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_7129920
_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
'[Cu34 (H2O)2 (C60) (C2O2F3)8 (C4H4O4S)14], 2(C7H8), 2(C2HO2F3), 2(C4H6O4S)'
_chemical_formula_sum            'C150 H78 Cu34 F30 O78 S14'
_chemical_formula_weight         6307.67
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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   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
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2022-03-16 deposited with the CCDC.	2022-04-01 downloaded from the CCDC.
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_cell_angle_alpha                64.831(2)
_cell_angle_beta                 74.884(2)
_cell_angle_gamma                74.914(2)
_cell_formula_units_Z            1
_cell_length_a                   17.0534(3)
_cell_length_b                   17.7446(4)
_cell_length_c                   18.0961(4)
_cell_measurement_reflns_used    18324
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.4330
_cell_measurement_theta_min      2.7660
_cell_volume                     4714.17(19)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49253
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        65.775
_diffrn_reflns_theta_max         65.775
_diffrn_reflns_theta_min         2.724
_exptl_absorpt_coefficient_mu    6.528
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.53046
_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.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_description       prism
_exptl_crystal_F_000             3082
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.585
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1397
_refine_ls_number_reflns         15798
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0839P)^2^+8.6013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12531
_reflns_number_total             15798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00683a2.cif
_cod_data_source_block           2
_cod_database_code               7129920
_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, All O(H,H) groups
2. Restrained distances
 O39-H39
 0.84 with sigma of 0.01
 C59B-O32B \\sim C59A-O32A
 with sigma of 0.01
 C59B-O31B \\sim C59A-O31A
 with sigma of 0.01
 C62B-O30B \\sim C62A-O30A
 with sigma of 0.01
 C62B-O29B \\sim C62A-O29A
 with sigma of 0.01
 C59B-C60B \\sim C59A-C60A
 with sigma of 0.01
 C61B-C62B \\sim C61A-C62A
 with sigma of 0.01
 C60B-S6B \\sim C60A-S6A
 with sigma of 0.01
 C61B-S6B \\sim C61A-S6A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C59B) \\sim Ueq, Uanis(C60B) \\sim Ueq, Uanis(C60B) \\sim Ueq,
Uanis(C62B) \\sim Ueq, Uanis(O32B) \\sim Ueq, Uanis(O31B) \\sim Ueq,
Uanis(O30B) \\sim Ueq, Uanis(O29B) \\sim Ueq, Uanis(S6B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(S6B) = Uanis(S6A)
Uanis(O32B) = Uanis(O32A)
Uanis(O31B) = Uanis(O31A)
Uanis(O30B) = Uanis(O30A)
Uanis(O29B) = Uanis(O29A)
Uanis(C59B) = Uanis(C59A)
Uanis(C60B) = Uanis(C60A)
Uanis(C61B) = Uanis(C61A)
Uanis(C62B) = Uanis(C62A)
4. Others
 Fixed Sof: S6A(0.5) S6B(0.5) O29A(0.5) O29B(0.5) O30A(0.5) O30B(0.5)
 O31A(0.5) O31B(0.5) O32A(0.5) O32B(0.5) C59A(0.5) C59B(0.5) C60A(0.5)
 H60A(0.5) H60B(0.5) C60B(0.5) H60C(0.5) H60D(0.5) C61A(0.5) H61A(0.5)
 H61B(0.5) C61B(0.5) H61C(0.5) H61D(0.5) C62A(0.5) C62B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 O37(H37A,H37B), 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), C60A(H60A,H60B), C60B(H60C,H60D), C61A(H61A,
 H61B), C61B(H61C,H61D), C64(H64A,H64B), C65(H65A,H65B)
5.b Aromatic/amide H refined with riding coordinates:
 C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
5.c Fitted hexagon refined as free rotating group:
 C69(C70,C71,C72,C73,C74)
5.d Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C)
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_shelx_res_checksum              59037
_shelx_hkl_checksum              44941
_shelx_fab_checksum              98161
_olex2_submission_special_instructions 'No special instructions were received'