High-nuclearity and thiol protected core-shell [Cu<sub>75</sub>(S-Adm)<sub>32</sub>]<sup>2+</sup>: distorted octahedra fixed to Cu<sub>15</sub> core <i>via</i> strong cuprophilic interactions.
Tang, Jie; Liu, Chong; Zhu, Chenyu; Sun, Keju; Wang, He; Yin, Wen; Xu, Chuting; Li, Yang; Wang, Weiguo; Wang, Li; Wu, Renan; Liu, Chao; Huang, Jiahui; Nanoscale 15 (2023) 2843–2848; doi:10.1039/d2nr05921e

data_1568222
_publ_section_title
;
 High-nuclearity and thiol protected core-shell
 [Cu<sub>75</sub>(S-Adm)<sub>32</sub>]<sup>2+</sup>: distorted octahedra
 fixed to Cu<sub>15</sub> core <i>via</i> strong cuprophilic interactions.
;
_journal_issue                   6
_journal_name_full               Nanoscale
_journal_page_first              2843
_journal_page_last               2848
_journal_paper_doi               10.1039/d2nr05921e
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C320 H480 Cu75 S32'
_chemical_formula_sum            'C320 H480 Cu75 S32'
_chemical_formula_weight         10118.43
_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
_audit_block_doi                 10.5517/ccdc.csd.cc2c1v09
_audit_creation_date             2021-09-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-02 deposited with the CCDC.	2022-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                112.1310(10)
_cell_angle_beta                 119.5380(10)
_cell_angle_gamma                92.9240(10)
_cell_formula_units_Z            1
_cell_length_a                   23.6279(5)
_cell_length_b                   23.6779(5)
_cell_length_c                   23.8819(5)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      62.026
_cell_measurement_theta_min      2.349
_cell_volume                     10292.9(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            93609
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        62.385
_diffrn_reflns_theta_max         62.385
_diffrn_reflns_theta_min         2.107
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.813
_exptl_absorpt_correction_T_max  0.1600
_exptl_absorpt_correction_T_min  0.0620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1284 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.3875.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             5087
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.499
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.594
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1828
_refine_ls_number_reflns         31471
_refine_ls_number_restraints     402
_refine_ls_restrained_S_all      1.585
_refine_ls_R_factor_all          0.2510
_refine_ls_R_factor_gt           0.1854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.4530
_refine_ls_wR_factor_ref         0.5012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15383
_reflns_number_total             31471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05921e2.cif
_cod_data_source_block           dicp_la
_cod_depositor_comments          'Adding full bibliography for 1568222.cif.'
_cod_database_code               1568222
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.594
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
2. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C52, C53, C54, C55, C56, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C81, C82, C83, C84, C85, C86, C87, C88, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C131, C132, C133, C134, C135, C136, C137, C138, C139, C140
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C76, C77, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C102, C105, C108, C110
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C145, C148, C146
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 C21(C22,C23,C24,C25,C26,C27,C28,C29,C30), C51(C52,C53,C54,C55,C56,C57,C58,C59,
 C60), C81(C82,C83,C84,C85,C86,C87,C88,C89,C90), C131(C132,C133,C134,C135,C136,
 C137,C138,C139,C140)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15), C16(H16), C17(H17), C25(H25), C26(H26),
 C27(H27), C35(H35), C36(H36), C37(H37), C45(H45), C46(H46), C47(H47), C55(H55),
  C56(H56), C57(H57), C65(H65), C66(H66), C67(H67), C75(H75), C76(H76),
 C77(H77), C85(H85), C86(H86), C87(H87), C95(H95), C96(H96), C97(H97),
 C105(H105), C106(H106), C107(H107), C115(H115), C116(H116), C117(H117),
 C125(H125), C126(H126), C127(H127), C135(H135), C136(H136), C137(H137),
 C145(H145), C146(H146), C147(H147), C155(H155), C156(H156), C157(H157)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C48(H48A,H48B), C49(H49A,H49B),
  C50(H50A,H50B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C58(H58A,
 H58B), C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C72(H72A,H72B),
  C73(H73A,H73B), C74(H74A,H74B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,
 H80B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C88(H88A,H88B),
 C89(H89A,H89B), C90(H90A,H90B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B),
  C98(H98A,H98B), C99(H99A,H99B), C100(H10C,H10D), C102(H10E,H10F), C103(H10G,
 H10H), C104(H10I,H10J), C108(H10K,H10L), C109(H10M,H10N), C110(H11A,H11B),
 C112(H11C,H11D), C113(H11E,H11F), C114(H11G,H11H), C118(H11I,H11J), C119(H11K,
 H11L), C120(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J),
 C128(H12K,H12L), C129(H12M,H12N), C130(H13C,H13D), C132(H13E,H13F), C133(H13G,
 H13H), C134(H13I,H13J), C138(H13K,H13L), C139(H13M,H13N), C140(H14C,H14D),
 C142(H14E,H14F), C143(H14G,H14H), C144(H14I,H14J), C148(H14K,H14L), C149(H14M,
 H14N), C150(H15A,H15B), C152(H15C,H15D), C153(H15E,H15F), C154(H15G,H15H),
 C158(H15I,H15J), C159(H15K,H15L), C160(H16A,H16B)
;
_shelx_res_checksum              8504
_shelx_fab_checksum              79883
_olex2_submission_special_instructions 'No special instructions were received'