Synergistic construction of highly symmetrical lanthanide single-ion magnets using neutral phosphoryl and anionic thiocyanate ligands.
Liu, Bei; Dong, Xiao-Yan; Gong, Hui-Wen; Sun, Zheng; Sun, Rong; Zhu, Wen-Hua; Zhang, Lei; Sun, Hao-Ling; Zhao, Man-Yun; Huang, Ning-Ning; Bian, Qing-Yan; Gao, Song; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9039–9048; doi:10.1039/d5dt00339c

data_7718589
_publ_section_title
;
 Synergistic construction of highly symmetrical lanthanide single-ion
 magnets using neutral phosphoryl and anionic thiocyanate ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9039
_journal_page_last               9048
_journal_paper_doi               10.1039/d5dt00339c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C27 H52 Dy N9 O10 P2 S3'
_chemical_formula_sum            'C27 H52 Dy N9 O10 P2 S3'
_chemical_formula_weight         983.39
_chemical_name_common            '[Dy(TMPO)2(SCN)3(H2O)2]'
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-03-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-04-15 deposited with the CCDC.	2025-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                69.7420(10)
_cell_angle_beta                 73.8000(10)
_cell_angle_gamma                86.7990(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0947(4)
_cell_length_b                   13.1152(5)
_cell_length_c                   17.2101(7)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    286.1
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.62
_cell_volume                     2050.59(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      286.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24503
_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         25.370
_diffrn_reflns_theta_min         2.618
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.268
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0102(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7506
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0219P)^2^+3.0572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6619
_reflns_number_total             7506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00339c2.cif
_cod_data_source_block           CCDC_2422425
_cod_depositor_comments
'Adding full bibliography for 7718589--7718592.cif.'
_cod_original_cell_volume        2050.60(14)
_cod_database_code               7718589
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.534
_exptl_absorpt_special_details
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 0.71101   10.103   13.127   17.216   69.700   73.802   86.778
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.96 with sigma of 0.02
 H3A-H3B
 1.52 with sigma of 0.02
 O4-H4A = O4-H4B
 0.96 with sigma of 0.02
 H4A-H4B
 1.52 with sigma of 0.02
 C25-O10 \\sim C25'-O10'
 with sigma of 0.01
 C26-O10 \\sim C26'-O10'
 with sigma of 0.01
3. Others
 Sof(C24')=Sof(H24C)=Sof(H24D)=Sof(C25')=Sof(H25C)=Sof(H25D)=Sof(O10')=
 Sof(C26')=Sof(H26C)=Sof(H26D)=Sof(C27')=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(O10)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C11(H11A,H11B), C8(H8A,H8B), C12(H12A,H12B), C14(H14A,H14B),
 C7(H7A,H7B), C23(H23A,H23B), C16(H16A,H16B), C19(H19A,H19B), C13(H13A,H13B),
 C20(H20A,H20B), C5(H5A,H5B), C6(H6A,H6B), C22(H22A,H22B), C21(H21A,H21B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C24'(H24C,
 H24D), C25'(H25C,H25D), C26'(H26C,H26D), C27'(H27C,H27D), C10(H10A,H10B),
 C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C4(H4C,H4D)
;
_shelx_res_checksum              31224
_shelx_hkl_checksum              63492
_olex2_submission_special_instructions 'No special instructions were received'