Homochiral Dy<sub>2</sub>Zn<sub>2</sub> zero-field single-molecule magnets derived from (<i>R</i>)/(<i>S</i>)-2-methoxy-2-phenylacetic acids.
Liu, Cai-Ming; Hao, Xiang; Zhang, Yi-Quan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13522–13528; doi:10.1039/d5dt01609f

data_7719264
_publ_section_title
;
 Homochiral Dy<sub>2</sub>Zn<sub>2</sub> zero-field single-molecule
 magnets derived from (<i>R</i>)/(<i>S</i>)-2-methoxy-2-phenylacetic
 acids.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13522
_journal_page_last               13528
_journal_paper_doi               10.1039/d5dt01609f
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C80 H76 Dy2 N6 O20 Zn2, 2(C3 H7 N O)'
_chemical_formula_sum            'C86 H90 Dy2 N8 O22 Zn2'
_chemical_formula_weight         2043.39
_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_creation_date             2025-06-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2025-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.0236(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.85337(11)
_cell_length_b                   16.76827(12)
_cell_length_c                   20.35111(16)
_cell_measurement_reflns_used    39097
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      74.5810
_cell_measurement_theta_min      3.6640
_cell_volume                     4236.32(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)'
_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      104(2)
_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 0.993
_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     20.00  45.00   0.50    0.05    --   41.06  63.00-136.43   50
  2  \w     20.00  45.00   0.50    0.05    --   41.06  63.00 -82.50   50
  3  \w     22.00  48.00   0.50    0.05    --   41.06  62.00 -70.21   52
  4  \w     23.00  54.00   0.50    0.05    --   41.06  55.00  89.34   62
  5  \w     20.00  46.00   0.50    0.05    --   41.06  63.00  38.71   52
  6  \w     30.00  55.00   0.50    0.05    --   41.06  61.00 -50.44   50
  7  \w     22.00  53.00   0.50    0.05    --   41.06  61.00-116.09   62
  8  \w     75.00 133.00   0.50    0.05    --  108.87  15.00-180.00  116
  9  \w    131.00 167.00   0.50    0.05    --  108.87  77.00-180.00   72
 10  \w    115.00 141.00   0.50    0.05    --  108.87  77.00-150.00   52
 11  \w     93.00 175.00   0.50    0.05    --  108.87  61.00-150.00  164
 12  \w    131.00 175.00   0.50    0.05    --  108.87  61.00  60.00   88
 13  \w    100.00 173.00   0.50    0.05    --  108.87  77.00 150.00  146
 14  \w    147.00 175.00   0.50    0.05    --  108.87  77.00 120.00   56
 15  \w     90.00 116.00   0.50    0.05    --  108.87  61.00  60.00   52
 16  \w     89.00 156.00   0.50    0.05    --  108.87  61.00  30.00  134
 17  \w     94.00 170.00   0.50    0.05    --  108.87  45.00  90.00  152
 18  \w     91.00 148.00   0.50    0.05    --  108.87  45.00  60.00  114
 19  \w     91.00 123.00   0.50    0.05    --  108.87  30.00  90.00   64
 20  \w     91.00 157.00   0.50    0.05    --  108.87  61.00 -60.00  132
 21  \w     89.00 175.00   0.50    0.05    --  108.87  45.00-120.00  172
 22  \w     89.00 163.00   0.50    0.05    --  108.87  61.00-180.00  148
 23  \w    135.00 160.00   0.50    0.05    --  108.87  30.00 -90.00   50
 24  \w     77.00 110.00   0.50    0.05    --  108.87  15.00  90.00   66
 25  \w    -29.00  42.00   0.50    0.05    --   41.06 -57.00  90.00  142
 26  \w    -23.00  41.00   0.50    0.05    --   41.06 -57.00-150.00  128
 27  \w    113.00 167.00   0.50    0.05    --  108.87 125.00  60.00  108
 28  \w     99.00 164.00   0.50    0.05    --  108.87  87.00 111.00  130
 29  \w     34.00  71.00   0.50    0.05    --  108.87 -77.00-150.00   74
 30  \w     34.00  71.00   0.50    0.05    --  108.87 -77.00-120.00   74
 31  \w     36.00  69.00   0.50    0.05    --  108.87 -77.00 -90.00   66
 32  \w     34.00  71.00   0.50    0.05    --  108.87 -77.00-180.00   74
 33  \w     34.00  64.00   0.50    0.05    --  108.87 -77.00  60.00   60
 34  \w     34.00  72.00   0.50    0.05    --  108.87 -77.00 120.00   76
 35  \w     34.00  59.00   0.50    0.05    --  108.87 -77.00  90.00   50
 36  \w     35.00  98.00   0.50    0.05    --  108.87-125.00   0.00  126
 37  \w     65.00  91.00   0.50    0.05    --  108.87 -95.00  60.00   52
 38  \w     35.00  61.00   0.50    0.05    --  108.87-125.00  60.00   52
 39  \w     75.00 100.00   0.50    0.05    --  108.87-125.00  60.00   50
 40  \w     35.00  99.00   0.50    0.05    --  108.87-125.00  90.00  128
 41  \w     35.00  95.00   0.50    0.05    --  108.87-125.00 150.00  120
 42  \w     67.00  92.00   0.50    0.05    --  108.87 -95.00 120.00   50
 43  \w     62.00  91.00   0.50    0.05    --  108.87 -95.00  90.00   58
 44  \w     36.00  92.00   0.50    0.05    --  108.87 -95.00  30.00  112
 45  \w     52.00  91.00   0.50    0.05    --  108.87 -95.00   0.00   78
 46  \w     40.00  66.00   0.50    0.05    --  108.87 -87.00  -6.00   52
 47  \w     36.00  62.00   0.50    0.05    --  108.87 -95.00 -90.00   52
 48  \w    -15.00  73.00   0.50    0.05    --   41.06 -87.00  -6.00  176
 49  \w     -5.00  30.00   0.50    0.05    --  -50.00  30.00   0.00   70
 50  \w     -4.00  28.00   0.50    0.05    --  -50.00  30.00-180.00   64
 51  \w    -18.00  26.00   0.50    0.05    --  -50.00  45.00-150.00   88
 52  \w     -3.00  27.00   0.50    0.05    --  -41.06  57.00  90.00   60
 53  \w    -37.00  -9.00   0.50    0.05    --  -41.06  57.00  90.00   56
 54  \w    -73.00 -16.00   0.50    0.05    --  -41.06  87.00 111.00  114
 55  \w    -61.00 -36.00   0.50    0.05    --  -50.00  87.00 111.00   50
 56  \w    -61.00 -30.00   0.50    0.05    --  -50.00 -56.00 174.21   62
 57  \w   -120.00 -65.00   0.50    0.05    --  -41.06 -38.00  90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1032611000
_diffrn_orient_matrix_UB_12      0.0499532000
_diffrn_orient_matrix_UB_13      -0.0086425000
_diffrn_orient_matrix_UB_21      0.0481537000
_diffrn_orient_matrix_UB_22      0.0653149000
_diffrn_orient_matrix_UB_23      -0.0365456000
_diffrn_orient_matrix_UB_31      -0.0492011000
_diffrn_orient_matrix_UB_32      -0.0409676000
_diffrn_orient_matrix_UB_33      -0.0687851000
_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  0.0340
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55372
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.724
_diffrn_reflns_theta_min         3.560
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.75a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 7651 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         16986
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0505P)^2^+2.7840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                16729
_reflns_number_total             16986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01609f2.cif
_cod_data_source_block           exp_197_auto
_cod_depositor_comments
'Adding full bibliography for 7719264--7719265.cif.'
_cod_database_code               7719264
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOZnDy
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N8-C84
 1.33 with sigma of 0.01
 N7-C83
 1.46 with sigma of 0.01
 C81-N7
 1.33 with sigma of 0.01
 N7-C82
 1.46 with sigma of 0.01
 C86-N8
 1.46 with sigma of 0.01
 N8-C85
 1.46 with sigma of 0.01
 C84-O22
 1.25 with sigma of 0.01
 O21-C81
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C84) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4.a Riding coordinates:
 C85(H85A,H85B,H85C)
4.b Ternary CH refined with riding coordinates:
 C58(H58), C67(H67)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C31(H31), C32(H32), C33(H33), C36(H36), C39(H39), C40(H40), C41(H41),
 C42(H42), C45(H45), C46(H46), C47(H47), C50(H50), C53(H53), C54(H54), C55(H55),
  C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C69(H69),
 C70(H70), C71(H71), C72(H72), C73(H73), C75(H75), C78(H78), C81(H81), C84(H84)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C43(H43A,H43B,
 H43C), C65(H65A,H65B,H65C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,
 H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C),
 C83(H83A,H83B,H83C), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              47317
_shelx_hkl_checksum              1259
_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 1.662
_oxdiff_exptl_absorpt_empirical_full_min 0.650