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_7719265
_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             2025-06-04
_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                 105.6000(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.90010(11)
_cell_length_b                   16.81720(12)
_cell_length_c                   20.47270(16)
_cell_measurement_reflns_used    32757
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.3040
_cell_measurement_theta_min      3.4400
_cell_volume                     4277.81(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 0.974
_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    -10.00  29.00   0.50    0.14    --  -46.49  19.00-120.00   78
  2  \w    -23.00  14.00   0.50    0.14    --  -46.49  19.00 -30.00   74
  3  \w    -23.00  29.00   0.50    0.14    --  -46.49  19.00 120.00  104
  4  \w     -9.00  16.00   0.50    0.14    --  -46.49  19.00 150.00   50
  5  \w     65.00  91.00   0.50    0.60    --  103.82 -95.00  90.00   52
  6  \w     34.00 111.00   0.50    0.60    --  103.82-125.00 150.00  154
  7  \w     75.00 102.00   0.50    0.14    --   46.49-151.00-121.00   54
  8  \w     82.00 112.00   0.50    0.60    --  103.82-125.00-180.00   60
  9  \w     45.00  73.00   0.50    0.60    --  103.82-125.00-180.00   56
 10  \w     35.00  96.00   0.50    0.60    --  103.82-125.00-120.00  122
 11  \w     87.00 130.00   0.50    0.60    --  103.82-151.00-121.00   86
 12  \w     34.00 101.00   0.50    0.60    --  103.82-125.00 -60.00  134
 13  \w     18.00  91.00   0.50    0.14    --   46.49-123.00  40.00  146
 14  \w     34.00 112.00   0.50    0.60    --  103.82-125.00  30.00  156
 15  \w     54.00 110.00   0.50    0.60    --  103.82-123.00  40.00  112
 16  \w     35.00  89.00   0.50    0.60    --  103.82 -95.00  60.00  108
 17  \w     33.00  59.00   0.50    0.60    --  103.82 -77.00  30.00   52
 18  \w     32.00  64.00   0.50    0.60    --  103.82 -61.00  90.00   64
 19  \w     39.00  64.00   0.50    0.60    --  103.82 -61.00-150.00   50
 20  \w     42.00  75.00   0.50    0.60    --  103.82 -61.00-180.00   66
 21  \w     90.00 126.00   0.50    0.60    --  103.82  15.00-120.00   72
 22  \w    134.00 178.00   0.50    0.60    --  103.82  15.00-120.00   88
 23  \w     62.00 126.00   0.50    0.60    --  103.82 151.00 -77.00  128
 24  \w     64.00 115.00   0.50    0.14    --   46.49 151.00 -77.00  102
 25  \w     85.00 111.00   0.50    0.60    --  103.82 123.00 121.00   52
 26  \w     24.00 116.00   0.50    0.14    --   46.49  77.00 120.00  184
 27  \w   -103.00 -70.00   0.50    0.14    --  -46.49 151.00 -77.00   66
 28  \w    -89.00 -63.00   0.50    0.60    -- -103.82 125.00-150.00   52
 29  \w   -129.00 -41.00   0.50    0.60    -- -103.82 151.00 -77.00  176
 30  \w   -108.00 -75.00   0.50    0.60    -- -103.82 109.00-101.94   66
 31  \w    -60.00 -35.00   0.50    0.60    -- -103.82 109.00-101.94   50
 32  \w    -95.00 -46.00   0.50    0.60    -- -103.82 125.00  30.00   98
 33  \w    -76.00 -51.00   0.50    0.14    --  -46.49 123.00 121.00   50
 34  \w    -96.00 -71.00   0.50    0.60    -- -103.82 123.00 121.00   50
 35  \w    -66.00 -33.00   0.50    0.60    -- -103.82  61.00 120.00   66
 36  \w    -66.00 -31.00   0.50    0.60    -- -103.82  61.00  90.00   70
 37  \w    -68.00 -35.00   0.50    0.60    -- -103.82  61.00  60.00   66
 38  \w    -95.00 -70.00   0.50    0.60    -- -103.82  77.00   0.00   50
 39  \w   -101.00 -32.00   0.50    0.60    -- -103.82  77.00 -30.00  138
 40  \w   -146.00 -93.00   0.50    0.60    -- -103.82 -15.00 -90.00  106
 41  \w   -116.00 -32.00   0.50    0.14    --  -46.49 -57.00-180.00  168
 42  \w   -122.00 -97.00   0.50    0.60    -- -103.82 -62.00 -41.54   50
 43  \w   -164.00-139.00   0.50    0.60    -- -103.82 -62.00 -41.54   50
 44  \w   -174.00-122.00   0.50    0.60    -- -103.82 -57.00  72.11  104
 45  \w   -117.00 -91.00   0.50    0.60    -- -103.82 -30.00 120.00   52
 46  \w   -170.00 -88.00   0.50    0.60    -- -103.82 -63.00 158.06  164
 47  \w   -173.00-140.00   0.50    0.60    -- -103.82 -30.00 120.00   66
 48  \w   -171.00-104.00   0.50    0.60    -- -103.82 -15.00 -60.00  134
 49  \w   -167.00 -75.00   0.50    0.60    -- -103.82-123.00  40.00  184
 50  \w   -112.00 -58.00   0.50    0.14    --  -46.49-151.00-121.00  108
 51  \w   -134.00-109.00   0.50    0.60    -- -103.82-151.00-121.00   50
;
_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      -0.1132918000
_diffrn_orient_matrix_UB_12      0.0146820000
_diffrn_orient_matrix_UB_13      0.0088539000
_diffrn_orient_matrix_UB_21      0.0137328000
_diffrn_orient_matrix_UB_22      0.0900099000
_diffrn_orient_matrix_UB_23      -0.0091662000
_diffrn_orient_matrix_UB_31      -0.0484074000
_diffrn_orient_matrix_UB_32      -0.0090601000
_diffrn_orient_matrix_UB_33      -0.0770434000
_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  0.0546
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67781
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.825
_diffrn_reflns_theta_min         3.454
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82247
_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    1.586
_exptl_crystal_description       cube
_exptl_crystal_F_000             2060
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 6099 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0055(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         17009
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                15198
_reflns_number_total             17009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01609f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7719264--7719265.cif.'
_cod_database_code               7719265
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOZnDy
_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
 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(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
4.a Riding coordinates:
 C82(H82A,H82B,H82C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C)
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), C83(H83A,H83B,H83C)
;
_shelx_res_checksum              37273
_shelx_hkl_checksum              4256
_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 1.625
_oxdiff_exptl_absorpt_empirical_full_min 0.613