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_7718592
_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
'C26 H54 Dy N8 O11 P2 S2, C27 H52 Dy N9 O10 P2 S3, C N S, 2(H2 O)'
_chemical_formula_sum            'C54 H110 Dy2 N18 O23 P4 S6'
_chemical_formula_weight         2020.83
_chemical_name_common
'[Dy(TMPO)2(SCN)3(H2O)2][Dy(TMPO)2(SCN)2(H2O)3](SCN)(H2O)2'
_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   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 103.526(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7170(4)
_cell_length_b                   24.9048(5)
_cell_length_c                   17.7571(3)
_cell_measurement_reflns_used    36382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0220
_cell_measurement_theta_min      4.1720
_cell_volume                     8477.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            70764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.586
_diffrn_reflns_theta_min         3.501
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    12.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light white'
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         17124
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0465P)^2^+5.7976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14459
_reflns_number_total             17124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00339c2.cif
_cod_data_source_block           CCDC_2422426
_cod_depositor_comments
'Adding full bibliography for 7718589--7718592.cif.'
_cod_database_code               7718592
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.485
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7C = O7-H7D
 0.96 with sigma of 0.02
 H7C-H7D
 1.52 with sigma of 0.02
 O8-H8C = O8-H8D
 0.96 with sigma of 0.02
 H8C-H8D
 1.52 with sigma of 0.02
 O9-H9C = O9-H9D
 0.96 with sigma of 0.02
 H9C-H9D
 1.52 with sigma of 0.02
 Dy1-H6A \\sim Dy1-H6B
 with sigma of 0.02
 C7-C8 \\sim C7'-C8'
 with sigma of 0.01
 C9-C10 \\sim C9'-C10'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C7')
Uanis(C9) = Uanis(C9')
Uanis(C23) = Uanis(C23')
Uanis(C25) = Uanis(C25')
Uanis(O16) = Uanis(O16')
4. Others
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(C9')=Sof(H9'A)=
 Sof(H9'B)=Sof(C10')=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C23')=Sof(H23C)=Sof(H23D)=Sof(C24')=Sof(H24C)=Sof(H24D)=Sof(C25')=
 Sof(H25C)=Sof(H25D)=Sof(C26')=Sof(H26C)=Sof(H26D)=Sof(O16')=1-FVAR(2)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(O16)=FVAR(2)
5.a Free rotating group:
 O6(H6A,H6B), O11(H11C,H11D), O10(H10E,H10F)
5.b Rotating group:
 O7(H7C,H7D), O5(H5A,H5B), O8(H8C,H8D), O9(H9C,H9D)
5.c Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C38(H38A,H38B), C36(H36A,H36B), C29(H29A,H29B), C35(H35A,
 H35B), C27(H27A,H27B), C37(H37A,H37B), C39(H39A,H39B), C31(H31A,H31B),
 C15(H15A,H15B), C34(H34A,H34B), C44(H44A,H44B), C28(H28A,H28B), C21(H21A,H21B),
  C45(H45A,H45B), C33(H33A,H33B), C16(H16A,H16B), C47(H47A,H47B), C30(H30A,
 H30B), C41(H41A,H41B), C20(H20A,H20B), C48(H48A,H48B), C40(H40A,H40B),
 C19(H19A,H19B), C17(H17A,H17B), C79(H79A,H79B), C22(H22A,H22B), C12(H12A,H12B),
  C46(H46A,H46B), C50(H50A,H50B), C78(H78A,H78B), C18(H18A,H18B), C42(H42A,
 H42B), C49(H49A,H49B), C11(H11A,H11B), C75(H75A,H75B), C13(H13A,H13B),
 C14(H14A,H14B), C76(H76A,H76B), C32(H32A,H32B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C7'(H7'A,H7'B), C8'(H8'A,H8'B), C9'(H9'A,H9'B),
 C10'(H10C,H10D), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C23'(H23C,H23D), C24'(H24C,H24D), C25'(H25C,H25D), C26'(H26C,H26D)
;
_shelx_res_checksum              2102
_shelx_hkl_checksum              62591
_olex2_submission_special_instructions 'No special instructions were received'