Unusual Tri-, Hexa-, and Nonanuclear Cu(II) Cage Methylsilsesquioxanes: Synthesis, Structures, and Catalytic Activity in Oxidations with Peroxides.
Bilyachenko, Alexey N.; Kulakova, Alena N.; Levitsky, Mikhail M.; Petrov, Artem A.; Korlyukov, Alexander A.; Shul'pina, Lidia S.; Khrustalev, Victor N.; Dorovatovskii, Pavel V.; Vologzhanina, Anna V.; Tsareva, Ulyana S.; Golub, Igor E.; Gulyaeva, Ekaterina S.; Shubina, Elena S.; Shul'pin, Georgiy B.; Inorganic chemistry 56 (2017) 4093–4103; doi:10.1021/acs.inorgchem.7b00061

data_4345549
_publ_section_title
;
 Unusual Tri-, Hexa-, and Nonanuclear Cu(II) Cage Methylsilsesquioxanes:
 Synthesis, Structures, and Catalytic Activity in Oxidations with
 Peroxides.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4093
_journal_page_last               4103
_journal_paper_doi               10.1021/acs.inorgchem.7b00061
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C28 H40 Cu3 N4 O15 Si8, 3(C2 H6 O)'
_chemical_formula_sum            'C34 H58 Cu3 N4 O18 Si8'
_chemical_formula_weight         1226.18
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.74(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.210(2)
_cell_length_b                   17.480(4)
_cell_length_c                   25.210(5)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.9
_cell_measurement_theta_min      2.4
_cell_volume                     5318.1(19)
_computing_cell_refinement       iMosflm
_computing_data_collection       Automar
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'MAR CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96600
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.1080
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33997
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        35.422
_diffrn_reflns_theta_max         38.258
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    3.305
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       prism
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00089(12)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0718
_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^)+(0.08P)^2^+24P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3642
_reflns_number_total             5473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00061_si_004.cif
_cod_data_source_block           1622
_cod_depositor_comments
'Adding full bibliography for 4345548--4345550.cif.'
_cod_database_code               4345549
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.638
_shelxl_version_number           2014/6
_shelx_res_checksum              74918
_shelx_hkl_checksum              67776