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_1572447
_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_absolute_configuration ad
_chemical_formula_moiety
'C86.40 H98.80 Cu4 N2 Na4 O30 Si12, C84 H94 Cu4 N2 Na4 O30 Si12'
_chemical_formula_sum            'C170.4 H192.8 Cu8 N4 Na8 O60 Si24'
_chemical_formula_weight         4623.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 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                 90.369(9)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   19.8450(18)
_cell_length_b                   12.7240(11)
_cell_length_c                   20.3720(19)
_cell_measurement_reflns_used    3425
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.38
_cell_volume                     5144.0(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79313
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41393
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        28.417
_diffrn_reflns_theta_max         31.015
_diffrn_reflns_theta_min         1.145
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       prism
_exptl_crystal_F_000             2379
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 6068 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.031(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         23286
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0655
_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^)+(0.099P)^2^+5.5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1816
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                15908
_reflns_number_total             23286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02173h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1572445--1572463.cif.'
_cod_original_sg_symbol_H-M      'P 2'
_cod_original_formula_sum        'C170.40 H192.80 Cu8 N4 Na8 O60 Si24'
_cod_database_code               1572447
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.946
_shelxl_version_number           2013-4
_shelx_res_checksum              3477