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_7044089
_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
'C80 H72 Cu4 N4 Na2 O24 Si12, 2(C9 H14 N), 4(C2 H3 N)'
_chemical_formula_sum            'C106 H112 Cu4 N10 Na2 O24 Si12'
_chemical_formula_weight         2547.27
_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     direct
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3032(10)
_cell_length_b                   20.2902(10)
_cell_length_c                   29.2211(15)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.16
_cell_volume                     11784.6(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            70369
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.868
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0839 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.7842.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5264
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         15213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0655P)^2^+23.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11326
_reflns_number_total             15213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02017a2.cif
_cod_data_source_block           732
_cod_database_code               7044089
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C41(0.5) H41A(0.5)
 H41B(0.5) H41C(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) H38C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5)
3.a Me refined with riding coordinates:
 C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C18(H18), C32(H32), C15(H15), C16(H16), C12(H12), C17(H17),
 C26(H26), C28(H28), C11(H11), C35(H35), C10(H10), C9(H9), C36(H36), C2(H2),
 C33(H33), C27(H27), C34(H34), C20(H20), C6(H6), C48(H48), C30(H30), C3(H3),
 C29(H29), C24(H24), C21(H21), C4(H4), C22(H22), C44(H44), C5(H5), C47(H47),
 C46(H46), C23(H23), C45(H45)
3.c Idealised Me refined as rotating group:
 C6S(H6SA,H6SB,H6SC), C2S(H2SA,H2SB,H2SC), C8S(H8SA,H8SB,H8SC), C4S(H4SA,H4SB,
 H4SC)
;
_shelx_res_checksum              52167
_olex2_submission_special_instructions 'No special instructions were received'