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_7044095
_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 H92 Cu4 Na4 O30 Si12, 0.5(C2 H6 O)'
_chemical_formula_sum            'C85 H95 Cu4 Na4 O30.5 Si12'
_chemical_formula_weight         2287.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-07-10 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 131.7610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.0472(11)
_cell_length_b                   12.7721(3)
_cell_length_c                   28.8454(14)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    120
_cell_measurement_theta_max      66.24
_cell_measurement_theta_min      3.03
_cell_volume                     10730.7(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26975
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.237
_diffrn_reflns_theta_min         3.034
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.947
_exptl_absorpt_correction_T_max  0.4657
_exptl_absorpt_correction_T_min  0.2906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.6240.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4708
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.025
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         13525
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+150.6861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                10995
_reflns_number_total             13525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02017a2.cif
_cod_data_source_block           a
_cod_original_formula_sum        'C85 H95 Cu4 Na4 O30.50 Si12'
_cod_database_code               7044095
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: O22(0.5) H22(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5)
 H10B(0.5) H10C(0.5) C34(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5) C23(0.5)
 H23(0.5) C21(0.5) H21(0.5) C22(0.5) H22A(0.5) O24(0.5) H24(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) O25(0.5) H25(0.5)
 C38(0.5) C14(0.5) H14(0.5) C13(0.5) H13(0.5) C39(0.5) H39(0.5) C12(0.5)
 H12(0.5) C11(0.5) H11(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) O42(0.5) H42(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 H6C(0.5) O44(0.5) H44(0.5) C97(0.5) H97A(0.5) H97B(0.5) C98(0.5) H98A(0.5)
 H98B(0.5) H98C(0.5) O45(0.5) H45A(0.5) C99(0.5) H99A(0.5) H99B(0.5) C100(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C41(0.5) C18(0.5) H18(0.5) C17(0.5) H17(0.5)
 C40(0.5) H40(0.5) C16(0.5) H16(0.5) C15(0.5) H15(0.5) C37(0.5) C26(0.5)
 H26(0.5) C25(0.5) H25A(0.5) C36(0.5) H36(0.5) C24(0.5) H24A(0.5) C4AA(0.5)
 H4AA(0.5) O43(0.5) H43A(0.5) C95(0.5) H95A(0.5) H95B(0.5) C96(0.5) H96A(0.5)
 H96B(0.5) H96C(0.5)
 Fixed Uiso: O22(0.1) H22(0.15) C9(0.15) H9A(0.18) H9B(0.18) C10(0.1)
 H10A(0.15) H10B(0.15) H10C(0.15) C34(0.15) H19(0.075) C20(0.15) H20(0.18)
 H23(0.076) H21(0.083) H22A(0.075) O24(0.15) H24(0.225) C7(0.1) H7A(0.12)
 H7B(0.12) C8(0.1) H8A(0.15) H8B(0.15) H8C(0.15) H25(0.129) O31(0.15) O30(0.15)
 C33(0.15) H33A(0.18) H33B(0.18) C5AA(0.15) H5AA(0.18) H5AB(0.18) C31(0.15)
 H31A(0.18) H31B(0.18) C32(0.15) H32A(0.18) H32B(0.18) H35(0.161) H3A(0.184)
 H3B(0.184) H4A(0.151) H4B(0.151) H4C(0.151) C14(0.15) H14(0.18) H13(0.096)
 C39(0.15) H39(0.18) C12(0.15) H12(0.18) H11(0.107) H1A(0.072) H1B(0.072)
 H2A(0.125) H2B(0.125) H2C(0.125) H42(0.154) C5(0.104) H5A(0.125) H5B(0.125)
 H6A(0.126) H6B(0.126) H6C(0.126) H44(0.144) C97(0.15) H97A(0.18) H97B(0.18)
 C98(0.15) H98A(0.225) H98B(0.225) H98C(0.225) H45A(0.22) C99(0.15) H99A(0.18)
 H99B(0.18) C100(0.15) H10D(0.225) H10E(0.225) H10F(0.225) C18(0.15) H18(0.18)
 H17(0.093) C40(0.15) H40(0.18) C16(0.15) H16(0.18) H15(0.037) C26(0.1)
 H26(0.12) H25A(0.06) H36(0.063) H24A(0.109) H4AA(0.047) H48(0.067) H49(0.071)
 H50(0.075) H51(0.068) H52(0.062) H82(0.087) H81(0.122) H80(0.088) H79(0.088)
 H78(0.059) H6AA(0.096) H2AA(0.097) H1AA(0.112) H0AA(0.158) H7AA(0.106)
 H46(0.101) H42A(0.131) H43(0.101) H44A(0.1) H45(0.142) H58(0.118) H54(0.071)
 H55(0.097) H56(0.13) H57(0.162) H64(0.081) H63(0.118) H62(0.121) H61(0.169)
 H60(0.094) H70(0.083) H69(0.108) H68(0.107) H67(0.134) H66(0.08) H75(0.076)
 H74(0.076) H73(0.083) H72(0.068) H76(0.104) H84(0.057) H85(0.075) H86(0.083)
 H87(0.086) H88(0.071) H94(0.149) H93(0.182) H92(0.135) H91(0.153) H90(0.113)
 H43A(0.178) H95A(0.088) H95B(0.088) H96A(0.154) H96B(0.154) H96C(0.154)
 Fixed X: H22(0.8966) H9A(0.9369) H9B(0.9064) H10A(0.9771) H10B(0.9409)
 H10C(0.9749) H19(0.503) H20(0.4773) H23(0.5304) H21(0.6091) H22A(0.6349)
 H24(0.4908) H7A(0.4162) H7B(0.4553) H8A(0.4111) H8B(0.4361) H8C(0.3868)
 H25(0.6292) H33A(0.7333) H33B(0.753) H5AA(0.7252) H5AB(0.7587) H31A(0.6245)
 H31B(0.6452) H32A(0.6183) H32B(0.6513) H35(0.6984) H3A(0.7763) H3B(0.7636)
 H4A(0.6918) H4B(0.7336) H4C(0.7063) H14(0.8666) H13(0.8966) H39(0.8506)
 H12(0.7746) H11(0.7446) H1A(0.6119) H1B(0.6088) H2A(0.6923) H2B(0.6844)
 H2C(0.686) H42(0.4687) H5A(0.444) H5B(0.4096) H6A(0.3935) H6B(0.4428)
 H6C(0.4041) H44(0.8985) H97A(0.9026) H97B(0.9453) H98A(0.8938) H98B(0.9205)
 H98C(0.9485) H45A(0.5039) H99A(0.4197) H99B(0.4353) H10D(0.4616) H10E(0.415)
 H10F(0.4143) H18(0.817) H17(0.8365) H40(0.8184) H16(0.7807) H15(0.7611)
 H26(0.6109) H25A(0.5983) H36(0.5619) H24A(0.538) H4AA(0.5507) H48(0.6542)
 H49(0.6551) H50(0.7046) H51(0.7532) H52(0.7519) H82(0.5347) H81(0.5216)
 H80(0.5628) H79(0.6171) H78(0.6302) H6AA(0.8306) H2AA(0.8466) H1AA(0.8945)
 H0AA(0.9104) H7AA(0.8785) H46(0.8791) H42A(0.8007) H43(0.8481) H44A(0.9109)
 H45(0.9264) H58(0.578) H54(0.5446) H55(0.5022) H56(0.4978) H57(0.5356)
 H64(0.5293) H63(0.4797) H62(0.4634) H61(0.4968) H60(0.5464) H70(0.4917)
 H69(0.4454) H68(0.465) H67(0.5309) H66(0.5772) H75(0.7631) H74(0.811)
 H73(0.8475) H72(0.836) H76(0.7516) H84(0.6233) H85(0.6209) H86(0.6698)
 H87(0.7212) H88(0.7237) H94(0.8353) H93(0.8775) H92(0.8786) H91(0.8373)
 H90(0.7951) H43A(0.918) H95A(0.9544) H95B(0.9669) H96A(0.9983) H96B(1.025)
 H96C(0.9879)
 Fixed Y: H22(-0.1655) H9A(-0.0329) H9B(-0.1053) H10A(-0.188) H10B(-0.2565)
 H10C(-0.1785) H19(-0.2825) H20(-0.3808) H23(-0.458) H21(-0.4369) H22A(-0.3385)
 H24(0.1532) H7A(0.1862) H7B(0.267) H8A(0.3842) H8B(0.344) H8C(0.2983) H25(-
 0.2741) H33A(0.0927) H33B(0.076) H5AA(-0.0962) H5AB(-0.0804) H31A(-0.0798)
 H31B(-0.0952) H32A(0.0759) H32B(0.0928) H35(-0.2868) H3A(-0.3636) H3B(-0.2451)
 H4A(-0.3883) H4B(-0.4024) H4C(-0.2938) H14(-0.2279) H13(-0.3396) H39(-0.4711)
 H12(-0.4911) H11(-0.3794) H1A(-0.4093) H1B(-0.3371) H2A(-0.3332) H2B(-0.4317)
 H2C(-0.3159) H42(0.0637) H5A(-0.1355) H5B(-0.0524) H6A(0.0239) H6B(-0.0028)
 H6C(-0.0916) H44(-0.1073) H97A(-0.0343) H97B(-0.0698) H98A(-0.237) H98B(-
 0.1723) H98C(-0.2262) H45A(0.2134) H99A(0.1372) H99B(0.1799) H10D(0.3329)
 H10E(0.2963) H10F(0.3346) H18(-0.2025) H17(-0.3233) H40(-0.5005) H16(-0.5569)
 H15(-0.4362) H26(-0.4312) H25A(-0.5502) H36(-0.4951) H24A(-0.321) H4AA(-0.202)
 H48(0.2667) H49(0.445) H50(0.5144) H51(0.4018) H52(0.2244) H82(-0.4417) H81(-
 0.6224) H80(-0.7284) H79(-0.6537) H78(-0.473) H6AA(0.0128) H2AA(0.2064)
 H1AA(0.3144) H0AA(0.2716) H7AA(0.1208) H46(-0.1916) H42A(-0.4443) H43(-0.5495)
 H44A(-0.4757) H45(-0.2968) H58(0.2386) H54(-0.0033) H55(0.1108) H56(0.2887)
 H57(0.3526) H64(0.2016) H63(0.3076) H62(0.2657) H61(0.1178) H60(0.0118) H70(-
 0.1999) H69(-0.3089) H68(-0.4851) H67(-0.5524) H66(-0.4435) H75(-0.6503) H74(-
 0.7261) H73(-0.6206) H72(-0.4392) H76(-0.469) H84(0.2198) H85(0.4002)
 H86(0.5129) H87(0.4452) H88(0.2648) H94(-0.0077) H93(0.1013) H92(0.2823)
 H91(0.3543) H90(0.2453) H43A(-0.4731) H95A(-0.4506) H95B(-0.5409) H96A(-0.333)
 H96B(-0.4349) H96C(-0.3796)
 Fixed Z: H22(1.0969) H9A(1.083) H9B(1.0219) H10A(1.0935) H10B(1.0897)
 H10C(1.1469) H19(0.5896) H20(0.5031) H23(0.5005) H21(0.5844) H22A(0.6709)
 H24(0.6819) H7A(0.5899) H7B(0.6089) H8A(0.6036) H8B(0.6723) H8C(0.6139)
 H25(1.0087) H33A(0.7085) H33B(0.6748) H5AA(0.6489) H5AB(0.7226) H31A(0.6205)
 H31B(0.5881) H32A(0.5727) H32B(0.6463) H35(0.719) H3A(0.7566) H3B(0.7317)
 H4A(0.6549) H4B(0.6571) H4C(0.6346) H14(1.2143) H13(1.2981) H39(1.2887)
 H12(1.1954) H11(1.1116) H1A(1.0325) H1B(1.0758) H2A(1.1) H2B(1.1263)
 H2C(1.149) H42(0.7497) H5A(0.7263) H5B(0.6721) H6A(0.7253) H6B(0.7912)
 H6C(0.7535) H44(1.1135) H97A(1.1993) H97B(1.2064) H98A(1.1945) H98B(1.2577)
 H98C(1.2416) H45A(0.6633) H99A(0.5967) H99B(0.5608) H10D(0.6389) H10E(0.6215)
 H10F(0.5681) H18(1.2153) H17(1.2907) H40(1.2649) H16(1.1638) H15(1.0885)
 H26(0.703) H25A(0.6312) H36(0.5303) H24A(0.5011) H4AA(0.5729) H48(0.8052)
 H49(0.7909) H50(0.7813) H51(0.7833) H52(0.7956) H82(0.6942) H81(0.684)
 H80(0.7726) H79(0.8713) H78(0.8815) H6AA(0.8422) H2AA(0.9668) H1AA(0.9657)
 H0AA(0.9028) H7AA(0.8411) H46(0.9273) H42A(0.8876) H43(0.8841) H44A(0.9022)
 H45(0.9238) H58(0.6868) H54(0.5722) H55(0.4871) H56(0.5018) H57(0.6017)
 H64(0.8259) H63(0.8244) H62(0.887) H61(0.9511) H60(0.9526) H70(0.8568)
 H69(0.8606) H68(0.8882) H67(0.9122) H66(0.9084) H75(0.9221) H74(1.0211)
 H73(1.1091) H72(1.0981) H76(0.9111) H84(0.9951) H85(1.007) H86(1.0105)
 H87(1.0021) H88(0.9903) H94(1.2183) H93(1.3056) H92(1.294) H91(1.1949)
 H90(1.1075) H43A(1.0957) H95A(1.0442) H95B(1.0921) H96A(1.1191) H96B(1.161)
 H96C(1.1602)
;
_shelx_res_checksum              89819
_olex2_submission_special_instructions 'No special instructions were received'