Slow magnetic dynamics in centrosymmetric didysprosium and equilateral triangular tridysprosium molecules.
Wu, Si-Guo; Zhan, Chang-Ye; Huang, Guo-Zhang; Ruan, Ze-Yu; Liu, Jun-Liang; Tong, Ming-Liang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4164–4171; doi:10.1039/d0dt00481b

data_7703968
_publ_section_title
;
 Slow magnetic dynamics in centrosymmetric didysprosium and equilateral
 triangular tridysprosium molecules.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4164
_journal_page_last               4171
_journal_paper_doi               10.1039/d0dt00481b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C136 H94 Dy3 N6 O11, 0.33(H3 O3), 7(H2 O), 3(CH2Cl2)'
_chemical_formula_sum            'C139 H115 Cl6 Dy3 N6 O19'
_chemical_formula_weight         2873.56
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-09 deposited with the CCDC.	2020-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.1474(8)
_cell_length_b                   22.1474(8)
_cell_length_c                   45.8653(18)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.181
_cell_measurement_theta_min      2.271
_cell_volume                     19483.2(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            37695
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.265
_diffrn_reflns_theta_min         2.170
_exptl_absorpt_coefficient_mu    1.899
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1086 before and 0.0488 after correction. The Ratio of minimum to maximum transmission is 0.7126. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             8658
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.091
_refine_diff_density_max         2.335
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         10729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0942P)^2^+80.1877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7752
_reflns_number_total             10729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00481b2.cif
_cod_data_source_block           Dy3
_cod_original_cell_volume        19483.2(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7703968
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H4 of O4, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H6 of O6
2. Others
 Fixed Sof: H46A(0.33333) H46B(0.33333) H46C(0.33333) H6(0.33333)
3.a Riding coordinates:
 O6(H6), O7(H7A,H7B)
3.b Ternary CH refined with riding coordinates:
 O4(H4)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4A), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13),
  C14(H14), C15(H15), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
 C25(H25), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C36(H36),
  C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44)
3.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              13080
_shelx_fab_checksum              43730