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_7044093
_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
'C92 H105 Cu4 Na4 O37 Si12, 2(C7 H5 N), 2(C4 H8 O2), H2 O'
_chemical_formula_sum            'C114 H133 Cu4 N2 Na4 O42 Si12'
_chemical_formula_weight         2886.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-05
_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                 104.474(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.936(4)
_cell_length_b                   24.531(5)
_cell_length_c                   26.959(6)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.21
_cell_volume                     12766(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            24993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.414
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             5980
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.883
_refine_diff_density_min         -2.726
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1528
_refine_ls_number_reflns         24993
_refine_ls_number_restraints     1321
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0979
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+200.3398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13981
_reflns_number_total             24993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02017a2.cif
_cod_data_source_block           lab595
_cod_database_code               7044093
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.750(3)
 0.250(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C4A-C3A
 1.52 with sigma of 0.005
 C7B-C0AA = C6A-C5A = C6B-C5B = C7A-C1
 1.5 with sigma of 0.005
 O28-C6A = O28-C6B = O28-C7B = O28-C7A = O27-C0AA = O27-C5B = O27-C5A = O27-C1
 1.41 with sigma of 0.005
 O25-C4B \\sim O25-C4A \\sim O25-C1B \\sim O25-C1A \\sim O26B-C2B \\sim
O26A-C2A \\sim O26A-C3A \\sim O26B-
 C3B
 with sigma of 0.005
 C4B-C3B \\sim C4A-C3A \\sim C2B-C1B \\sim C2A-C1A
 with sigma of 0.05
 C20B-C19B \\sim C20A-C19A \\sim C18A-C17A \\sim C18B-C17B
 with sigma of 0.005
 O29-C20A \\sim O29-C20B \\sim O29-C17A \\sim O29-C17B \\sim O30B-C18B \\sim
O30A-C18A \\sim O30B-C19B
 \\sim O30A-C19A
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(O4)
\\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.006
Uanis(C94) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.006
Uanis(C66) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.006
Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of
0.006 and sigma for terminal atoms of 0.006
Uanis(C9) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(O1AA) = Uanis(O0AA)
Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84)
Uanis(O15) = Uanis(O24)
Uanis(C9) = Uanis(C8) = Uanis(O31)
5. Rigid body (RIGU) restrains
 C41, C46, C45, C44, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C51B(0.5) C52B(0.5) H52B(0.5) C53B(0.5) H53B(0.5) C54B(0.5)
 H54B(0.5) C55B(0.5) H55B(0.5) C56B(0.5) H56B(0.5) O26B(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) O30B(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) C4B(0.5) H4BA(0.5) H4BB(0.5)
 C17B(0.5) H17A(0.5) H17B(0.5) C18B(0.5) H18A(0.5) H18B(0.5) C20B(0.5)
 H20A(0.5) H20B(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5)
 C3B(0.5) H3BA(0.5) H3BB(0.5) C19B(0.5) H19A(0.5) H19B(0.5) C51A(0.5) C56A(0.5)
 H56A(0.5) C55A(0.5) H55A(0.5) C54A(0.5) H54A(0.5) C53A(0.5) H53A(0.5)
 C52A(0.5) H52A(0.5) O0AA(0.5) O1AA(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) C7B(0.5)
 H7BA(0.5) H7BB(0.5) O26A(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) C1A(0.5) H1AA(0.5)
 H1AB(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) O30A(0.5)
 C19A(0.5) H19C(0.5) H19D(0.5) C20A(0.5) H20C(0.5) H20D(0.5) C17A(0.5)
 H17C(0.5) H17D(0.5) C18A(0.5) H18C(0.5) H18D(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5)
 C6A(0.5) H6AA(0.5) H6AB(0.5) C1(0.5) H1A(0.5) H1B(0.5) C7A(0.5) H7AA(0.5)
 H7AB(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C68(H68A,H68B), C67(H67A,H67B), C9(H9A,H9B), C50(H50A,H50B),
 C40(H40A,H40B), C1B(H1BA,H1BB), C39(H39A,H39B), C37(H37A,H37B), C47(H47A,H47B),
  C49(H49A,H49B), C48(H48A,H48B), C6B(H6BA,H6BB), C60(H60A,H60B), C4B(H4BA,
 H4BB), C38(H38A,H38B), C17B(H17A,H17B), C18B(H18A,H18B), C57(H57A,H57B),
 C59(H59A,H59B), C20B(H20A,H20B), C5B(H5BA,H5BB), C2B(H2BA,H2BB), C3B(H3BA,
 H3BB), C19B(H19A,H19B), C58(H58A,H58B), C0AA(H0AA,H0AB), C7B(H7BA,H7BB),
 C2A(H2AA,H2AB), C1A(H1AA,H1AB), C4A(H4AA,H4AB), C3A(H3AA,H3AB), C19A(H19C,
 H19D), C20A(H20C,H20D), C17A(H17C,H17D), C18A(H18C,H18D), C5A(H5AA,H5AB),
 C6A(H6AA,H6AB), C1(H1A,H1B), C7A(H7AA,H7AB)
7.b Aromatic/amide H refined with riding coordinates:
 C116(H116), C82(H82), C76(H76), C52B(H52B), C53B(H53B), C54B(H54B),
 C55B(H55B), C56B(H56B), C126(H126), C112(H112), C14(H14), C114(H114), C84(H84),
  C22(H22), C74(H74), C124(H124), C72(H72), C123(H123), C73(H73), C113(H113),
 C85(H85), C23(H23), C122(H122), C62(H62), C83(H83), C103(H103), C115(H115),
 C125(H125), C32(H32), C13(H13), C12(H12), C102(H102), C16(H16), C36(H36),
 C75(H75), C92(H92), C106(H106), C131(H131), C128(H128), C34(H34), C44(H44),
 C127(H127), C42(H42), C104(H104), C95(H95), C15(H15), C96(H96), C129(H129),
 C64(H64), C66(H66), C93(H93), C33(H33), C105(H105), C136(H136), C43(H43),
 C35(H35), C132(H132), C138(H138), C63(H63), C135(H135), C65(H65), C134(H134),
 C139(H139), C94(H94), C46(H46), C25(H25), C45(H45), C26(H26), C24(H24),
 C56A(H56A), C55A(H55A), C54A(H54A), C53A(H53A), C52A(H52A)
7.c Fitted hexagon refined as free rotating group:
 C51B(C52B,C53B,C54B,C55B,C56B), C51A(C56A,C55A,C54A,C53A,C52A)
;
_shelx_res_checksum              22346
_olex2_submission_special_instructions 'No special instructions were received'