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_7243884
_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_absolute_configuration ad
_chemical_formula_moiety         'C68 H61 Dy N2 O4 Si3, C4 H8 O'
_chemical_formula_sum            'C72 H69 Dy N2 O5 Si3'
_chemical_formula_weight         1289.06
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-10 deposited with the CCDC.	2021-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.8060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2745(4)
_cell_length_b                   16.2901(5)
_cell_length_c                   15.0762(4)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.72
_cell_volume                     3156.10(16)
_computing_cell_refinement       'Saint 8.37a'
_computing_data_collection       APEX3
_computing_data_reduction        'Saint 8.37a'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_structure_solution    'SHELXT 2018/2'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52387
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.111
_diffrn_reflns_theta_min         2.501
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 6626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         18482
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0201P)^2^+0.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                15818
_reflns_number_total             18482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01266e2.cif
_cod_data_source_block           dyosiph3bipy
_cod_depositor_comments
'Adding full bibliography for 7243882--7243885.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7243884
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              55526