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_7044090
_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         'C90 H102 Cs2 Cu4 N6 Na2 O30 Si12, 0.5(H2 O)'
_chemical_formula_sum            'C90 H103 Cs2 Cu4 N6 Na2 O30.5 Si12'
_chemical_formula_weight         2659.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                86.5740(10)
_cell_angle_beta                 68.2550(10)
_cell_angle_gamma                70.2400(10)
_cell_formula_units_Z            1
_cell_length_a                   13.5529(4)
_cell_length_b                   15.0155(5)
_cell_length_c                   15.3739(5)
_cell_measurement_reflns_used    9444
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.59
_cell_measurement_theta_min      3.10
_cell_volume                     2727.21(15)
_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 0.911
_diffrn_measured_fraction_theta_max 0.971
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33847
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.968
_diffrn_reflns_theta_min         3.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.003
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1185 before and 0.0382 after correction. The Ratio of minimum to maximum transmission is 0.6390. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1345
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.948
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         8993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+1.6087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8837
_reflns_number_total             8993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02017a2.cif
_cod_data_source_block           656dmf
_cod_original_formula_sum        'C90 H103 Cs2 Cu4 N6 Na2 O30.50 Si12'
_cod_database_code               7044090
_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, All O(H,H) groups
2. Others
 Fixed Sof: O14(0.25) H14A(0.25) H14B(0.25)
3.a Riding coordinates:
 O14(H14A,H14B)
3.b Ternary CH refined with riding coordinates:
 C7(H7)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), 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), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45)
3.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3C,H3B,H3A), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8B,
 H8C,H8A), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              29890
_olex2_submission_special_instructions 'No special instructions were received'