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_7718591
_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 Ho N9 O10 P2 S3'
_chemical_formula_sum            'C27 H52 Ho N9 O10 P2 S3'
_chemical_formula_weight         985.82
_chemical_name_common            '[Ho(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     direct
_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                69.6750(10)
_cell_angle_beta                 73.7700(10)
_cell_angle_gamma                86.7580(10)
_cell_formula_units_Z            2
_cell_length_a                   10.08750(10)
_cell_length_b                   13.10110(10)
_cell_length_c                   17.17690(10)
_cell_measurement_reflns_used    20615
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      76.4250
_cell_measurement_theta_min      3.5800
_cell_volume                     2041.81(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_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      153.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27957
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.560
_diffrn_reflns_theta_min         3.601
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00243(11)
_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   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8229
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0401P)^2^+0.8707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7878
_reflns_number_total             8229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00339c2.cif
_cod_data_source_block           CCDC_2422427
_cod_depositor_comments
'Adding full bibliography for 7718589--7718592.cif.'
_cod_database_code               7718591
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.396
_shelx_estimated_absorpt_t_min   0.337
_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(C26')=
 Sof(H26C)=Sof(H26D)=Sof(C27')=Sof(H27C)=Sof(H27D)=Sof(O10')=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(O10)=FVAR(1)
 Sof(S1')=1-FVAR(2)
 Sof(S1)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C11(H11A,H11B), C8(H8A,H8B), C12(H12A,H12B), C14(H14A,H14B),
 C4(H4C,H4D), 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), C10(H10A,H10B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B),
 C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C26(H26A,H26B), C24'(H24C,
 H24D), C25'(H25C,H25D), C26'(H26C,H26D), C27'(H27C,H27D)
;
_shelx_res_checksum              41626
_shelx_hkl_checksum              24099
_olex2_submission_special_instructions 'No special instructions were received'