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_1572457
_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         'C84 H88 Cu4 N4 O28 Rb4 Si12'
_chemical_formula_sum            'C84 H88 Cu4 N4 O28 Rb4 Si12'
_chemical_formula_weight         2534.75
_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   geom
_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                 105.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.853(3)
_cell_length_b                   38.608(8)
_cell_length_c                   21.007(4)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.1
_cell_volume                     10042(4)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.74500
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            109576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         31.084
_diffrn_reflns_theta_min         1.106
_exptl_absorpt_coefficient_mu    3.347
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       prism
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.701
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1234
_refine_ls_number_reflns         27853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+5.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21685
_reflns_number_total             27853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02173h2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 1572445--1572463.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572457
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.940
_shelxl_version_number           2013-4
_shelx_res_checksum              37460