Solvent-controlled synthesis of tetranuclear cage-like copper(II) silsesquioxanes. Remarkable features of the cage structures and their high catalytic activity in oxidation with peroxides.
Dronova, Marina S.; Bilyachenko, Alexey N.; Yalymov, Alexey I.; Kozlov, Yuriy N.; Shul'pina, Lidia S.; Korlyukov, Alexander A.; Arkhipov, Dmitry E.; Levitsky, Mikhail M.; Shubina, Elena S.; Shul'pin, Georgiy B.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 872–882; doi:10.1039/c3dt52508b

data_7028319
_publ_section_title
;
 Solvent-controlled synthesis of tetranuclear cage-like copper(II)
 silsesquioxanes. Remarkable features of the cage structures and their
 high catalytic activity in oxidation with peroxides.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              872
_journal_page_last               882
_journal_paper_doi               10.1039/c3dt52508b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C48 H54 Cu2 Na2 O18 Si6'
_chemical_formula_sum            'C48 H54 Cu2 Na2 O18 Si6'
_chemical_formula_weight         1260.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.765(2)
_cell_length_b                   20.851(2)
_cell_length_c                   28.856(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.39
_cell_volume                     11892(2)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18324
_diffrn_reflns_theta_full        30.65
_diffrn_reflns_theta_max         30.65
_diffrn_reflns_theta_min         1.41
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.8451
_exptl_absorpt_correction_T_min  0.8169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
;
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         18324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                10441
_reflns_number_total             18324
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            c3dt52508b.txt
_cod_data_source_block           yaai72
_cod_database_code               7028319
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.032) H3A(0.038) H4A(0.033) H5A(0.029) H6A(0.023) H8A(0.04)
 H9A(0.059) H10A(0.061) H11A(0.054) H12A(0.035) H14A(0.027) H15A(0.036)
 H16A(0.041) H17A(0.038) H18A(0.03) H20A(0.025) H21A(0.029) H22A(0.031)
 H23A(0.033) H24A(0.025) H26A(0.038) H27A(0.051) H28A(0.047) H29A(0.044)
 H30A(0.031) H32A(0.032) H33A(0.044) H34A(0.042) H35A(0.035) H36A(0.028)
 H1SA(0.037) H1SB(0.037) H2SA(0.046) H2SB(0.046) H3SA(0.039) H3SB(0.039)
 H4SA(0.03) H4SB(0.03) H5SA(0.044) H5SB(0.044) H6SA(0.04) H6SB(0.04)
 H7SA(0.043) H7SB(0.043) H8SA(0.04) H8SB(0.04) H9SA(0.041) H9SB(0.041)
 H10B(0.031) H10C(0.031) H11B(0.03) H11C(0.03) H12B(0.035) H12C(0.035)
 Fixed X: H2A(0.2493) H3A(0.3483) H4A(0.4356) H5A(0.4251) H6A(0.3273)
 H8A(0.3345) H9A(0.4313) H10A(0.4241) H11A(0.3203) H12A(0.2222) H14A(0.1513)
 H15A(0.2035) H16A(0.2545) H17A(0.2508) H18A(0.195) H20A(-0.1215) H21A(-0.1249)
 H22A(-0.0933) H23A(-0.0625) H24A(-0.0576) H26A(0.1156) H27A(0.1769)
 H28A(0.1422) H29A(0.0404) H30A(-0.0245) H32A(0.0306) H33A(0.0699) H34A(0.0759)
 H35A(0.0361) H36A(-0.0036) H1SA(0.1173) H1SB(0.1436) H2SA(0.0552) H2SB(0.0981)
 H3SA(-0.0773) H3SB(-0.0495) H4SA(-0.0326) H4SB(0.0098) H5SA(-0.2402) H5SB(-
 0.2957) H6SA(-0.3458) H6SB(-0.3441) H7SA(-0.2122) H7SB(-0.2678) H8SA(-0.1627)
 H8SB(-0.1587) H9SA(-0.29) H9SB(-0.283) H10B(-0.3761) H10C(-0.3279) H11B(-
 0.2439) H11C(-0.2367) H12B(-0.1988) H12C(-0.151)
 Fixed Y: H2A(0.4969) H3A(0.4602) H4A(0.4174) H5A(0.4131) H6A(0.4504)
 H8A(0.5581) H9A(0.5198) H10A(0.4387) H11A(0.3983) H12A(0.4365) H14A(0.7392)
 H15A(0.7661) H16A(0.6873) H17A(0.5799) H18A(0.5518) H20A(0.4808) H21A(0.454)
 H22A(0.3511) H23A(0.2744) H24A(0.3025) H26A(0.3333) H27A(0.2569) H28A(0.1506)
 H29A(0.1219) H30A(0.1987) H32A(0.1737) H33A(0.0766) H34A(0.0608) H35A(0.1391)
 H36A(0.2361) H1SA(0.3962) H1SB(0.353) H2SA(0.28) H2SB(0.2877) H3SA(0.3765)
 H3SB(0.3334) H4SA(0.4418) H4SB(0.4505) H5SA(0.3478) H5SB(0.3595) H6SA(0.2595)
 H6SB(0.3021) H7SA(0.1632) H7SB(0.1767) H8SA(0.2198) H8SB(0.2619) H9SA(0.3248)
 H9SB(0.2757) H10B(0.2458) H10C(0.2411) H11B(0.1595) H11C(0.1103) H12B(0.1934)
 H12C(0.1889)
 Fixed Z: H2A(1.1671) H3A(1.2027) H4A(1.1582) H5A(1.0784) H6A(1.0424)
 H8A(0.9753) H9A(0.9392) H10A(0.8835) H11A(0.8632) H12A(0.8978) H14A(0.8628)
 H15A(0.7929) H16A(0.7479) H17A(0.7713) H18A(0.8393) H20A(0.7928) H21A(0.7146)
 H22A(0.6909) H23A(0.7458) H24A(0.8241) H26A(0.8851) H27A(0.8447) H28A(0.8432)
 H29A(0.8776) H30A(0.9158) H32A(0.9984) H33A(1.0281) H34A(1.1084) H35A(1.1578)
 H36A(1.1288) H1SA(1.243) H1SB(1.2007) H2SA(1.2127) H2SB(1.2595) H3SA(1.2473)
 H3SB(1.2054) H4SA(1.1888) H4SB(1.2357) H5SA(0.8546) H5SB(0.8942) H6SA(0.878)
 H6SB(0.8318) H7SA(0.8491) H7SB(0.8884) H8SA(0.9119) H8SB(0.8655) H9SA(1.0212)
 H9SB(1.0636) H10B(1.0169) H10C(0.9724) H11B(0.9691) H11C(1.0115) H12B(1.0601)
 H12C(1.0154)
;