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_7044096
_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         '0.5(C180 H204 Cu8 K4 N12 Na4 O60 Si24)'
_chemical_formula_sum            'C90 H102 Cu4 K2 N6 Na2 O30 Si12'
_chemical_formula_weight         2463.19
_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
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-10 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3886(3)
_cell_length_b                   27.7686(5)
_cell_length_c                   26.0338(5)
_cell_measurement_reflns_used    9332
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.33
_cell_measurement_theta_min      3.18
_cell_volume                     10883.2(4)
_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)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69006
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.705
_diffrn_reflns_theta_min         3.339
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.562
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1491 before and 0.0541 after correction. The Ratio of minimum to maximum transmission is 0.7114. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+91.5120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8765
_reflns_number_total             9401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02017a2.cif
_cod_data_source_block           yaa185
_cod_database_code               7044096
_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. Restrained distances
 N3-C8 = N3-C9
 1.48 with sigma of 0.005
 N3-C7
 1.34 with sigma of 0.005
 O14-C7
 1.22 with sigma of 0.005
 O16-C64
 1.22 with sigma of 0.005
 N4-C66
 1.49 with sigma of 0.005
 N4-C65
 1.48 with sigma of 0.005
 N4-C64
 1.37 with sigma of 0.005
 O16-N4
 2.301 with sigma of 0.01
 C65-C66
 2.5 with sigma of 0.01
 C8-C9
 2.5 with sigma of 0.01
 C8-C7
 2.4 with sigma of 0.01
 C9-O14
 2.701 with sigma of 0.01
3. Restrained planarity
 O14, C7, N3, C8, C9
 with sigma of 0.05
 O16, C64, N4, C66, C65
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
C61 \\sim C55: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C63 \\sim C57: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C52 \\sim C58: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C53 \\sim C59: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C59 \\sim C53: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C55 \\sim C61: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C54 \\sim C60: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C62 \\sim C56: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
5. Others
 Fixed Sof: O14(0.5) O16(0.5) N3(0.5) N4(0.5) C7(0.5) H7(0.5) C8(0.5) H8A(0.5)
 H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C28(0.5) C33(0.5)
 H33(0.5) C32(0.5) H32(0.5) C31(0.5) H31(0.5) C30(0.5) H30(0.5) C29(0.5)
 H29(0.5) C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5) H39(0.5) C34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) C44(0.5) H44(0.5) C43(0.5) H43(0.5)
 C42(0.5) H42(0.5) C41(0.5) H41(0.5) C40(0.5) C45(0.5) H45(0.5) C49(0.5)
 H49(0.5) C50(0.5) H50(0.5) C51(0.5) H51(0.5) C46(0.5) C47(0.5) H47(0.5)
 C48(0.5) H48(0.5) C56(0.25) H56(0.25) C55(0.25) H55(0.25) C54(0.25) H54(0.25)
 C53(0.25) H53(0.25) C52(0.25) C57(0.25) H57(0.25) C59(0.75) H59(0.75)
 C58(0.75) C63(0.75) H63(0.75) C62(0.75) H62(0.75) C61(0.75) H61(0.75)
 C60(0.75) H60(0.75) C64(0.5) H64(0.5) C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5)
 C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5)
 Fixed Uiso: O14(0.15849) O16(0.11315) N3(0.1608) N4(0.12435) C7(0.12287)
 C8(0.14208) C9(0.14794) C54(0.11863) C62(0.11032) C64(0.10793) C65(0.11768)
 C66(0.11893)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C33(H33), C32(H32), C31(H31), C30(H30), C29(H29),
 C37(H37), C38(H38), C39(H39), C35(H35), C36(H36), C44(H44), C43(H43), C42(H42),
  C41(H41), C45(H45), C49(H49), C50(H50), C51(H51), C47(H47), C48(H48),
 C56(H56), C55(H55), C54(H54), C53(H53), C57(H57), C59(H59), C63(H63), C62(H62),
  C61(H61), C60(H60), C64(H64)
6.b Fitted hexagon refined as free rotating group:
 C28(C33,C32,C31,C30,C29), C37(C38,C39,C34,C35,C36), C44(C43,C42,C41,C40,C45),
 C49(C50,C51,C46,C47,C48), C56(C55,C54,C53,C52,C57), C59(C58,C63,C62,C61,C60)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              25658
_olex2_submission_special_instructions 'No special instructions were received'