Designing asymmetric Dy<sub>2</sub> single-molecule magnets with two-step relaxation processes by the modification of the coordination environments of Dy(iii) ions.
Huang, Yuan; Li, Jia-Xin; Ge, Yu; Zhang, Xia-Mei; Xu, Yang; Li, Yahong; Zhang, Yi-Quan; Yao, Jin-Lei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8976–8984; doi:10.1039/d0dt01619e

data_7704642
_publ_section_title
;
 Designing asymmetric Dy<sub>2</sub> single-molecule magnets with two-step
 relaxation processes by the modification of the coordination environments
 of Dy(iii) ions.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8976
_journal_page_last               8984
_journal_paper_doi               10.1039/d0dt01619e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C47 H43 Cl3 Dy2 N4 O13, 0.5(C2 H5 O)'
_chemical_formula_sum            'C48 H45.5 Cl3 Dy2 N4 O13.5'
_chemical_formula_weight         1325.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-05 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                68.245(2)
_cell_angle_beta                 75.962(2)
_cell_angle_gamma                79.189(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8154(6)
_cell_length_b                   15.4086(9)
_cell_length_c                   19.4191(12)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.45
_cell_volume                     2630.7(3)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97882
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.588
_diffrn_reflns_theta_min         2.151
_exptl_absorpt_coefficient_mu    3.036
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1514 before and 0.0866 after correction.
The Ratio of minimum to maximum transmission is 0.6355.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       block
_exptl_crystal_F_000             1305
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         12144
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+7.4032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10088
_reflns_number_total             12144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01619e2.cif
_cod_data_source_block           t11
_cod_depositor_comments
'Adding full bibliography for 7704641--7704642.cif.'
_cod_original_formula_sum        'C48 H45.50 Cl3 Dy2 N4 O13.50'
_cod_database_code               7704642
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12-H12
 0.85 with sigma of 0.01
 C49-O14
 2.45 with sigma of 0.01
 C42-H12
 1.927201 with sigma of 0.02
 Dy2-H12
 2.95214 with sigma of 0.02
3. Rigid bond restraints
 C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C44, C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C46: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C44 \\sim C45 \\sim C46: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C44, C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O14, C48, C49
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6. Others
 Fixed Sof: O14(0.5) C48(0.5) H48A(0.5) H48B(0.5) C49(0.5) H49A(0.5) H49B(0.5)
 H49C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C17(H17A,H17B), C40(H40A,H40B), C42(H42A,H42B), C48(H48A,H48B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C8(H8), C14(H14), C15(H15), C20(H20), C21(H21),
 C25(H25), C27(H27), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37),
  C39(H39), C41(H41), C44(H44), C45(H45), C46(H46)
7.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C38(H38A,H38B,H38C), C43(H43A,H43B,H43C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              26150
_olex2_submission_special_instructions 'No special instructions were received'