   0.50    0.09    --   43.05 -19.00-180.00  120
 15  \w     76.00 101.00   0.50    0.09    --   43.05-160.00 -64.00   50
 16  \w     61.00  86.00   0.50    0.38    --  109.26-160.00 -64.00   50
 17  \w    -80.00 -55.00   0.50    0.09    --  -43.05 117.00 174.00   50
 18  \w    -54.00 -24.00   0.50    0.38    -- -100.00  45.00  60.00   60
 19  \w    -53.00 -26.00   0.50    0.38    -- -100.00  45.00   0.00   54
 20  \w    -51.00 -25.00   0.50    0.38    -- -100.00  45.00 -30.00   52
 21  \w    -52.00 -24.00   0.50    0.38    -- -100.00  45.00  30.00   56
 22  \w    -54.00 -24.00   0.50    0.38    -- -100.00  45.00 120.00   60
 23  \w    -54.00 -28.00   0.50    0.38    -- -100.00  45.00 150.00   52
 24  \w    -60.00 -26.00   0.50    0.38    -- -100.00 125.00  90.00   68
 25  \w    -91.00 -66.00   0.50    0.38    -- -100.00 117.00 174.00   50
 26  \w   -111.00 -81.00   0.50    0.38    -- -100.00 125.00  90.00   60
 27  \w   -111.00 -86.00   0.50    0.38    -- -100.00 160.00 -33.00   50
 28  \w    -74.00 -49.00   0.50    0.38    -- -100.00  61.00-180.00   50
 29  \w    -52.00 -27.00   0.50    0.38    -- -100.00  45.00-180.00   50
 30  \w   -119.00 -81.00   0.50    0.38    -- -100.00 -45.00 -90.00   76
 31  \w   -114.00 -83.00   0.50    0.09    --  -43.05-160.00 -64.00   62
 32  \w   -132.00-107.00   0.50    0.38    -- -100.00-160.00 -64.00   50
 33  \w   -172.00 -83.00   0.50    0.38    -- -100.00-125.00  60.00  178
 34  \w   -155.00-130.00   0.50    0.38    -- -100.00-117.00  87.00   50
 35  \w   -176.00-132.00   0.50    0.38    -- -100.00 -45.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0001215000
_diffrn_orient_matrix_UB_12      -0.0303243000
_diffrn_orient_matrix_UB_13      -0.0399413000
_diffrn_orient_matrix_UB_21      0.0290673000
_diffrn_orient_matrix_UB_22      0.0346171000
_diffrn_orient_matrix_UB_23      -0.0336391000
_diffrn_orient_matrix_UB_31      0.1519752000
_diffrn_orient_matrix_UB_32      -0.0066137000
_diffrn_orient_matrix_UB_33      0.0071198000
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            74034
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.061
_diffrn_reflns_theta_min         2.015
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.723
_exptl_crystal_description       needle
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.128
_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     1230
_refine_ls_number_reflns         19062
_refine_ls_number_restraints     1572
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+32.2274P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17069
_reflns_number_total             19062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01737d2.cif
_cod_data_source_block           6-AuCl
_cod_depositor_comments
'Adding full bibliography for 7160252--7160260.cif.'
_cod_database_code               7160255
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C12-C02Z = C02Z-C20
 1.54 with sigma of 0.02
 C02Z-C20 = C20-C13
 1.54 with sigma of 0.02
 C02I-C02P = C02P-C9
 1.54 with sigma of 0.02
 C02P-C9 = C9-C24
 1.54 with sigma of 0.02
 C17-C8 = C8-C11
 1.54 with sigma of 0.02
 C8-C11 = C11-C24
 1.54 with sigma of 0.02
 C02Y-C22 = C22-C97
 1.54 with sigma of 0.02
 C12-C20
 2.507 with sigma of 0.04
 C02Z-C13
 2.507 with sigma of 0.04
 C8-C24
 2.507 with sigma of 0.04
 C17-C11
 2.507 with sigma of 0.04
 C02I-C9
 2.507 with sigma of 0.04
 C02P-C24
 2.507 with sigma of 0.04
 C02Y-C97
 2.507 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C01T) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C01N) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C022) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C027) \\sim Ueq,
Uanis(C0) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(C02A) \\sim Ueq, Uanis(O7) \\sim Ueq,
Uanis(O7A) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C02I) \\sim Ueq, Uanis(C02P) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C02Y) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C97) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C12, C02Z, C13, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Te, C16, Te1, C01N, O7, C01T, C022, C027, H20A, C029, C9, C02A, C02I, C22,
 C02P, C02Y, C20, H20B, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C24, C17, C02S, C18, C8, Te1A, C0, C7, C3, C11, TeA, C19, C4, C5, O7A, O9A, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O7A, C17, C8, C11, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C02I, C02P, C9, C24, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(Te1A)=Sof(TeA)=1-FVAR(1)
 Sof(Te)=Sof(Te1)=FVAR(1)
 Fixed Sof: C01N(0.5) C01T(0.5) C022(0.5) C027(0.5) C029(0.55) C02A(0.45)
 H24A(0.7) H24B(0.7) H24C(0.7) H24D(0.3) H24E(0.3) H24F(0.3) C02I(0.7)
 H02A(0.7) H02B(0.7) C02P(0.7) H02I(0.7) H02J(0.7) C02S(0.5) H02K(0.5)
 H02L(0.5) C02Y(0.5) H02P(0.5) H02Q(0.5) O9(0.5) O7(0.55) C9(0.7) H9A(0.7)
 H9B(0.7) C0(0.5) C3(0.5) C4(0.55) C5(0.45) O7A(0.45) O9A(0.5) C6(0.5) C7(0.5)
 C8(0.3) H8A(0.3) H8B(0.3) C11(0.3) H11A(0.3) H11B(0.3) C17(0.3) H17A(0.3)
 H17B(0.3) C16(0.5) H16A(0.5) H16B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) C18(0.5) H18A(0.5) H18B(0.5) C21(0.65) H21A(0.65)
 H21B(0.65) H21C(0.65) C97(0.35) H97A(0.35) H97B(0.35) H97C(0.35)
6.a Secondary CH2 refined with riding coordinates:
 C01C(H01A,H01B), C01D(H01C,H01D), C01I(H01G,H01I), C01Q(H01M,H01N), C01V(H01O,
 H01P), C01W(H01Q,H01T), C020(H02T,H02U), C021(H02V,H02W), C023(H02X,H02Y),
 C024(H02Z,H), C026(H02,HA), C02B(H2,HD), C02C(H3,HE), C02D(H4,HF), C02E(H5,HG),
  C02G(H6,HH), C02I(H02A,H02B), C02J(H7,HI), C02L(H02C,H02D), C02M(H02E,H02F),
 C02O(H02G,H02H), C02P(H02I,H02J), C02S(H02K,H02L), C02Y(H02P,H02Q), C02Z(H02R,
 H02S), C030(H03A,H03B), C032(H03C,H03D), C10(H10A,H10B), C14(H14A,H14B),
 C15(H15A,H15B), C40(H40A,H40B), C12(H12A,H12B), C9(H9A,H9B), C1(H1A,H1B),
 C8(H8A,H8B), C11(H11A,H11B), C17(H17A,H17B), C16(H16A,H16B), C19(H19A,H19B),
 C22(H22A,H22B), C18(H18A,H18B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C019(H019), C01E(H01E), C01F(H01F), C01H(H01H), C01J(H01J), C01K(H01K),
 C01L(H01L), C01R(H01R), C01S(H01S), C01U(H01U)
6.c Idealised Me refined as rotating group:
 C028(H1,HB,HC), C24(H24A,H24B,H24C), C24(H24D,H24E,H24F), C02K(H8,HJ,HK),
 C02Q(H9,HL,HM), C02R(H10,HN,HO), C02V(H11,HP,HQ), C02W(H12,HR,HS), C02X(H02M,
 H02N,H02O), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C), C2(H2A,H2B,H2C),
 C21(H21A,H21B,H21C), C97(H97A,H97B,H97C)
;
_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 2.751
_oxdiff_exptl_absorpt_empirical_full_min 0.542