Nested Keplerian architecture of [Cu58H20(SPr)36(PPh3)8]2+ nanocluster
Biswas, Sourav; Hossain, Sakiat; Kosaka, Taiga; Sakai, Jin; Arima, Daichi; Niihori, Yoshiki; Mitsui, Masaaki; Jiang, De-en; Das, Saikat; Wang, Song; Negishi, Yuichi; Chemical Communications  (2023) –; doi:10.1039/D3CC01811C

data_7131739
_publ_section_title
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 Nested Keplerian architecture of [Cu58H20(SPr)36(PPh3)8]2+ nanocluster
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC01811C
_journal_year                    2023
_chemical_formula_moiety         'C252 H372 Cu58 P8 S36, 3(C6 H14), (B F4)'
_chemical_formula_sum            'C270 H414 B Cu58 F4 P8 S36'
_chemical_formula_weight         8834.71
_chemical_name_systematic        Cu58
_chemical_properties_physical    Air-sensitive,Hygroscopic,Heat-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-21
_audit_creation_method
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Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
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_audit_update_record
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2023-06-24 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.3990(7)
_cell_length_b                   23.3990(7)
_cell_length_c                   57.171(4)
_cell_measurement_reflns_used    2333
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      20.785
_cell_measurement_theta_min      2.683
_cell_volume                     27108(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3, v2019.1 '
_computing_data_reduction        'SAINT V8.40A (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.919
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14513
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        20.810
_diffrn_reflns_theta_max         20.810
_diffrn_reflns_theta_min         2.041
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.615
_exptl_absorpt_correction_T_max  0.5600
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0772 before and 0.0416 after correction.
The Ratio of minimum to maximum transmission is 0.8775.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             13482
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.927
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0587
_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^)+(0.1155P)^2^+268.9969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.2028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3984
_reflns_number_total             5817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01811c2.cif
_cod_data_source_block           Cu58
_cod_original_cell_volume        27108(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7131739
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.326
_shelx_estimated_absorpt_t_min   0.220
_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
2. Restrained distances
 F1-B1 = F2-B1
 1.43 with sigma of 0.02
 C25-C17
 1.39 with sigma of 0.02
 C16-C15 = C41-C15
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C15 \\sim C48 \\sim C4 \\sim C9 \\sim C6 \\sim C27 \\sim C8 \\sim C2
\\sim C10 \\sim C12 \\sim C25 \\sim C14 \\sim C16 \\sim C18 \\sim C17 \\sim C20
\\sim C19 \\sim C22 \\sim C41 \\sim C24 \\sim C3 \\sim C26 \\sim C13 \\sim C28
\\sim C7 \\sim C30 \\sim C29 \\sim C32 \\sim C31 \\sim C34 \\sim C33 \\sim C36
\\sim C35 \\sim C38 \\sim C37 \\sim C40 \\sim C39 \\sim C42 \\sim C5 \\sim C44
\\sim C46: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 1.7A
C21 \\sim C43 \\sim C11 \\sim C45 \\sim C47 \\sim C23: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
4. Rigid body (RIGU) restrains
 C1, C15, C48, C4, C9, C6, C27, C8, C2, C10, C12, C25, C14, C16, C18, C17, C20,
  C19, C22, C41, C24, C3, C26, C13, C28, C7, C30, C29, C32, C31, C34, C33, C36,
 C35, C38, C37, C40, C39, C42, C5, C44, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C43, C11, C45, C23, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, B1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C45(0.5) H45A(0.5) H45B(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) H23C(0.5) C47(0.5) H47A(0.5) H47B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C8(H8A,H8B), C12(H12A,H12B), C14(H14A,H14B),
 C16(H16A,H16B), C24(H24A,H24B), C26(H26A,H26B), C36(H36A,H36B), C13(H13A,H13B),
  C7(H7A,H7B), C15(H15A,H15B), C43(H43A,H43B), C11(H11A,H11B), C45(H45A,H45B),
 C47(H47A,H47B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C20(H20), C22(H22), C30(H30), C32(H32), C34(H34), C38(H38),
 C42(H42), C48(H48), C3(H3), C27(H27), C29(H29), C31(H31), C33(H33), C17(H17),
 C35(H35), C9(H9), C19(H19), C39(H39)
6.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C2(H2A,H2B,H2C), C37(H37A,H37B,
 H37C), C5(H5A,H5B,H5C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              55891
_shelx_hkl_checksum              87396
_olex2_submission_original_sample_id Cu58
_olex2_submission_special_instructions 'No special instructions were received'