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_7160260
_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 Se4, 0.5(C2 H3 N)'
_chemical_formula_sum            'C97 H119.5 Cl2 N0.5 O12 P2 Pt Se4'
_chemical_formula_weight         2128.19
_chemical_name_common            5-PtCl2
_chemical_name_systematic        5-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     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                89.8577(9)
_cell_angle_beta                 78.6933(10)
_cell_angle_gamma                86.8545(11)
_cell_formula_units_Z            4
_cell_length_a                   17.1838(2)
_cell_length_b                   22.6370(3)
_cell_length_c                   24.0907(2)
_cell_measurement_reflns_used    95871
_cell_measurement_temperature    149.96(13)
_cell_measurement_theta_max      77.3210
_cell_measurement_theta_min      1.8730
_cell_volume                     9174.99(18)
_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 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.96(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.997
_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     36.00 119.00   0.50    0.05    --   47.45  22.00 158.00  166
  2  \w    101.00 151.00   0.50    0.05    --  107.75  22.00 158.00  100
  3  \w     95.00 174.00   0.50    0.05    --  107.75  37.00  60.00  158
  4  \w     95.00 160.00   0.50    0.05    --  107.75  19.00-150.00  130
  5  \w     34.00  69.00   0.50    0.05    --   47.45 -77.00 -90.00   70
  6  \w     -1.00  25.00   0.50    0.05    --   47.45 -77.00 -90.00   52
  7  \w    -26.00  22.00   0.50    0.05    --   47.45 -19.00-150.00   96
  8  \w    -17.00   9.00   0.50    0.05    --   47.45 -19.00 -90.00   52
  9  \w     -5.00  24.00   0.50    0.05    --   47.45 -22.00  -7.00   58
 10  \w    -24.00  22.00   0.50    0.05    --   47.45 -19.00 150.00   92
 11  \w     61.00  89.00   0.50    0.05    --   47.45-125.00   0.00   56
 12  \w     18.00  46.00   0.50    0.05    --   47.45-125.00   0.00   56
 13  \w     83.00 112.00   0.50    0.05    --  107.75-125.00 -90.00   58
 14  \w     46.00 104.00   0.50    0.05    --  107.75-125.00  60.00  116
 15  \w     35.00 112.00   0.50    0.05    --  107.75-125.00  90.00  154
 16  \w     38.00 106.00   0.50    0.05    --  107.75-106.00 133.14  136
 17  \w     51.00  77.00   0.50    0.05    --  107.75-106.00 157.62   52
 18  \w     82.00 107.00   0.50    0.05    --  107.75-106.00 157.62   50
 19  \w     78.00 106.00   0.50    0.05    --  107.75 -99.00  60.00   56
 20  \w     40.00  66.00   0.50    0.05    --  107.75 -99.00   0.00   52
 21  \w     35.00  69.00   0.50    0.05    --  107.75 -99.00 -30.00   68
 22  \w     38.00  86.00   0.50    0.05    --  107.75 -99.00 -60.00   96
 23  \w     44.00  69.00   0.50    0.05    --  107.75 -77.00-150.00   50
 24  \w     35.00  60.00   0.50    0.05    --  107.75 -57.00-180.00   50
 25  \w     36.00  61.00   0.50    0.05    --  107.75 -57.00 -60.00   50
 26  \w     37.00  63.00   0.50    0.05    --  107.75 -57.00 -30.00   52
 27  \w     35.00  63.00   0.50    0.05    --  107.75 -57.00  30.00   56
 28  \w     48.00  73.00   0.50    0.05    --  107.75 -77.00  90.00   50
 29  \w     35.00  60.00   0.50    0.05    --  107.75 -57.00  60.00   50
 30  \w    -30.00   8.00   0.50    0.05    --  -47.45  22.00 158.00   76
 31  \w    -68.00 -42.00   0.50    0.05    -- -100.00  57.00 150.00   52
 32  \w    -68.00 -43.00   0.50    0.05    -- -100.00  57.00 120.00   50
 33  \w    -58.00 -27.00   0.50    0.05    -- -100.00 125.00  60.00   62
 34  \w   -112.00 -70.00   0.50    0.05    -- -100.00 125.00  60.00   84
 35  \w    -93.00 -39.00   0.50    0.05    -- -100.00 125.00 150.00  108
 36  \w    -95.00 -28.00   0.50    0.05    --  -47.45 125.00 -60.00  134
 37  \w    -81.00 -38.00   0.50    0.05    -- -100.00 138.00-152.95   86
 38  \w   -121.00 -88.00   0.50    0.05    -- -100.00 138.00-152.95   66
 39  \w   -112.00 -37.00   0.50    0.05    -- -100.00 125.00-120.00  150
 40  \w    -54.00 -28.00   0.50    0.05    -- -100.00 125.00 -90.00   52
 41  \w   -109.00 -50.00   0.50    0.05    -- -100.00 117.00 -38.85  118
 42  \w   -121.00 -35.00   0.50    0.05    --  -47.45 -22.00  -7.00  172
 43  \w   -121.00 -92.00   0.50    0.05    -- -100.00 -99.00 -90.00   58
 44  \w   -174.00 -89.00   0.50    0.05    -- -100.00 -22.00  -7.00  170
 45  \w   -166.00 -85.00   0.50    0.05    -- -100.00 -57.00 150.00  162
 46  \w   -171.00-121.00   0.50    0.05    -- -100.00-125.00  60.00  100
 47  \w   -167.00 -84.00   0.50    0.05    -- -100.00-125.00 120.00  166
;
_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      -0.0843896000
_diffrn_orient_matrix_UB_12      0.0230160000
_diffrn_orient_matrix_UB_13      -0.0049589000
_diffrn_orient_matrix_UB_21      -0.0176845000
_diffrn_orient_matrix_UB_22      -0.0620875000
_diffrn_orient_matrix_UB_23      -0.0186585000
_diffrn_orient_matrix_UB_31      -0.0308253000
_diffrn_orient_matrix_UB_32      -0.0161616000
_diffrn_orient_matrix_UB_33      0.0622934000
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            116819
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.024
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43923
_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            'metallic light black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       needle
_exptl_crystal_F_000             4316
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.437
_refine_diff_density_min         -3.530
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2159
_refine_ls_number_reflns         32357
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+30.8582P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29790
_reflns_number_total             32357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01737d2.cif
_cod_data_source_block           5-PtCl2
_cod_depositor_comments
'Adding full bibliography for 7160252--7160260.cif.'
_cod_original_cell_volume        9175.00(19)
_cod_original_formula_sum        'C97 H119.50 Cl2 N0.50 O12 P2 Pt Se4'
_cod_database_code               7160260
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.753
_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
 C05L-C06A
 1.54 with sigma of 0.02
 C05L-C06A = C06A-C06J
 1.54 with sigma of 0.02
 C06D-C06N = C06N-C06H
 1.54 with sigma of 0.02
 C1-C06D = C06D-C06N
 1.54 with sigma of 0.02
 C05L-C06J
 2.515 with sigma of 0.04
 C06D-C025
 2.515 with sigma of 0.04
 C06D-C06H
 2.515 with sigma of 0.04
 C1-C06N
 2.515 with sigma of 0.04
3. Rigid bond restraints
 C06N, C06H, C06D, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C05W, C06F, O012
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim C05W \\sim C06F \\sim O012: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
C06H \\sim C06N \\sim C06D \\sim C1: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
5. Rigid body (RIGU) restrains
 C05L, C06A, C06J
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C06D, C06N, C06H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, C06D, C06N, C06H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C028(H02A,H02B), C02M(H02C,H02D), C02Y(H02E,H02F), C031(H03Q,H03R), C036(H03A,
 H03B), C03D(H03C,H03D), C03E(H03E,H03F), C03H(H03S,H03U), C03I(H03W,H03X),
 C03J(H03G,H03H), C03K(H03I,H03J), C03L(H03K,H03L), C03N(H03Y,H), C03O(H03M,
 H03N), C03P(H03Z,HA), C03U(H03,HB), C03W(H03O,H03P), C03X(H8,HC), C041(H04A,
 H04B), C042(H04C,H04D), C045(H04E,H04F), C046(H04G,H04H), C047(H04I,H04J),
 C048(H04K,H04L), C049(H04M,H04N), C04A(H04O,H04P), C04B(H04Q,H04R), C04C(H10,
 HD), C04G(H14,HE), C04J(H04U,H04V), C04K(H15,HF), C04M(H04Z,HG), C04N(H04,HH),
 C04O(H1,HI), C04P(H2,HJ), C04Q(H16,HK), C04R(H3,HL), C04U(H17,HO), C04V(H18,
 HP), C04W(H6,HQ), C04X(H19,HR), C04Y(H20,HS), C04Z(H21,HT), C050(H22,HU),
 C051(H05A,H05B), C052(H05C,H05D), C054(H23,HV), C055(H24,HW), C056(H05E,H05F),
 C059(H26,HZ), C05E(H30,H51), C05F(H05J,H05K), C05H(H05O,H05P), C05I(H05Q,H05R),
  C05K(H31,H52), C05L(H32,H53), C05M(H33,H54), C05N(H34,H55), C05P(H35,H56),
 C05Q(H36,H57), C05U(H38,H60), C05W(H39,H63), C05X(H05,H64), C062(H06A,H06B),
 C064(H06C,H06D), C066(H06E,H06F), C06A(H41,H76), C06D(H42,H77), C06F(H43,H78),
 C06I(H06S,H06T), C06N(H47,H85), C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C01W(H01W), C02K(H02K), C02L(H02L), C032(H032), C038(H038), C039(H039),
 C03T(H03T), C03V(H03V), C03Z(H9), C043(H043), C04D(H11), C04E(H12), C04F(H13),
 C04H(H04S), C04I(H04T), C04T(H5), C053(H053), C05B(H28), C05C(H29), C05O(H05V)
6.c Idealised Me refined as rotating group:
 C04L(H04W,H04X,H04Y), C04S(H4,HM,HN), C058(H25,HX,HY), C05A(H27,H49,H50),
 C05D(H05G,H05H,H05I), C05G(H05L,H05M,H05N), C05J(H05S,H05T,H05U), C05R(H37,H58,
 H59), C05S(H05W,H05X,H05Y), C05V(H05Z,H61,H62), C05Y(H7,H65,H66), C05Z(H40,H67,
 H68), C061(H06U,H06V,H06W), C063(H06X,H06Y,H69), C065(H06Z,H70,H71), C067(H48,
 H72,H73), C068(H06,H74,H75), C069(H06G,H06H,H06I), C06B(H06J,H06K,H06L),
 C06E(H06M,H06N,H06O), C06G(H06P,H06Q,H06R), C06H(H44,H79,H80), C06J(H45,H81,
 H82), C06K(H46,H83,H84), C5(H5A,H5B,H5C)
;
_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 3.493
_oxdiff_exptl_absorpt_empirical_full_min 0.489