Bi- and Tri-metallic Cage Silsesquioxanes: Features of Supramolecular Assembling and Magnetic Properties
Bilyachenko, Alexey; Korlyukov, Aleksander; Vologzhanina, Anna V. V.; Khrustalev, Victor N.; Kulakova, Alena Nikolaevna; Long, Jerome; Larionova, Joulia; Guari, Yannick; Dronova, Marina; Tsareva, Ulyana; Dorovatovskii, Pavel; Shubina, Elena; Levitsky, Mikhail; Dalton Trans.  (2017) –; doi:10.1039/C7DT02017A

data_7044092
_publ_section_title
;
 Bi- and Tri-metallic Cage Silsesquioxanes: Features of Supramolecular
 Assembling and Magnetic Properties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02017A
_journal_year                    2017
_chemical_formula_moiety         'C84 H88 Cs Cu4 N4 Na3 O28 Si12'
_chemical_formula_sum            'C84 H88 Cs Cu4 N4 Na3 O28 Si12'
_chemical_formula_weight         2394.70
_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   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-07-25 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.330(3)
_cell_length_b                   27.390(6)
_cell_length_c                   26.060(5)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      3.6
_cell_volume                     10728(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 0.796
_diffrn_measured_fraction_theta_max 0.736
_diffrn_measurement_device_type  'MAR CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.1687
_diffrn_reflns_Laue_measured_fraction_full 0.796
_diffrn_reflns_Laue_measured_fraction_max 0.736
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39087
_diffrn_reflns_point_group_measured_fraction_full 0.796
_diffrn_reflns_point_group_measured_fraction_max 0.736
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.293
_diffrn_reflns_theta_min         3.568
_exptl_absorpt_coefficient_mu    3.084
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       prism
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0037(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   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         8621
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.2057
_refine_ls_R_factor_gt           0.1283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+90P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2857
_refine_ls_wR_factor_ref         0.3454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3879
_reflns_number_total             8621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02017a2.cif
_cod_data_source_block           PAA91
_cod_database_code               7044092
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.745
_shelxl_version_number           2014/6
_shelx_res_checksum              64190