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_7720400
_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         'C108 H104 Dy8 N40 O44'
_chemical_formula_sum            'C108 H104 Dy8 N40 O44'
_chemical_formula_weight         3966.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2026-01-10
_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                90
_cell_angle_beta                 126.481(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.5183(10)
_cell_length_b                   18.0719(2)
_cell_length_c                   31.6045(9)
_cell_measurement_reflns_used    18097
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.4340
_cell_measurement_theta_min      3.8760
_cell_volume                     14933.6(10)
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     59.00  90.00   0.50    0.40    --  108.87 -95.00 150.00   62
  2  \w     36.00  79.00   0.50    0.40    --  108.87-125.00  90.00   86
  3  \w     34.00  60.00   0.50    0.40    --  108.87 -95.00   0.00   52
  4  \w     65.00  91.00   0.50    0.40    --  108.87 -95.00   0.00   52
  5  \w     41.00  67.00   0.50    0.40    --  108.87 -95.00 -90.00   52
  6  \w     44.00  69.00   0.50    0.40    --  108.87 -77.00 -90.00   50
  7  \w     40.00  70.00   0.50    0.40    --  108.87 -77.00-150.00   60
  8  \w     38.00  70.00   0.50    0.40    --  108.87 -77.00-180.00   64
  9  \w     38.00  64.00   0.50    0.40    --  108.87 -77.00-120.00   52
 10  \w     40.00  67.00   0.50    0.40    --  108.87 -77.00  60.00   54
 11  \w     45.00  71.00   0.50    0.40    --  108.87 -77.00  90.00   52
 12  \w     34.00  68.00   0.50    0.40    --  108.87 -77.00 120.00   68
 13  \w     87.00 125.00   0.50    0.40    --  108.87  15.00 150.00   76
 14  \w    100.00 130.00   0.50    0.40    --  108.87  77.00  60.00   60
 15  \w    136.00 174.00   0.50    0.40    --  108.87  77.00  60.00   76
 16  \w    107.00 168.00   0.50    0.40    --  108.87  77.00 -30.00  122
 17  \w     90.00 152.00   0.50    0.40    --  108.87  30.00 -90.00  124
 18  \w    114.00 161.00   0.50    0.40    --  108.87  30.00-120.00   94
 19  \w     88.00 167.00   0.50    0.40    --  108.87  62.00 -42.00  158
 20  \w     75.00 129.00   0.50    0.40    --  108.87  15.00  90.00  108
 21  \w    -22.00  11.00   0.50    0.12    --   41.06 -62.00 179.00   66
 22  \w     23.00  49.00   0.50    0.12    --   41.06 -62.00 179.00   52
 23  \w    -27.00  26.00   0.50    0.12    --  -41.06  62.00 -42.00  106
 24  \w    -54.00 -17.00   0.50    0.12    --  -50.00  61.00 -90.00   74
 25  \w     -4.00  21.00   0.50    0.12    --  -50.00  61.00 -90.00   50
 26  \w     -9.00  32.00   0.50    0.12    --  -50.00  30.00-180.00   82
 27  \w    -39.00 -14.00   0.50    0.12    --  -50.00  62.00 -42.00   50
 28  \w     -2.00  24.00   0.50    0.12    --  -50.00  30.00  30.00   52
 29  \w      1.00  27.00   0.50    0.12    --  -50.00  30.00  90.00   52
 30  \w    -53.00  25.00   0.50    0.12    --  -50.00  61.00  60.00  156
 31  \w    -38.00  15.00   0.50    0.12    --   41.06 -38.00 -90.00  106
;
_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      0.0364607000
_diffrn_orient_matrix_UB_12      0.0229793000
_diffrn_orient_matrix_UB_13      -0.0136507000
_diffrn_orient_matrix_UB_21      -0.0393861000
_diffrn_orient_matrix_UB_22      0.0574073000
_diffrn_orient_matrix_UB_23      -0.0394373000
_diffrn_orient_matrix_UB_31      0.0242563000
_diffrn_orient_matrix_UB_32      0.0587110000
_diffrn_orient_matrix_UB_33      0.0439662000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39305
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        59.993
_diffrn_reflns_theta_max         59.993
_diffrn_reflns_theta_min         3.735
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49177
_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    1.764
_exptl_crystal_description       block
_exptl_crystal_F_000             7648
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.620
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         11047
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+109.6239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9334
_reflns_number_total             11047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00214e1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7720400--7720402.cif.'
_cod_original_cell_volume        14933.6(9)
_cod_database_code               7720400
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNODy
_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
 H42-H40C
 2.2 with sigma of 0.01
 Dy2-H2WA \\sim Dy2-H2WB
 with sigma of 0.02
 Dy1-H1WA \\sim Dy1-H1WB
 with sigma of 0.02
3.a Riding coordinates:
 C40(H40A,H40B,H40C)
3.b Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.c Rotating group:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C21(H21), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C34(H34),
  C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C47(H47), C51(H51), C52(H52)
3.e X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N10(H10A,H10B), N15(H15A,H15B), N20(H20A,H20B)
3.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C27(H27A,H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94633
_shelx_fab_checksum              19175
_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 2.076
_oxdiff_exptl_absorpt_empirical_full_min 0.648