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_7160253
_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 Pd Te4'
_chemical_formula_sum            'C96 H118 Cl2 O12 P2 Pd Te4'
_chemical_formula_weight         2213.54
_chemical_name_common            6-PdCl2
_chemical_name_systematic        6-PdCl2
_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                94.148(2)
_cell_angle_beta                 96.151(2)
_cell_angle_gamma                90.060(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0020(4)
_cell_length_b                   17.4424(4)
_cell_length_c                   17.9639(5)
_cell_measurement_reflns_used    17836
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.14
_cell_measurement_theta_min      2.48
_cell_volume                     4661.1(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type
'No syntax errors found.                               CIF dictionary'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49926
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.138
_diffrn_reflns_theta_min         2.480
_exptl_absorpt_coefficient_mu    12.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)'
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.650
_refine_diff_density_min         -1.988
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         17836
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+42.8980P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14321
_reflns_number_total             17836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01737d2.cif
_cod_data_source_block           6-PdCl2
_cod_depositor_comments
'Adding full bibliography for 7160252--7160260.cif.'
_cod_database_code               7160253
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.432
_shelx_estimated_absorpt_t_min   0.187
_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. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C032) \\sim Ueq, Uanis(C036)
\\sim Ueq, Uanis(C02Y) \\sim Ueq, Uanis(C037) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C02V(0.5) H16(0.5) Hu(0.5) H18(0.5) Hw(0.5) Hx(0.5) Hy(0.5)
 Hz(0.5) H21(0.5) C02Z(0.5) H20(0.5) H23(0.5) C034(0.5) H03l(0.5) H03m(0.5)
 C44(0.5) H44a(0.5) H44b(0.5) C48(0.5) H48a(0.5) H48b(0.5) C15(0.5) H15a(0.5)
 H15b(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C01M(H01a,H01b), C01O(H01c,H01d), C01P(H01e,H01f), C01W(H01i,H01j), C020(H02a,
 H02b), C021(H02c,H02d), C023(H02e,H02f), C024(H02g,H02h), C026(H02i,H02j),
 C027(H02k,H02l), C028(H02m,H02n), C029(H02o,H02p), C02A(H02q,H02r), C02C(H02v,
 H02w), C02D(H02x,H02y), C02E(H02z,H), C02F(H02,Ha), C02G(H1,Hb), C02H(H2,Hc),
 C02I(H3,Hd), C02K(H5,Hg), C02L(H6,Hh), C02N(H8,Hk), C02O(H9,Hl), C02P(H10,Hm),
 C02R(H12,Hp), C02S(H13,Hq), C02T(H14,Hr), C02V(H16,Hu), C02W(H17,Hv), C02Y(H19,
 H22), C02Z(H20,H23), C032(H03g,H03h), C034(H03l,H03m), C035(H03n,H03o),
 C44(H44a,H44b), C48(H48a,H48b), C15(H15a,H15b), C4(H4a,H4b)
4.b Me refined with riding coordinates:
 C02X(H18,Hw,Hx), C02X(Hy,Hz,H21)
4.c Aromatic/amide H refined with riding coordinates:
 C01G(H01G), C01H(H01H), C01K(H01K), C01L(H01L), C01R(H01R), C01T(H01T),
 C01U(H01U), C01Y(H01Y), C022(H022), C025(H025)
4.d Idealised Me refined as rotating group:
 C02B(H02s,H02t,H02u), C02J(H4,He,Hf), C02M(H7,Hi,Hj), C02Q(H11,Hn,Ho),
 C02U(H15,Hs,Ht), C030(H03a,H03b,H03c), C031(H03d,H03e,H03f), C033(H03i,H03j,
 H03k), C036(H03p,H03q,H03r), C037(H03s,H03t,H03u), C11(H11a,H11b,H11c)
;
_olex2_submission_special_instructions 'No special instructions were received'