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_7717939
_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.cc2kwjss
_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                 108.2780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.25390(10)
_cell_length_b                   26.5654(2)
_cell_length_c                   14.43670(10)
_cell_measurement_reflns_used    43968
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.5970
_cell_measurement_theta_min      3.2260
_cell_volume                     3734.13(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 0.982
_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    -67.00 -31.00   0.50    0.19    -- -103.72  61.00-150.00   72
  2  \w    -21.00   4.00   0.50    0.05    --  -46.47  18.00 -56.00   50
  3  \w    -82.00 -33.00   0.50    0.19    -- -103.72  77.00 120.00   98
  4  \w    -23.00   2.00   0.50    0.05    --  -46.47  19.00  90.00   50
  5  \w     25.00  61.00   0.50    0.05    --   46.47  77.00   0.00   72
  6  \w     29.00  65.00   0.50    0.05    --   46.47  77.00  30.00   72
  7  \w     33.00  69.00   0.50    0.05    --   46.47  57.00   0.00   72
  8  \w     83.00 115.00   0.50    0.05    --   46.47  18.00 -56.00   64
  9  \w     39.00 117.00   0.50    0.05    --   46.47  19.00  30.00  156
 10  \w     28.00  79.00   0.50    0.05    --   46.47  77.00  90.00  102
 11  \w     24.00 118.00   0.50    0.05    --   46.47  77.00  60.00  188
 12  \w     81.00 108.00   0.50    0.19    --  103.72  77.00   0.00   54
 13  \w     88.00 119.00   0.50    0.19    --  103.72  61.00  60.00   62
 14  \w    123.00 176.00   0.50    0.19    --  103.72  61.00  60.00  106
 15  \w     94.00 120.00   0.50    0.19    --  103.72  18.00 -56.00   52
 16  \w     32.00  71.00   0.50    0.19    --  103.72 -61.00-180.00   78
 17  \w     32.00  75.00   0.50    0.19    --  103.72 -61.00-150.00   86
 18  \w     45.00  74.00   0.50    0.19    --  103.72 -61.00 -30.00   58
 19  \w     34.00  65.00   0.50    0.19    --  103.72 -61.00   0.00   62
 20  \w     46.00  73.00   0.50    0.19    --  103.72 -61.00  30.00   54
 21  \w     34.00  75.00   0.50    0.19    --  103.72 -61.00  60.00   82
 22  \w      1.00  26.00   0.50    0.05    --   46.47 -18.00 135.00   50
 23  \w    -25.00  46.00   0.50    0.05    --   46.47 -38.00   0.00  142
 24  \w     31.00  70.00   0.50    0.19    --  103.72 -95.00   0.00   78
 25  \w     75.00 102.00   0.50    0.19    --  103.72 -95.00   0.00   54
 26  \w     33.00  95.00   0.50    0.19    --  103.72 -95.00 -30.00  124
 27  \w     34.00 110.00   0.50    0.19    --  103.72-125.00  90.00  152
 28  \w     24.00  92.00   0.50    0.05    --   46.47-125.00 -90.00  136
 29  \w   -106.00 -80.00   0.50    0.19    -- -103.72 -78.00  18.55   52
 30  \w   -106.00 -80.00   0.50    0.19    -- -103.72 -78.00  33.79   52
 31  \w   -106.00 -81.00   0.50    0.19    -- -103.72 -77.00  90.00   50
 32  \w   -108.00 -81.00   0.50    0.19    -- -103.72 -77.00  60.00   54
 33  \w   -108.00 -81.00   0.50    0.19    -- -103.72 -76.00  53.48   54
 34  \w   -106.00 -81.00   0.50    0.19    -- -103.72 -76.00  61.91   50
 35  \w   -106.00 -81.00   0.50    0.19    -- -103.72 -76.00  74.21   50
 36  \w   -107.00 -82.00   0.50    0.19    -- -103.72 -75.00 115.21   50
 37  \w   -167.00-142.00   0.50    0.19    -- -103.72 -76.00  74.21   50
 38  \w   -172.00-146.00   0.50    0.19    -- -103.72 -76.00  61.91   52
 39  \w   -167.00-141.00   0.50    0.19    -- -103.72 -76.00  53.48   52
 40  \w   -166.00-139.00   0.50    0.19    -- -103.72 -74.00 106.45   54
 41  \w   -169.00-144.00   0.50    0.19    -- -103.72 -75.00 115.21   50
 42  \w   -107.00 -82.00   0.50    0.19    -- -103.72 -74.00 106.45   50
 43  \w   -108.00 -82.00   0.50    0.19    -- -103.72 -75.00  97.12   52
 44  \w   -108.00 -82.00   0.50    0.19    -- -103.72 -74.00  66.23   52
 45  \w   -108.00 -82.00   0.50    0.19    -- -103.72 -74.00  -5.72   52
 46  \w   -110.00 -83.00   0.50    0.19    -- -103.72 -73.00  46.17   54
 47  \w   -110.00 -84.00   0.50    0.19    -- -103.72 -69.00  82.54   52
 48  \w   -113.00 -83.00   0.50    0.19    -- -103.72 -72.00 106.36   60
 49  \w   -117.00 -83.00   0.50    0.19    -- -103.72 -71.00 130.69   68
 50  \w   -165.00-130.00   0.50    0.19    -- -103.72 -71.00 130.69   70
 51  \w   -111.00 -85.00   0.50    0.19    -- -103.72 -68.00  16.15   52
 52  \w   -112.00 -85.00   0.50    0.19    -- -103.72 -69.00 -17.93   54
 53  \w   -149.00-121.00   0.50    0.19    -- -103.72 -68.00 -24.07   56
 54  \w   -166.00 -86.00   0.50    0.19    -- -103.72 -68.00 -31.49  160
 55  \w   -114.00 -85.00   0.50    0.19    -- -103.72 -68.00 -24.07   58
 56  \w   -111.00 -85.00   0.50    0.19    -- -103.72 -66.00  -7.93   52
 57  \w   -111.00 -85.00   0.50    0.19    -- -103.72 -68.00  31.97   52
 58  \w   -112.00 -85.00   0.50    0.19    -- -103.72 -67.00  45.41   54
 59  \w   -120.00 -85.00   0.50    0.19    -- -103.72 -66.00   8.45   70
 60  \w   -112.00 -85.00   0.50    0.19    -- -103.72 -66.00 -18.31   54
 61  \w   -174.00-139.00   0.50    0.19    -- -103.72 -68.00  16.15   70
 62  \w   -172.00-146.00   0.50    0.19    -- -103.72 -66.00   8.45   52
 63  \w   -174.00 -86.00   0.50    0.19    -- -103.72 -65.00  22.72  176
 64  \w   -112.00 -86.00   0.50    0.19    -- -103.72 -64.00  -6.20   52
 65  \w   -112.00 -86.00   0.50    0.19    -- -103.72 -65.00 -12.63   52
 66  \w   -112.00 -86.00   0.50    0.19    -- -103.72 -63.00  -2.95   52
 67  \w   -113.00 -86.00   0.50    0.19    -- -103.72 -63.00  69.24   54
 68  \w   -113.00 -87.00   0.50    0.19    -- -103.72 -61.00  60.00   52
 69  \w   -115.00 -86.00   0.50    0.19    -- -103.72 -64.00  85.76   58
 70  \w   -113.00 -87.00   0.50    0.19    -- -103.72 -62.00 112.54   52
 71  \w   -112.00 -86.00   0.50    0.19    -- -103.72 -65.00 110.85   52
 72  \w   -114.00 -87.00   0.50    0.19    -- -103.72 -61.00  86.80   54
 73  \w   -132.00 -90.00   0.50    0.19    -- -103.72 -61.00  30.00   84
 74  \w   -114.00 -88.00   0.50    0.19    -- -103.72 -59.00  61.60   52
 75  \w   -173.00 -91.00   0.50    0.19    -- -103.72 -45.00  41.58  164
 76  \w   -173.00 -91.00   0.50    0.19    -- -103.72 -45.00  59.11  164
 77  \w   -152.00-127.00   0.50    0.19    -- -103.72 -18.00 135.00   50
 78  \w   -122.00 -87.00   0.50    0.05    --  -46.47 -18.00 135.00   70
;
_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      0.1239363000
_diffrn_orient_matrix_UB_12      0.0108777000
_diffrn_orient_matrix_UB_13      -0.0356774000
_diffrn_orient_matrix_UB_21      -0.0980455000
_diffrn_orient_matrix_UB_22      0.0087453000
_diffrn_orient_matrix_UB_23      -0.1040531000
_diffrn_orient_matrix_UB_31      -0.0087381000
_diffrn_orient_matrix_UB_32      0.0562677000
_diffrn_orient_matrix_UB_33      0.0230364000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            71821
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.909
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75041
_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    1.663
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 6275 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         14595
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0772P)^2^+5.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.892
_reflns_number_gt                14309
_reflns_number_total             14595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03408b2.cif
_cod_data_source_block           2r
_cod_depositor_comments
'Adding full bibliography for 7717939--7717940.cif.'
_cod_database_code               7717939
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFPDy
_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
 Dy2-H13
 2.879925 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Riding coordinates:
 C65(H65A,H65B,H65C), 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:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              84439
_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 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.820