Fixing CO<sub>2</sub> from the air to assemble Dy<sub>8</sub> zero-field single-molecule magnets and Gd<sub>8</sub> magnetocaloric molecular materials.
Liu, Cai-Ming; Hao, Xiang; Dalton transactions (Cambridge, England : 2003) 55 (2026) 5055–5063; doi:10.1039/d6dt00214e

data_7720402
_publ_section_title
;
 Fixing CO<sub>2</sub> from the air to assemble Dy<sub>8</sub> zero-field
 single-molecule magnets and Gd<sub>8</sub> magnetocaloric molecular
 materials.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5055
_journal_page_last               5063
_journal_paper_doi               10.1039/d6dt00214e
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'C38 H55 Dy2 N13 O12, 2(C F3 O3 S), 3(C4 H9 N O), H2 O'
_chemical_formula_sum            'C52 H84 Dy2 F6 N16 O22 S2'
_chemical_formula_weight         1788.47
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-01-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2026-01-12 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                65.1480(10)
_cell_angle_beta                 87.5400(10)
_cell_angle_gamma                83.2340(10)
_cell_formula_units_Z            1
_cell_length_a                   11.7867(2)
_cell_length_b                   12.4022(2)
_cell_length_c                   13.6136(2)
_cell_measurement_reflns_used    30498
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6300
_cell_measurement_theta_min      3.9320
_cell_volume                     1793.14(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.75a 64-bit (release 14-06-2023))'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  46.00   0.50    0.05    --   40.81  62.00-129.25   52
  2  \w     20.00  45.00   0.50    0.05    --   40.81  63.00 -86.52   50
  3  \w     25.00  51.00   0.50    0.05    --   40.81  62.00 -66.01   52
  4  \w     22.00  56.00   0.50    0.05    --   40.81  58.00 102.40   68
  5  \w     21.00  46.00   0.50    0.05    --   40.81  59.00 177.92   50
  6  \w     22.00  50.00   0.50    0.05    --   40.81  62.00  44.25   56
  7  \w     19.00  44.00   0.50    0.05    --   40.81  65.00  -1.25   50
  8  \w     36.00  62.00   0.50    0.05    --  108.87 -85.00 -42.00   52
  9  \w     64.00  90.00   0.50    0.05    --  108.87-125.00  60.00   52
 10  \w     36.00  66.00   0.50    0.05    --  108.87-125.00   0.00   60
 11  \w     35.00 100.00   0.50    0.05    --  108.87-125.00 -30.00  130
 12  \w     33.00  92.00   0.50    0.05    --  108.87 -95.00 -90.00  118
 13  \w     37.00 100.00   0.50    0.05    --  108.87-125.00-120.00  126
 14  \w     63.00  92.00   0.50    0.05    --  108.87 -95.00 -60.00   58
 15  \w     64.00  90.00   0.50    0.05    --  108.87 -95.00-150.00   52
 16  \w     62.00  90.00   0.50    0.05    --  108.87 -95.00   0.00   56
 17  \w     37.00  92.00   0.50    0.05    --  108.87 -95.00  30.00  110
 18  \w     31.00  58.00   0.50    0.05    --  108.87 -95.00  90.00   54
 19  \w     62.00  91.00   0.50    0.05    --  108.87 -95.00  90.00   58
 20  \w     65.00  91.00   0.50    0.05    --  108.87 -95.00 150.00   52
 21  \w     35.00  61.00   0.50    0.05    --  108.87 -95.00 150.00   52
 22  \w     33.00  89.00   0.50    0.05    --  108.87 -95.00 120.00  112
 23  \w     64.00  90.00   0.50    0.05    --  108.87 -95.00  60.00   52
 24  \w     33.00  61.00   0.50    0.05    --  108.87 -95.00  60.00   56
 25  \w     62.00  92.00   0.50    0.05    --  108.87 -95.00 -30.00   60
 26  \w     32.00  92.00   0.50    0.05    --  108.87 -95.00-120.00  120
 27  \w    -16.00  72.00   0.50    0.05    --   40.81 -85.00 -42.00  176
 28  \w     35.00  72.00   0.50    0.05    --  108.87 -77.00 -30.00   74
 29  \w     97.00 159.00   0.50    0.05    --  108.87  30.00 -90.00  124
 30  \w    133.00 161.00   0.50    0.05    --  108.87  30.00 -60.00   56
 31  \w     98.00 124.00   0.50    0.05    --  108.87  30.00 -60.00   52
 32  \w     75.00 125.00   0.50    0.05    --  108.87  15.00 -90.00  100
 33  \w     83.00 132.00   0.50    0.05    --  108.87  15.00-180.00   98
 34  \w    108.00 134.00   0.50    0.05    --  108.87  30.00  60.00   52
 35  \w     78.00 133.00   0.50    0.05    --  108.87  15.00  30.00  110
 36  \w     77.00 133.00   0.50    0.05    --  108.87  15.00  60.00  112
 37  \w     80.00 131.00   0.50    0.05    --  108.87  15.00  90.00  102
 38  \w     77.00 128.00   0.50    0.05    --  108.87  15.00 150.00  102
 39  \w     38.00  68.00   0.50    0.05    --  108.87 -77.00 150.00   60
 40  \w     99.00 133.00   0.50    0.05    --  108.87  15.00-150.00   68
 41  \w     89.00 118.00   0.50    0.05    --  108.87 125.00-150.00   58
 42  \w    133.00 171.00   0.50    0.05    --  108.87 125.00-150.00   76
 43  \w    108.00 168.00   0.50    0.05    --  108.87 125.00 -60.00  120
 44  \w    105.00 171.00   0.50    0.05    --  108.87  85.00  76.00  132
 45  \w    -32.00  28.00   0.50    0.05    --  -50.00  45.00-180.00  120
 46  \w     -6.00  31.00   0.50    0.05    --  -50.00  30.00-120.00   74
 47  \w     16.00  41.00   0.50    0.05    --  -40.81  19.00-150.00   50
 48  \w     -8.00  32.00   0.50    0.05    --  -50.00  30.00 -60.00   80
 49  \w     17.00  42.00   0.50    0.05    --  -40.81  19.00  30.00   50
 50  \w     16.00  41.00   0.50    0.05    --  -40.81  19.00-180.00   50
 51  \w     16.00  42.00   0.50    0.05    --  -40.81  19.00  60.00   52
 52  \w     16.00  42.00   0.50    0.05    --  -40.81  19.00  90.00   52
 53  \w     16.00  41.00   0.50    0.05    --  -40.81  19.00 120.00   50
 54  \w     -8.00  32.00   0.50    0.05    --  -50.00  30.00 150.00   80
 55  \w    -81.00  11.00   0.50    0.05    --  -50.00  85.00  76.00  184
 56  \w    -54.00 -29.00   0.50    0.05    --  -40.81  85.00  76.00   50
 57  \w     24.00  73.00   0.50    0.05    --   41.06  38.00 -90.00   98
 58  \w    -30.00  -5.00   0.50    0.05    --   10.00 105.00  33.49   50
 59  \w    -29.00  -4.00   0.50    0.05    --  -30.00 -74.00  66.11   50
 60  \w    -36.00 -11.00   0.50    0.05    --  -34.00 -70.00-178.70   50
 61  \w    -41.00 -16.00   0.50    0.05    --  -38.00 -68.00  49.46   50
 62  \w    -44.00  33.00   0.50    0.05    --  -41.06  57.00-120.00  154
 63  \w     78.00 119.00   0.50    0.05    --   41.06  38.00 -90.00   82
 64  \w    -45.00 -19.00   0.50    0.05    --  -42.00 -67.00  -3.10   52
 65  \w    -46.00 -21.00   0.50    0.05    --  -42.00 -67.00 -50.50   50
 66  \w    -46.00 -21.00   0.50    0.05    --  -42.00 -67.00 125.89   50
 67  \w    -51.00 -26.00   0.50    0.05    --  -46.00 -65.00 -14.69   50
 68  \w    -60.00 -30.00   0.50    0.05    --  -50.00 -60.00  89.27   60
 69  \w    -28.00  27.00   0.50    0.05    --  -50.00  45.00   0.00  110
 70  \w     -5.00  21.00   0.50    0.05    --  -50.00  30.00 -90.00   52
 71  \w    -99.00 -42.00   0.50    0.05    --  -50.00 125.00  30.00  114
 72  \w    -56.00 -31.00   0.50    0.05    --  -50.00 -62.00-136.32   50
 73  \w    -32.00   6.00   0.50    0.05    --  -50.00  45.00 -30.00   76
 74  \w    -56.00 -31.00   0.50    0.05    --  -50.00 -62.00-105.08   50
 75  \w    -56.00 -31.00   0.50    0.05    --  -50.00 -62.00-167.10   50
 76  \w    -59.00 -29.00   0.50    0.05    --  -50.00 -56.00 145.15   60
 77  \w    -55.00 -29.00   0.50    0.05    --  -50.00 -62.00 -79.79   52
 78  \w    -58.00 -30.00   0.50    0.05    --  -50.00 -60.00  46.10   56
 79  \w    -59.00 -30.00   0.50    0.05    --  -50.00 -60.00  27.18   58
 80  \w    -58.00 -29.00   0.50    0.05    --  -50.00 -55.00 107.45   58
 81  \w    -58.00 -32.00   0.50    0.05    --  -50.00 -58.00 -55.34   52
 82  \w    -54.00 -29.00   0.50    0.05    --  -50.00 -62.00 104.92   50
 83  \w    -61.00 -32.00   0.50    0.05    --  -50.00 -57.00 -16.60   58
 84  \w    138.00 167.00   0.50    0.05    --  108.87  61.00 -60.00   58
 85  \w    150.00 175.00   0.50    0.05    --  108.87  45.00-150.00   50
 86  \w     89.00 116.00   0.50    0.05    --  108.87  61.00 -60.00   54
 87  \w     89.00 115.00   0.50    0.05    --  108.87  61.00  60.00   52
 88  \w     89.00 115.00   0.50    0.05    --  108.87  61.00-150.00   52
 89  \w     89.00 115.00   0.50    0.05    --  108.87  45.00 120.00   52
 90  \w     88.00 117.00   0.50    0.05    --  108.87  45.00-150.00   58
 91  \w    148.00 173.00   0.50    0.05    --  108.87  45.00-120.00   50
 92  \w     88.00 117.00   0.50    0.05    --  108.87  45.00-120.00   58
 93  \w    143.00 173.00   0.50    0.05    --  108.87  45.00  30.00   60
 94  \w     89.00 114.00   0.50    0.05    --  108.87  61.00   0.00   50
 95  \w     90.00 120.00   0.50    0.05    --  108.87  45.00  90.00   60
 96  \w    144.00 170.00   0.50    0.05    --  108.87  45.00   0.00   52
 97  \w     88.00 114.00   0.50    0.05    --  108.87  45.00  30.00   52
 98  \w    141.00 172.00   0.50    0.05    --  108.87  45.00-180.00   62
 99  \w     88.00 117.00   0.50    0.05    --  108.87  45.00   0.00   58
100  \w     88.00 114.00   0.50    0.05    --  108.87  45.00 -30.00   52
101  \w    148.00 174.00   0.50    0.05    --  108.87  61.00-180.00   52
102  \w     89.00 115.00   0.50    0.05    --  108.87  61.00-180.00   52
103  \w    148.00 174.00   0.50    0.05    --  108.87  45.00 -90.00   52
104  \w    144.00 175.00   0.50    0.05    --  108.87  61.00 -90.00   62
105  \w     91.00 117.00   0.50    0.05    --  108.87  61.00 -90.00   52
106  \w     88.00 114.00   0.50    0.05    --  108.87  45.00 -90.00   52
107  \w    134.00 172.00   0.50    0.05    --  108.87  61.00   0.00   76
108  \w     89.00 115.00   0.50    0.05    --  108.87  61.00  30.00   52
109  \w    147.00 173.00   0.50    0.05    --  108.87  61.00  30.00   52
110  \w    141.00 170.00   0.50    0.05    --  108.87  45.00 150.00   58
111  \w     89.00 115.00   0.50    0.05    --  108.87  61.00 -30.00   52
112  \w     89.00 115.00   0.50    0.05    --  108.87  45.00-180.00   52
113  \w     88.00 113.00   0.50    0.05    --  108.87  45.00  60.00   50
114  \w    129.00 155.00   0.50    0.05    --  108.87  61.00-150.00   52
115  \w     89.00 114.00   0.50    0.05    --  108.87  61.00-120.00   50
116  \w    149.00 175.00   0.50    0.05    --  108.87  61.00-120.00   52
117  \w     88.00 114.00   0.50    0.05    --  108.87  45.00 -60.00   52
118  \w    130.00 175.00   0.50    0.05    --  108.87  61.00 120.00   90
119  \w     89.00 115.00   0.50    0.05    --  108.87  61.00  90.00   52
120  \w     90.00 116.00   0.50    0.05    --  108.87  61.00 120.00   52
121  \w    148.00 175.00   0.50    0.05    --  108.87  61.00 150.00   54
122  \w     89.00 121.00   0.50    0.05    --  108.87  45.00 150.00   64
123  \w     89.00 119.00   0.50    0.05    --  108.87  61.00 150.00   60
124  \w    134.00 165.00   0.50    0.05    --  108.87  61.00  60.00   62
;
_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      -0.0659742000
_diffrn_orient_matrix_UB_12      0.0783279000
_diffrn_orient_matrix_UB_13      -0.1060875000
_diffrn_orient_matrix_UB_21      0.0109997000
_diffrn_orient_matrix_UB_22      -0.1066071000
_diffrn_orient_matrix_UB_23      -0.0312402000
_diffrn_orient_matrix_UB_31      -0.1133629000
_diffrn_orient_matrix_UB_32      -0.0383293000
_diffrn_orient_matrix_UB_33      0.0576488000
_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     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33926
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        62.498
_diffrn_reflns_theta_max         62.498
_diffrn_reflns_theta_min         3.578
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.409
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49747
_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 yellow'
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             902
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         1.755
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 4457 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         10359
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0750P)^2^+5.4696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.811
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                10233
_reflns_number_total             10359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00214e1.cif
_cod_data_source_block           n
_cod_depositor_comments
'Adding full bibliography for 7720400--7720402.cif.'
_cod_database_code               7720402
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O F S Dy '
_reflns_odcompleteness_completeness 99.36
_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 N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C31-N12
 1.3 with sigma of 0.01
 N13-C35
 1.3 with sigma of 0.01
 N12-C34
 1.49 with sigma of 0.01
 C38-N13
 1.49 with sigma of 0.01
 C33-N12
 1.49 with sigma of 0.01
 N13-C37
 1.49 with sigma of 0.01
 C37-N13
 1.49 with sigma of 0.02
 N13-C38
 1.49 with sigma of 0.01
 Dy2-H2WA \\sim Dy2-H2WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C38: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
C31 \\sim C32: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
C35 \\sim C36: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
O9 \\sim C35: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
N13 \\sim C37: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
N13 \\sim C38: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
O8 \\sim C31: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
N12 \\sim C31: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O4W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N12) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C32) = Uanis(C33)
4.a Riding coordinates:
 O4W(H4WA,H4WB)
4.b Free rotating group:
 O2W(H2WA,H2WB)
4.c Rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C16(H16), C17(H17),
 C18(H18), C20(H20), C24(H24), C25(H25)
4.e X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N10(H10A,H10B)
4.f Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              70850
_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 2.105
_oxdiff_exptl_absorpt_empirical_full_min 0.626