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_4345550
_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
'C36 H52 Cu6 N4 O22 Si10', 2(C H4 O), 0.75(C4 H8 O2)'
_chemical_formula_sum            'C41 H66 Cu6 N4 O25.5 Si10'
_chemical_formula_weight         1685.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                95.38(3)
_cell_angle_beta                 103.83(3)
_cell_angle_gamma                104.40(3)
_cell_formula_units_Z            2
_cell_length_a                   14.497(3)
_cell_length_b                   14.823(3)
_cell_length_c                   16.597(3)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      3.5
_cell_volume                     3309.5(14)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Automar (MarXperts, 2015)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65780
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.504
_diffrn_reflns_theta_min         3.542
_exptl_absorpt_coefficient_mu    4.996
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       prism
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0085(6)
_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   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         13293
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0892
_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^)+(0.08P)^2^+16.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7960
_reflns_number_total             13293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00061_si_006.cif
_cod_data_source_block           PAA1531
_cod_depositor_comments
'Adding full bibliography for 4345548--4345550.cif.'
_cod_original_formula_sum        'C41 H66 Cu6 N4 O25.50 Si10'
_cod_database_code               4345550
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.866
_shelxl_version_number           2014/6
_shelx_res_checksum              32681
_shelx_hkl_checksum              70403