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_7243883
_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         'C66 H69 Dy O6 Si3, C4 H8 O'
_chemical_formula_sum            'C70 H77 Dy O7 Si3'
_chemical_formula_weight         1277.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-09-17 deposited with the CCDC.	2021-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.635(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.334(2)
_cell_length_b                   16.468(2)
_cell_length_c                   14.540(2)
_cell_measurement_reflns_used    2933
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.47
_cell_volume                     3144.3(7)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.1365
_diffrn_reflns_av_unetI/netI     0.1443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.966
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1016 before and 0.0892 after correction.
The Ratio of minimum to maximum transmission is 0.8113.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       prism
_exptl_crystal_F_000             1322
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.287
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         12339
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9051
_reflns_number_total             12339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01266e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7243882--7243885.cif.'
_cod_original_cell_volume        3144.3(8)
_cod_database_code               7243883
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.983(15)
 0.017(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66') = Uanis(C66)
Uanis(C65) = Uanis(C65')
Uanis(C64) = Uanis(C64')
4. Others
 Sof(H63C)=Sof(H63D)=Sof(C64')=Sof(H64C)=Sof(H64D)=Sof(C65')=Sof(H65C)=
 Sof(H65D)=Sof(C66')=Sof(H66C)=Sof(H66D)=1-FVAR(1)
 Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C63(H63C,H63D), C64(H64A,H64B), C64'(H64C,H64D), C65(H65A,H65B), C65'(H65C,
 H65D), C66(H66A,H66B), C66'(H66C,H66D), C1S(H1SA,H1SB), C2S(H2SA,H2SB),
 C3S(H3SA,H3SB), C4S(H4SA,H4SB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
;
_shelx_res_checksum              57694
_olex2_submission_special_instructions 'No special instructions were received'