Tuning the coordination sphere of octahedral Dy(iii) complexes with silanolate/stannanolate ligands: synthesis, structures and slow relaxation of the magnetization
Long, Jérôme; Tolpygin, Aleksei O.; Cherkasov, Anton V.; Nelyubina, Yulia V.; Guari, Yannick; Larionova, Joulia; Trifonov, Alexander A.; CrystEngComm 23 (2021) 8351–8359; doi:10.1039/D1CE01266E

data_7243882
_publ_section_title
;
 Tuning the coordination sphere of octahedral Dy(iii) complexes with
 silanolate/stannanolate ligands: synthesis, structures and slow
 relaxation of the magnetization
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              8351
_journal_page_last               8359
_journal_paper_doi               10.1039/D1CE01266E
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'C104 H124 Dy2 O12 Si4, 2(C24 H20 B), 2(C4 H8 O), C3 H3'
_chemical_formula_sum            'C163 H183 B2 Dy2 O14 Si4'
_chemical_formula_weight         2825.06
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-07-10 deposited with the CCDC.	2021-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.5840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   46.8542(19)
_cell_length_b                   18.1479(8)
_cell_length_c                   18.2239(8)
_cell_measurement_reflns_used    5879
_cell_measurement_temperature    120
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      2.24
_cell_volume                     14307.6(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_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_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54365
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.804
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3701
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0722 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8547.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       prism
_exptl_crystal_F_000             5884
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.263
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         12598
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0488P)^2^+141.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8557
_reflns_number_total             12598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01266e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7243882--7243885.cif.'
_cod_database_code               7243882
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Si1-C7' \\sim Si1-C7
 with sigma of 0.02
 Si1-C1 \\sim Si1-C1'
 with sigma of 0.02
 Si1-C13 \\sim Si1-C13'
 with sigma of 0.02
 Dy1-O3' \\sim Dy1-O3
 with sigma of 0.02
 O3-C37 \\sim O3'-C37'
 with sigma of 0.02
 C39'-C38' \\sim C39-C38
 with sigma of 0.02
 O3-C40 \\sim O3'-C40'
 with sigma of 0.02
 C38-C37 \\sim C38'-C37'
 with sigma of 0.02
 C40'-C39' \\sim C40-C39
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C34') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8S) \\sim Ueq, Uanis(C7S) \\sim Ueq, Uanis(C6S) \\sim Ueq, Uanis(C5S)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C32') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34') \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C37') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C38') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(C40') \\sim Ueq, Uanis(C40)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C36') \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32')
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34') \\sim Ueq, Uanis(C34) \\sim Ueq,
Uanis(C35') \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14') \\sim Ueq, Uanis(C15') \\sim Ueq, Uanis(C16') \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11') \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1S) \\sim Ueq, Uanis(O1S') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1S') \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3S') \\sim Ueq, Uanis(C3S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) = Uanis(C34')
Uanis(C35') = Uanis(C35)
Uanis(C36') = Uanis(C36)
Uanis(C32') = Uanis(C32)
Uanis(C37) = Uanis(C37')
Uanis(C38) = Uanis(C38')
Uanis(C39) = Uanis(C39')
Uanis(O3) = Uanis(O3')
Uanis(C40) = Uanis(C40')
Uanis(C33') = Uanis(C33)
Uanis(C8) = Uanis(C8')
Uanis(C10') = Uanis(C10)
Uanis(C9') = Uanis(C9)
Uanis(C7) = Uanis(C12)
Uanis(C11') = Uanis(C11)
Uanis(C12') = Uanis(C12)
Uanis(C7') = Uanis(C7)
Uanis(C13) = Uanis(C13')
Uanis(C18) = Uanis(C18')
Uanis(C17) = Uanis(C17')
Uanis(C16') = Uanis(C16)
Uanis(C15') = Uanis(C15)
Uanis(C14) = Uanis(C14')
Uanis(C5) = Uanis(C5')
Uanis(C6) = Uanis(C6')
Uanis(C4') = Uanis(C4)
Uanis(C1) = Uanis(C1')
Uanis(C3') = Uanis(C3)
Uanis(C2') = Uanis(C2)
Uanis(O1S') = Uanis(O1S)
Uanis(C4S) = Uanis(C4S')
Uanis(C1S) = Uanis(C1S')
Uanis(C2S) = Uanis(C2S')
Uanis(C3S) = Uanis(C3S')
4. Others
 Sof(C32')=Sof(H32')=Sof(C33')=Sof(H33')=Sof(C34')=Sof(H34')=Sof(C35')=
 Sof(H35')=Sof(C36')=Sof(H36')=1-FVAR(1)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=
 Sof(C36)=Sof(H36)=FVAR(1)
 Sof(C8')=Sof(H8')=Sof(C9')=Sof(H9')=Sof(C10')=Sof(H10')=Sof(C11')=Sof(H11')=
 Sof(C12')=Sof(H12')=Sof(C7')=1-FVAR(2)
 Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=FVAR(2)
 Sof(C13')=Sof(C14')=Sof(H14')=Sof(C15')=Sof(H15')=Sof(C16')=Sof(H16')=
 Sof(C17')=Sof(H17')=Sof(C18')=Sof(H18')=1-FVAR(3)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=FVAR(3)
 Sof(C1')=Sof(C6')=Sof(H6')=Sof(C5')=Sof(H5')=Sof(C4')=Sof(H4')=Sof(C3')=
 Sof(H3')=Sof(C2')=Sof(H2')=1-FVAR(4)
 Sof(C1)=Sof(C6)=Sof(H6)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=
 Sof(C2)=Sof(H2)=FVAR(4)
 Sof(O1S')=Sof(C1S')=Sof(H1SA)=Sof(H1SB)=Sof(C2S')=Sof(H2SA)=Sof(H2SB)=
 Sof(C3S')=Sof(H3SA)=Sof(H3SB)=Sof(C4S')=Sof(H4SA)=Sof(H4SB)=1-FVAR(5)
 Sof(O1S)=Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(C2S)=Sof(H2SC)=Sof(H2SD)=Sof(C3S)=
 Sof(H3SC)=Sof(H3SD)=Sof(C4S)=Sof(H4SC)=Sof(H4SD)=FVAR(5)
 Sof(O3')=Sof(C37')=Sof(H37C)=Sof(H37D)=Sof(C38')=Sof(H38C)=Sof(H38D)=
 Sof(C39')=Sof(H39C)=Sof(H39D)=Sof(C40')=Sof(H40C)=Sof(H40D)=1-FVAR(6)
 Sof(O3)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(6)
 Fixed Sof: C5S(0.25) H5S(0.25) C6S(0.5) H6S(0.5) C7S(0.5) H7S(0.5) C8S(0.25)
 H8S(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B), C37'(H37C,H37D), C38'(H38C,H38D), C39'(H39C,
 H39D), C40'(H40C,H40D), C1S'(H1SA,H1SB), C2S'(H2SA,H2SB), C3S'(H3SA,H3SB),
 C4S'(H4SA,H4SB), C1S(H1SC,H1SD), C2S(H2SC,H2SD), C3S(H3SC,H3SD), C4S(H4SC,H4SD)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C32'(H32'), C33'(H33'), C34'(H34'), C35'(H35'), C36'(H36'), C6'(H6'),
  C5'(H5'), C4'(H4'), C3'(H3'), C2'(H2'), C8'(H8'), C9'(H9'), C10'(H10'),
 C11'(H11'), C12'(H12'), C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17'),
 C18'(H18'), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
  C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72),
 C73(H73), C74(H74), C75(H75), C76(H76), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S)
5.c Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C7(C8,C9,C10,C11,C12), C13(C14,C15,C16,C17,C18), C1'(C6',
 C5',C4',C3',C2'), C8'(C9',C10',C11',C12',C7'), C13'(C14',C15',C16',C17',C18')
;
_shelx_res_checksum              60253
_olex2_submission_special_instructions 'No special instructions were received'