A H<sub>2</sub>@C<sub>60</sub><sup>1</sup>H NMR probe for sensitively detecting the supramolecular interactions between a molecular tweezer and C<sub>60</sub>.
He, Yixing; Yu, Zhi; Jiang, Yanzi; Zhu, Jinjie; Yao, Selina X.; Liang, Wenjie; Diederich, François; Saunders, Martin; Xu, Hai; Chemical communications (Cambridge, England) 60 (2024) 8716–8719; doi:10.1039/d4cc02695k

data_7133381
_publ_section_title
;
 A H<sub>2</sub>@C<sub>60</sub><sup>1</sup>H NMR probe for sensitively
 detecting the supramolecular interactions between a molecular tweezer and
 C<sub>60</sub>.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8716
_journal_page_last               8719
_journal_paper_doi               10.1039/d4cc02695k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C184 H142 N18 Ni2 O12'
_chemical_formula_sum            'C184 H142 N18 Ni2 O12'
_chemical_formula_weight         2914.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-04-07 deposited with the CCDC.	2024-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.411(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.418(2)
_cell_length_b                   40.637(3)
_cell_length_c                   19.4953(12)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      53.96
_cell_measurement_theta_min      2.76
_cell_volume                     22096(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82430
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.905
_diffrn_reflns_theta_min         1.671
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1103 before and 0.0619 after correction.
The Ratio of minimum to maximum transmission is 0.7625.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.876
_exptl_crystal_description       block
_exptl_crystal_F_000             6096
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         20157
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1704
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2845
_refine_ls_wR_factor_ref         0.3413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8663
_reflns_number_total             20157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02695k2.cif
_cod_data_source_block           230312li_lidz095702_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133381.cif.
;
_cod_original_cell_volume        22096(2)
_cod_database_code               7133381
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.862
_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
2. Restrained distances
 C89-C88 = C89-C90 = C90-C91 = C92-C91 = C89A-C88 = C90A-C89A = C90A-C91A =
 C92A-C91A
 1.5 with sigma of 0.01
 C88-C90A
 2.5 with sigma of 0.01
 C90A-C92A
 2.5 with sigma of 0.01
 C90-C88
 2.5 with sigma of 0.01
 C89A-C91A
 2.5 with sigma of 0.01
 C89-C91
 2.5 with sigma of 0.01
 C90-C92
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C88 \\sim C89 \\sim C89A \\sim C90A \\sim C91A \\sim C92A \\sim C91 \\sim C92
\\sim C90: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C28 \\sim C29 \\sim C24 \\sim C27 \\sim C25 \\sim C26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C13 \\sim C15 \\sim C14 \\sim C18 \\sim C16 \\sim C17: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(H88C)=Sof(H88D)=Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90C)=
 Sof(H90D)=Sof(C91A)=Sof(H91C)=Sof(H91D)=Sof(C92A)=Sof(H92D)=Sof(H92E)=
 Sof(H92F)=1-FVAR(1)
 Sof(H88A)=Sof(H88B)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=
 Sof(H92C)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C89)=Sof(H89A)=Sof(H89B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C65(H65), C80(H80)
5.b Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C87(H87A,H87B), C82(H82A,H82B), C88(H88A,H88B), C88(H88C,
 H88D), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C91(H91A,H91B),
 C90(H90A,H90B), C89(H89A,H89B), C89A(H89C,H89D), C90A(H90C,H90D), C91A(H91C,
 H91D)
5.c Aromatic/amide H refined with riding coordinates:
 C63(H63), C37(H37), C40(H40), C2(H2), C36(H36), C46(H46), C41(H41), C68(H68),
 C71(H71), C32(H32), C60(H60), C31(H31), C44(H44), C43(H43), C3(H3), C10(H10),
 C9(H9), C28(H28), C29(H29), C50(H50), C6(H6), C21(H21), C20(H20), C4(H4),
 C27(H27), C5(H5), C78(H78), C75(H75), C15(H15), C14(H14), C18(H18), C77(H77),
 C16(H16), C25(H25), C76(H76), C26(H26), C17(H17)
5.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C92(H92A,H92B,H92C), C86(H86A,H86B,
 H86C), C92A(H92D,H92E,H92F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30681
_shelx_hkl_checksum              34832
_shelx_fab_checksum              71625
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU