Regioisomeric Core-shell Cuprofullerene C60@Cu24
Guo, You-Shi; Zhan, Shun-Ze; Zhong, Jia-Jing; Lu, Weigang; Ng, Seik Weng; Li, Dan; Chemical Communications  (2022) –; doi:10.1039/D2CC00683A

data_7129919
_publ_section_title
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 Regioisomeric Core-shell Cuprofullerene C60@Cu24
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00683A
_journal_year                    2022
_chemical_formula_moiety         'Cu24 C60 (C8 H8 O2)12 (C2 F3 O2)24'
_chemical_formula_sum            'C204 H96 Cu24 F72 O72'
_chemical_formula_weight         6592.01
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2022-03-16 deposited with the CCDC.	2022-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   32.3438(3)
_cell_length_b                   32.3438(3)
_cell_length_c                   18.03400(19)
_cell_measurement_reflns_used    10818
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7910
_cell_measurement_theta_min      3.9830
_cell_volume                     16338.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16363
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.143
_diffrn_reflns_theta_min         2.732
_exptl_absorpt_coefficient_mu    3.809
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.79333
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       prism
_exptl_crystal_F_000             9720
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0819P)^2^+63.9474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6411
_reflns_number_total             7079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00683a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        16338.2(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7129919
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8 = O10-H10
 0.84 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C30(H30), C31(H31)
3.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
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_shelx_res_checksum              53610
_shelx_hkl_checksum              19737
_olex2_submission_special_instructions 'No special instructions were received'