Engineering dysprosium(iii) single-ion magnets via modular synthesis with strongly axial ligands
Zhang, Kun-Hua; He, Zhi; Huang, Long; Yu, Xing-Yi; Zhao, Bingshan; Yang, Jiong; Shao, Dong; CrystEngComm 27 (2025) 5662–5668; doi:10.1039/D5CE00636H

data_7250700
_publ_section_title
;
 Engineering dysprosium(iii) single-ion magnets via modular synthesis with
 strongly axial ligands
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              5662
_journal_page_last               5668
_journal_paper_doi               10.1039/D5CE00636H
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C48 H34 Cl6 Dy N4 O5 Si'
_chemical_formula_sum            'C48 H34 Cl6 Dy N4 O5 Si'
_chemical_formula_weight         1150.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-07-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-17 deposited with the CCDC.	2025-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.079(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.347(3)
_cell_length_b                   9.7398(11)
_cell_length_c                   20.919(2)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.27
_cell_volume                     4715.7(9)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1439 before and 0.0855 after correction.
The Ratio of minimum to maximum transmission is 0.6704.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9671
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+5.5214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7077
_reflns_number_total             9671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00636h2.cif
_cod_data_source_block           dy3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7250699--7250700.cif.
;
_cod_original_cell_volume        4715.8(9)
_cod_database_code               7250700
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O5 \\sim N16 \\sim C3 \\sim C41 \\sim C47 \\sim N16A \\sim C3A \\sim C41A \\sim
C47A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
3. Same fragment restrains
{O5, N16A, C3A, C41A, C47A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O5, N16, C3, C41, C47}
4. Others
 Sof(N16A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C41A)=Sof(H41A)=
 Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=1-FVAR(1)
 Sof(N16)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C41)=Sof(H41)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C41(H41), C2(H2), C5(H5), C9(H9), C11(H11), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C27(H27), C29(H29), C30(H30),
  C31(H31), C33(H33), C34(H34), C35(H35), C37(H37), C40(H40), C42(H42),
 C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C41A(H41A)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C47(H47A,H47B,H47C), C3A(H3AA,H3AB,H3AC), C47A(H47D,H47E,H47F)
;
_shelx_res_checksum              27231
_olex2_submission_special_instructions 'No special instructions were received'