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_7160259
_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 Se2, 0.25(C2 H3 N)'
_chemical_formula_sum            'C48.5 H59.75 Au Cl N0.25 O6 P Se2'
_chemical_formula_weight         1163.52
_chemical_name_common            5-AuCl
_chemical_name_systematic        5-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     iterative
_audit_creation_date             2023-08-17
_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                 91.8893(6)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.00533(19)
_cell_length_b                   38.3306(3)
_cell_length_c                   17.81397(12)
_cell_measurement_reflns_used    54948
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      76.2450
_cell_measurement_theta_min      1.9680
_cell_volume                     19112.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 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 0.993
_diffrn_measured_fraction_theta_max 0.939
_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     33.00 119.00   0.50    0.29    --   47.45  57.00-150.00  172
  2  \w     49.00 119.00   0.50    0.29    --   47.45 166.00-172.00  140
  3  \w     50.00 125.00   0.50    1.16    --  107.75 166.00-172.00  150
  4  \w    104.00 129.00   0.50    1.16    --  107.75 115.00  41.00   50
  5  \w    101.00 172.00   0.50    1.16    --  107.75  37.00  30.00  142
  6  \w     46.00 102.00   0.50    1.16    --  107.75 -99.00 -30.00  112
  7  \w     36.00 109.00   0.50    1.16    --  107.75-115.00 -48.00  146
  8  \w     26.00  51.00   0.50    0.29    --   47.45-115.00 -48.00   50
  9  \w     55.00  80.00   0.50    0.29    --   47.45-166.00 165.00   50
 10  \w     38.00  63.00   0.50    1.16    --  107.75 -57.00 120.00   50
 11  \w     59.00  99.00   0.50    1.16    --  107.75 -77.00 -30.00   80
 12  \w     38.00  63.00   0.50    1.16    --  107.75 -57.00 -60.00   50
 13  \w     35.00  60.00   0.50    1.16    --  107.75 -57.00 -30.00   50
 14  \w   -106.00 -81.00   0.50    0.29    --  -47.45 166.00-172.00   50
 15  \w   -114.00 -89.00   0.50    1.16    -- -100.00 166.00-172.00   50
 16  \w    -80.00 -53.00   0.50    0.29    --  -47.45 115.00  41.00   54
 17  \w   -109.00 -72.00   0.50    1.16    -- -100.00 115.00  41.00   74
 18  \w    -67.00 -28.00   0.50    1.16    -- -100.00  77.00  60.00   78
 19  \w    -66.00 -39.00   0.50    1.16    -- -100.00  57.00  30.00   54
 20  \w    -63.00 -38.00   0.50    1.16    -- -100.00  57.00 -30.00   50
 21  \w    -68.00 -31.00   0.50    1.16    -- -100.00  57.00 -90.00   74
 22  \w    -68.00 -27.00   0.50    1.16    -- -100.00  57.00-120.00   82
 23  \w    -60.00 -33.00   0.50    1.16    -- -100.00  57.00  60.00   54
 24  \w   -174.00 -88.00   0.50    1.16    -- -100.00 -19.00 150.00  172
;
_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      0.0013460000
_diffrn_orient_matrix_UB_12      0.0396032000
_diffrn_orient_matrix_UB_13      -0.0145706000
_diffrn_orient_matrix_UB_21      0.0538837000
_diffrn_orient_matrix_UB_22      -0.0023447000
_diffrn_orient_matrix_UB_23      -0.0140697000
_diffrn_orient_matrix_UB_31      -0.0111288000
_diffrn_orient_matrix_UB_32      -0.0065006000
_diffrn_orient_matrix_UB_33      -0.0841098000
_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  0.0646
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            127745
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.727
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       needle
_exptl_crystal_F_000             9272
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.590
_refine_diff_density_min         -5.074
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2164
_refine_ls_number_reflns         38279
_refine_ls_number_restraints     1632
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0801
_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^)+(0.1272P)^2^+189.1734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2264
_refine_ls_wR_factor_ref         0.2391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31132
_reflns_number_total             38279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01737d2.cif
_cod_data_source_block           5-AuCl
_cod_depositor_comments
'Adding full bibliography for 7160252--7160260.cif.'
_cod_original_formula_sum        'C48.50 H59.75 Au Cl N0.25 O6 P Se2'
_cod_database_code               7160259
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.397
_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
2. Restrained distances
 C04X-C05C = C05C-C067
 1.54 with sigma of 0.02
 C05C-C067 = C067-C13
 1.54 with sigma of 0.02
 C05M-C064 = C064-C3
 1.54 with sigma of 0.02
 C064-C3 = C3-C2
 1.54 with sigma of 0.02
 C06A-C1 = C1-C22
 1.54 with sigma of 0.02
 C05T-C06A = C06A-C1
 1.54 with sigma of 0.02
 C05C-C13
 2.515 with sigma of 0.04
 C04X-C067
 2.515 with sigma of 0.04
 C064-C2
 2.515 with sigma of 0.04
 C05M-C3
 2.515 with sigma of 0.04
 C06A-C22
 2.515 with sigma of 0.04
 C05T-C1
 2.515 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
4. Rigid body (RIGU) restrains
 C04X, C05C, C067, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C05M, C064, C3, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C05T, C06A, C1, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C049, C05B, C065, C068, C05V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C01W(H01a,H01b), C01Y(H01c,H01d), C02A(H02i,H02j), C02K(H02k,H02l), C02O(H02a,
 H02b), C02Q(H02c,H02d), C02V(H02e,H02f), C02Z(H02g,H02h), C031(H03s,H03t),
 C03H(H03a,H03b), C03I(H03d,H03e), C03N(H03n,H03o), C03P(H03f,H03g), C03R(H03y,
 H), C03U(H03z,Ha), C03V(H03h,H03i), C03W(H03j,H03k), C03Y(H03p,H03r),
 C03Z(H03l,H03m), C041(H18,Hd), C045(H5,He), C047(H04h,H04i), C048(H6,Hf),
 C04A(H7,Hg), C04C(H04a,H04b), C04D(H9,Hh), C04E(H10,Hi), C04F(H04j,H04k),
 C04G(H22,Hj), C04H(H04m,H04n), C04I(H23,Hk), C04K(H24,Hl), C04M(H04c,H04d),
 C04P(H04r,H04s), C04R(H04t,H04u), C04T(H12,Hm), C04U(H25,Hn), C04V(H13,Ho),
 C04W(H04v,H04w), C04X(H04x,H04y), C04Y(H04z,Hp), C050(H05t,H05u), C052(H05v,
 H05w), C053(H26,Hq), C056(H27,Hr), C057(H28,Hs), C058(H05d,H05e), C05A(H05f,
 H05g), C05C(H05x,H05y), C05F(H05,Hx), C05I(H30,H37), C05M(H15,H44), C05N(H33,
 H45), C05P(H05k,H05l), C05Q(H2,H48), C05S(H3,H51), C05T(H17,H52), C05U(H05m,
 H05n), C05X(H05o,H05p), C05Y(H34,H53), C060(H06i,H06j), C061(H06w,H06x),
 C063(H06y,H54), C064(H06s,H06t), C066(H06z,H55), C067(H06n,H06o), C069(H06a,
 H06b), C06A(H06u,H06v), C06E(H06,H56), C18(H18a,H18b), C1(H1a,H1b), C3(H3a,H3b)
5.b Me refined with riding coordinates:
 C13(H13a,H13b,H13c)
5.c Aromatic/amide H refined with riding coordinates:
 C032(H032), C039(H039), C03C(H03C), C03D(H03u), C03Q(H03Q), C044(H044),
 C046(H046), C05B(H19), C065(H065), C05W(H20), C068(H068), C05V(H21), C04B(H8),
 C04J(H04p), C04L(H04L), C04N(H11), C04O(H04O), C04Q(H04Q), C04Z(H04),
 C051(H051)
5.d Fitted hexagon refined as free rotating group:
 C049(C05B,C065,C05W,C068,C05V)
5.e Idealised Me refined as rotating group:
 C03X(H03v,H03w,H03x), C040(H4,Hb,Hc), C04S(H04e,H04f,H04g), C055(H05a,H05b,
 H05c), C05D(H36,Ht,Hu), C05E(H05z,Hv,Hw), C05G(H05h,H05i,H05j), C05H(H29,Hy,
 Hz), C05J(H31,H38,H39), C05K(H14,H40,H41), C05L(H32,H42,H43), C05O(H1,H46,H47),
  C05R(H16,H49,H50), C05Z(H05q,H05r,H05s), C062(H06k,H06l,H06m), C06D(H06c,H06d,
 H06e), C06F(H06p,H06q,H06r), C06G(H06f,H06g,H06h), C06H(H35,H57,H58), C14(H14a,
 H14b,H14c), C26(H26a,H26b,H26c), C5(H5a,H5b,H5c), C22(H22a,H22b,H22c), C2(H2a,
 H2b,H2c)
;
_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 3.523
_oxdiff_exptl_absorpt_empirical_full_min 0.555