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_7129921
_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
'[Cu32 (C60) (C2O2F3)12 (C4H4O4S)10 (C4H6O4S)2], (C7 H8)'
_chemical_formula_sum            'C139 H60 Cu32 F36 O72 S12'
_chemical_formula_weight         5984.19
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-16
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-04-01 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 91.855(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.0045(3)
_cell_length_b                   19.5007(4)
_cell_length_c                   24.9159(6)
_cell_measurement_reflns_used    19016
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8090
_cell_measurement_theta_min      2.8490
_cell_volume                     8257.8(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 0.998
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46534
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.562
_diffrn_reflns_theta_min         2.878
_exptl_absorpt_coefficient_mu    6.952
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.36585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.407
_exptl_crystal_description       prism
_exptl_crystal_F_000             5828
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.377
_refine_diff_density_min         -2.785
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         16308
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1158P)^2^+36.8328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13358
_reflns_number_total             16308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00683a2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7129921
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
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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 O(H) groups
2. Restrained distances
 C73-C67
 1.5 with sigma of 0.01
 C73-C68 \\sim C73-C72
 with sigma of 0.01
3. Restrained planarity
 C67, C68, C69, C70, C71, C72, C73
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C73) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C67(0.5) C68(0.5) H68(0.5) C69(0.5) H69(0.5) C70(0.5) H70(0.5)
 C71(0.5) H71(0.5) C72(0.5) H72(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5)
6.a Riding coordinates:
 O32(H32), O36(H36)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C34(H34A,H34B), C36(H36A,H36B), C42(H42A,H42B), C44(H44A,
 H44B), C46(H46A,H46B), C50(H50A,H50B), C54(H54A,H54B), C55(H55A,H55B),
 C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B)
6.c Aromatic/amide H refined with riding coordinates:
 C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
6.d Fitted hexagon refined as free rotating group:
 C67(C68,C69,C70,C71,C72)
6.e Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C)
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_shelx_res_checksum              36760
_shelx_hkl_checksum              33245
_olex2_submission_special_instructions 'No special instructions were received'