Homochiral Dy<sub>2</sub> zero-field single-molecule magnets derived from axial chiral ligands (<i>R</i>)/(<i>S</i>)-octahydro-1,1'-bi-2-naphthyl phosphate.
Liu, Cai-Ming; Hao, Xiang; Zhang, Yi-Quan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4159–4166; doi:10.1039/d4dt03408b

data_7717940
_publ_section_title
;
 Homochiral Dy<sub>2</sub> zero-field single-molecule magnets derived from
 axial chiral ligands (<i>R</i>)/(<i>S</i>)-octahydro-1,1'-bi-2-naphthyl
 phosphate.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4159
_journal_page_last               4166
_journal_paper_doi               10.1039/d4dt03408b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C65 H60 Dy2 F2 N8 O14 P2, 2(C H4 O), 2(C2 H3 N), C H2 Cl2, 2(H2 O)'
_chemical_formula_sum            'C72 H80 Cl2 Dy2 F2 N10 O18 P2'
_chemical_formula_weight         1869.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2kwjtt
_audit_creation_date             2024-10-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-17 deposited with the CCDC.	2025-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.5200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.25120(10)
_cell_length_b                   26.5780(2)
_cell_length_c                   14.38300(10)
_cell_measurement_reflns_used    37113
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.3100
_cell_measurement_theta_min      3.1760
_cell_volume                     3715.80(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.114a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.114a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.114a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -18.00  28.00   0.50    0.05    --  -46.47  19.00-180.00   92
  2  \w    -20.00   7.00   0.50    0.05    --  -46.47  19.00 -90.00   54
  3  \w    -20.00  18.00   0.50    0.05    --  -46.47  19.00 -30.00   76
  4  \w    -68.00 -43.00   0.50    0.15    -- -103.72  61.00 150.00   50
  5  \w    -21.00  18.00   0.50    0.05    --  -46.47  19.00 150.00   78
  6  \w     46.00  95.00   0.50    0.15    --  103.72 -95.00  90.00   98
  7  \w     36.00 111.00   0.50    0.15    --  103.72-125.00  90.00  150
  8  \w     40.00  81.00   0.50    0.15    --  103.72-155.00  88.00   82
  9  \w     86.00 131.00   0.50    0.15    --  103.72-155.00  88.00   90
 10  \w     74.00 106.00   0.50    0.05    --   46.47-155.00  88.00   64
 11  \w     68.00  93.00   0.50    0.15    --  103.72-125.00 -60.00   50
 12  \w     43.00  69.00   0.50    0.05    --   46.47-121.00-114.00   52
 13  \w     70.00  97.00   0.50    0.15    --  103.72-121.00-114.00   54
 14  \w     80.00 108.00   0.50    0.15    --  103.72 -77.00 -90.00   56
 15  \w     33.00  75.00   0.50    0.15    --  103.72 -61.00-150.00   84
 16  \w     32.00  76.00   0.50    0.15    --  103.72 -77.00 -90.00   88
 17  \w     36.00  61.00   0.50    0.15    --  103.72 -61.00-120.00   50
 18  \w     36.00  75.00   0.50    0.15    --  103.72 -61.00 -90.00   78
 19  \w     34.00  75.00   0.50    0.15    --  103.72 -61.00 -60.00   82
 20  \w     38.00  75.00   0.50    0.15    --  103.72 -61.00 120.00   74
 21  \w   -118.00 -24.00   0.50    0.05    --  -46.47 -77.00-150.00  188
 22  \w   -114.00 -25.00   0.50    0.05    --  -46.47 -77.00-180.00  178
 23  \w   -167.00-141.00   0.50    0.15    -- -103.72 -30.00 120.00   52
 24  \w   -128.00 -98.00   0.50    0.15    -- -103.72 -30.00 120.00   60
 25  \w   -154.00-108.00   0.50    0.15    -- -103.72 -45.00 150.00   92
 26  \w    -99.00 -53.00   0.50    0.05    --  -46.47-155.00  88.00   92
 27  \w   -131.00-106.00   0.50    0.15    -- -103.72-155.00  88.00   50
 28  \w   -117.00 -88.00   0.50    0.15    -- -103.72-121.00-114.00   58
 29  \w   -142.00 -85.00   0.50    0.15    -- -103.72 -95.00-150.00  114
 30  \w   -106.00 -34.00   0.50    0.15    -- -103.72 121.00 -31.00  144
 31  \w   -122.00 -88.00   0.50    0.15    -- -103.72 138.00 100.14   68
 32  \w   -104.00 -31.00   0.50    0.15    -- -103.72 155.00 125.00  146
 33  \w   -122.00 -31.00   0.50    0.15    -- -103.72 141.00 162.89  182
 34  \w   -124.00 -93.00   0.50    0.15    -- -103.72 141.00 136.25   62
 35  \w    -95.00 -70.00   0.50    0.05    --  -46.47 155.00 125.00   50
 36  \w    -91.00 -46.00   0.50    0.15    -- -103.72 125.00  60.00   90
 37  \w   -110.00 -84.00   0.50    0.15    -- -103.72 125.00   0.00   52
 38  \w    -81.00 -34.00   0.50    0.15    -- -103.72 125.00   0.00   94
 39  \w    -58.00 -32.00   0.50    0.15    -- -103.72 138.00-107.49   52
 40  \w   -122.00 -91.00   0.50    0.15    -- -103.72 138.00-107.49   62
 41  \w    -90.00 -14.00   0.50    0.05    --  -46.47 121.00 -31.00  152
 42  \w     87.00 175.00   0.50    0.15    --  103.72  61.00-120.00  176
 43  \w    100.00 175.00   0.50    0.15    --  103.72  61.00 -60.00  150
 44  \w    121.00 155.00   0.50    0.15    --  103.72 121.00 -31.00   68
 45  \w     91.00 175.00   0.50    0.15    --  103.72  45.00  60.00  168
 46  \w     78.00 118.00   0.50    0.05    --   46.47 155.00 125.00   80
 47  \w     72.00 111.00   0.50    0.15    --  103.72 155.00 125.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1285992000
_diffrn_orient_matrix_UB_12      0.0168708000
_diffrn_orient_matrix_UB_13      -0.0252552000
_diffrn_orient_matrix_UB_21      0.0487164000
_diffrn_orient_matrix_UB_22      -0.0550786000
_diffrn_orient_matrix_UB_23      0.0053562000
_diffrn_orient_matrix_UB_31      -0.0790758000
_diffrn_orient_matrix_UB_32      -0.0065442000
_diffrn_orient_matrix_UB_33      -0.1098763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53129
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.503
_diffrn_reflns_theta_min         3.326
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.114a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 6350 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0023(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         14920
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0564P)^2^+7.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                14338
_reflns_number_total             14920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03408b2.cif
_cod_data_source_block           2s
_cod_depositor_comments
'Adding full bibliography for 7717939--7717940.cif.'
_cod_database_code               7717940
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONPDy
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 O14-C66
 1.42 with sigma of 0.01
 C67-O15
 1.42 with sigma of 0.01
 C31-C30
 1.52 with sigma of 0.01
 C30-C29
 1.52 with sigma of 0.01
 C32-C31
 1.52 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 C65-H13
 1.880684 with sigma of 0.02
 Dy1-H13
 2.879925 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O3W)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O1W(H1WA,H1WB), O13(H13), O14(H14A), O15(H15A), C71(H71A,H71B,H71C), O2W(H2WA,
 H2WB), O3W(H3WA,H3WB)
4.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C49(H49A,H49B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C57(H57A,H57B), C58(H58A,H58B),
  C59(H59A,H59B), C60(H60A,H60B), C72(H72A,H72B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C19(H19), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C42(H42), C43(H43), C46(H46), C47(H47), C62(H62), C63(H63)
4.d Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,
 H69C)
;
_shelx_res_checksum              91701
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.829