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_7160254
_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         'C96 H118 Cl2 O12 P2 Pt Te4'
_chemical_formula_sum            'C96 H118 Cl2 O12 P2 Pt Te4'
_chemical_formula_weight         2302.23
_chemical_name_common            6-PtCl2
_chemical_name_systematic        6-PtCl2
_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             2023-08-17
_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                83.1891(8)
_cell_angle_beta                 65.4490(9)
_cell_angle_gamma                88.1601(8)
_cell_formula_units_Z            2
_cell_length_a                   16.26452(15)
_cell_length_b                   16.53506(16)
_cell_length_c                   19.14664(18)
_cell_measurement_reflns_used    45990
_cell_measurement_temperature    129.99(10)
_cell_measurement_theta_max      74.9940
_cell_measurement_theta_min      2.5320
_cell_volume                     4649.78(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      129.99(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 0.932
_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     65.00  91.00   0.50    0.05    --  109.26 -94.00 120.00   52
  2  \w     36.00  67.00   0.50    0.05    --  109.26 -61.00  60.00   62
  3  \w     42.00  68.00   0.50    0.05    --  109.26 -61.00 -30.00   52
  4  \w     66.00 110.00   0.50    0.05    --  109.26-125.00   0.00   88
  5  \w     41.00  77.00   0.50    0.05    --   43.05-179.00 120.00   72
  6  \w     92.00 119.00   0.50    0.05    --   43.05-179.00 120.00   54
  7  \w      6.00  39.00   0.50    0.05    --   43.05 -37.00  90.00   66
  8  \w    -33.00  39.00   0.50    0.05    --   43.05 -37.00  30.00  144
  9  \w    -37.00  23.00   0.50    0.05    --   43.05 -19.00 -90.00  120
 10  \w    -19.00  76.00   0.50    0.05    --   43.05 -87.00-176.00  190
 11  \w     55.00  90.00   0.50    0.05    --  109.26 -87.00-176.00   70
 12  \w    -11.00  15.00   0.50    0.05    --   43.05 -19.00-180.00   52
 13  \w     87.00 156.00   0.50    0.05    --  109.26  61.00 -90.00  138
 14  \w     99.00 145.00   0.50    0.05    --  109.26  87.00 -58.00   92
 15  \w    -37.00  21.00   0.50    0.05    --   43.05 -19.00 150.00  116
 16  \w    -34.00   2.00   0.50    0.05    --   43.05 -37.00  90.00   72
 17  \w    -55.00  14.00   0.50    0.05    --  -43.05  87.00 -58.00  138
 18  \w    -90.00 -64.00   0.50    0.05    -- -100.00  87.00 -58.00   52
 19  \w    -56.00 -30.00   0.50    0.05    -- -100.00  87.00 -58.00   52
 20  \w    -54.00 -24.00   0.50    0.05    -- -100.00  45.00 -60.00   60
 21  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00-150.00   50
 22  \w    -92.00 -31.00   0.50    0.05    -- -100.00 125.00 -60.00  122
 23  \w    -64.00 -38.00   0.50    0.05    -- -100.00 141.00-109.66   52
 24  \w   -103.00 -27.00   0.50    0.05    -- -100.00  77.00 -60.00  152
 25  \w    -56.00 -31.00   0.50    0.05    -- -100.00 141.00  42.98   50
 26  \w    -66.00 -37.00   0.50    0.05    -- -100.00 113.00 120.20   58
 27  \w    -72.00 -26.00   0.50    0.05    -- -100.00 125.00 150.00   92
 28  \w    -52.00 -24.00   0.50    0.05    -- -100.00  45.00  60.00   56
 29  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00  30.00   50
 30  \w    -75.00 -50.00   0.50    0.05    -- -100.00 -15.00  60.00   50
 31  \w    -74.00 -42.00   0.50    0.05    -- -100.00  61.00 150.00   64
 32  \w    -54.00 -26.00   0.50    0.05    -- -100.00  45.00 150.00   56
 33  \w    -88.00 -62.00   0.50    0.05    -- -100.00  77.00  60.00   52
 34  \w    -98.00 -37.00   0.50    0.05    -- -100.00 125.00   0.00  122
 35  \w   -119.00 -73.00   0.50    0.05    -- -100.00 141.00  42.98   92
 36  \w   -108.00 -83.00   0.50    0.05    -- -100.00 113.00 120.20   50
 37  \w   -112.00 -82.00   0.50    0.05    -- -100.00 125.00 150.00   60
 38  \w   -126.00 -52.00   0.50    0.05    -- -100.00 144.00  -7.92  148
 39  \w   -109.00 -44.00   0.50    0.05    -- -100.00  77.00-120.00  130
 40  \w   -112.00 -52.00   0.50    0.05    -- -100.00 125.00-180.00  120
 41  \w   -123.00 -79.00   0.50    0.05    -- -100.00 141.00-109.66   88
 42  \w   -177.00-135.00   0.50    0.05    -- -100.00 -15.00  60.00   84
 43  \w   -175.00 -77.00   0.50    0.05    -- -100.00 -30.00  90.00  196
 44  \w   -163.00 -88.00   0.50    0.05    -- -100.00 -94.00-120.00  150
 45  \w   -130.00 -79.00   0.50    0.05    -- -100.00 -30.00-150.00  102
 46  \w   -173.00-141.00   0.50    0.05    -- -100.00 -30.00-150.00   64
 47  \w   -148.00 -84.00   0.50    0.05    -- -100.00 -87.00-176.00  128
 48  \w   -118.00 -89.00   0.50    0.05    --  -43.05-179.00-180.00   58
 49  \w   -163.00 -90.00   0.50    0.05    -- -100.00 -94.00 -60.00  146
;
_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      0.0907917000
_diffrn_orient_matrix_UB_12      0.0475319000
_diffrn_orient_matrix_UB_13      -0.0366145000
_diffrn_orient_matrix_UB_21      0.0302293000
_diffrn_orient_matrix_UB_22      -0.0473559000
_diffrn_orient_matrix_UB_23      -0.0709608000
_diffrn_orient_matrix_UB_31      -0.0411194000
_diffrn_orient_matrix_UB_32      0.0656177000
_diffrn_orient_matrix_UB_33      -0.0394356000
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61442
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.846
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44751
_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    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.096
_refine_diff_density_min         -4.990
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         18064
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+8.0683P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16911
_reflns_number_total             18064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01737d2.cif
_cod_data_source_block           6-PtCl2
_cod_depositor_comments
'Adding full bibliography for 7160252--7160260.cif.'
_cod_database_code               7160254
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.369
_shelx_estimated_absorpt_t_min   0.247
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C036) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
3. Others
 Fixed Sof: H02e(0.65) H02f(0.65) H02g(0.35) H02h(0.35) C036(0.75) H03o(0.75)
 H03p(0.75) C2(0.65) H2a(0.65) H2b(0.65) C6(0.35) H6a(0.35) H6b(0.35) C19(0.25)
 H19a(0.25) H19b(0.25) H8aa(0.75) H8ab(0.75) H8ac(0.75) H8bd(0.25) H8be(0.25)
 H8bf(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C01I(H01a,H01b), C01M(H01d,H01e), C01P(H01f,H01g), C01Q(H01h,H01i), C01S(H01j,
 H01l), C01T(H01m,H01n), C01W(H01o,H01p), C01Y(H01q,H01r), C020(H02a,H02b),
 C021(H02c,H02d), C022(H02e,H02f), C022(H02g,H02h), C023(H02i,H02j), C024(H02k,
 H02l), C025(H02m,H02n), C028(H02r,H02s), C029(H02t,H02u), C02C(H02x,H02y),
 C02D(H02z,H), C02F(H1,Ha), C02G(H2,Hb), C02H(H3,Hc), C02K(H6,Hf), C02L(H7,Hg),
 C02N(H9,Hj), C02O(H10,Hk), C02R(H13,Hn), C02S(H14,Ho), C02T(H15,Hp), C02U(H16,
 Hq), C02X(H19,Hv), C030(H03a,H03b), C031(H03c,H03d), C032(H03e,H03f),
 C035(H03m,H03n), C036(H03o,H03p), C2(H2a,H2b), C6(H6a,H6b), C19(H19a,H19b)
4.b Me refined with riding coordinates:
 C8(H8aa,H8ab,H8ac), C8(H8bd,H8be,H8bf)
4.c Aromatic/amide H refined with riding coordinates:
 C010(H010), C01C(H01C), C01K(H01K), C01X(H01X), C027(H027), C02A(H02v),
 C02B(H02w), C02E(H02), C02I(H4), C02P(H11)
4.d Idealised Me refined as rotating group:
 C026(H02o,H02p,H02q), C02J(H5,Hd,He), C02M(H8,Hh,Hi), C02Q(H12,Hl,Hm),
 C02V(H17,Hr,Hs), C02W(H18,Ht,Hu), C02Y(H20,Hw,Hx), C02Z(H21,Hy,Hz), C033(H03g,
 H03h,H03i), C034(H03j,H03k,H03l), C037(H03q,H03r,H03s)
;
_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 3.680
_oxdiff_exptl_absorpt_empirical_full_min 0.466