Rational (supra)molecular design and catalytic activity of cage-like Cu<sub>4</sub>-based phenylsilsesquioxanes.
Zueva, Anna Y.; Bilyachenko, Alexey N.; Khrustalev, Victor N.; Shul'pina, Lidia S.; Ikonnikov, Nikolay S.; Dorovatovskii, Pavel V.; Shubina, Elena S.; Ragimov, Karim; Lobanov, Nikolai N.; Sun, Di; Nanoscale 16 (2024) 18389–18398; doi:10.1039/d4nr02173h

data_1572461
_publ_section_title
;
 Rational (supra)molecular design and catalytic activity of cage-like
 Cu<sub>4</sub>-based phenylsilsesquioxanes.
;
_journal_issue                   39
_journal_name_full               Nanoscale
_journal_page_first              18389
_journal_page_last               18398
_journal_paper_doi               10.1039/d4nr02173h
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C75 H79 Cu4 Na4 O30.50 Si12, C2 H6 O'
_chemical_formula_sum            'C77 H85 Cu4 Na4 O31.5 Si12'
_chemical_formula_weight         2197.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2024-05-14 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.023(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.5879(10)
_cell_length_b                   12.4253(3)
_cell_length_c                   25.4831(5)
_cell_measurement_reflns_used    17812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.3
_cell_volume                     9878.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1156
_diffrn_reflns_av_unetI/netI     0.1187
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            92499
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.782
_diffrn_reflns_theta_min         2.324
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             4508
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.714
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         14618
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0981
_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^)+(0.0509P)^2^+150.9P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9641
_reflns_number_total             14618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02173h2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 1572445--1572463.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C77 H85 Cu4 Na4 O31.50 Si12'
_cod_database_code               1572461
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.979
_shelxl_version_number           2013-4
_shelx_res_checksum              81100