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_7720401
_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 Gd8 N40 O44'
_chemical_formula_sum            'C108 H104 Gd8 N40 O44'
_chemical_formula_weight         3924.31
_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                 118.271(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.5485(8)
_cell_length_b                   18.1561(4)
_cell_length_c                   28.8794(8)
_cell_measurement_reflns_used    18669
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      74.1990
_cell_measurement_theta_min      3.6820
_cell_volume                     15030.7(8)
_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      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -62.00 -36.00   0.50    0.50    --  -40.81  80.00 -53.00   52
  2  \w    -17.00  68.00   0.50    0.50    --   40.81 -80.00-176.00  170
  3  \w    -56.00 -30.00   0.50    0.50    --  -50.00  80.00 -53.00   52
  4  \w    103.00 167.00   0.50    1.00    --  108.87  80.00 -53.00  128
  5  \w     47.00  72.00   0.50    1.00    --  108.87 -80.00-176.00   50
  6  \w     16.00  41.00   0.50    0.50    --  -40.81  19.00  60.00   50
  7  \w     16.00  42.00   0.50    0.50    --  -40.81  19.00  30.00   52
  8  \w    -34.00   5.00   0.50    0.50    --  -40.81  80.00 -53.00   78
  9  \w     16.00  41.00   0.50    0.50    --  -40.81  19.00 -90.00   50
 10  \w     16.00  42.00   0.50    0.50    --  -40.81  19.00-180.00   52
 11  \w     16.00  41.00   0.50    0.50    --  -40.81  19.00  90.00   50
 12  \w     16.00  42.00   0.50    0.50    --  -40.81  19.00-120.00   52
 13  \w    -38.00  16.00   0.50    0.50    --   40.81 -38.00  90.00  108
 14  \w     20.00  46.00   0.50    0.50    --   40.81  63.00  42.58   52
 15  \w     22.00  48.00   0.50    0.50    --   40.81  63.00 -48.92   52
 16  \w     27.00  53.00   0.50    0.50    --   40.81  59.00  94.05   52
 17  \w     22.00  56.00   0.50    0.50    --   40.81  60.00 -63.83   68
 18  \w     20.00  45.00   0.50    0.50    --   40.81  63.00  77.02   50
 19  \w     21.00  47.00   0.50    0.50    --   40.81  63.00-105.13   52
 20  \w     20.00  46.00   0.50    0.50    --   40.81  63.00 102.86   52
 21  \w     -8.00  30.00   0.50    0.50    --  -50.00  30.00 -30.00   76
 22  \w     -6.00  21.00   0.50    0.50    --  -50.00  30.00  90.00   54
 23  \w    -59.00 -30.00   0.50    0.50    --  -50.00 -61.00  60.00   58
 24  \w     -2.00  32.00   0.50    0.50    --  -50.00  30.00   0.00   68
 25  \w    -30.00  18.00   0.50    0.50    --  -50.00  45.00  30.00   96
 26  \w     -9.00  17.00   0.50    0.50    --  -50.00  30.00-120.00   52
 27  \w     35.00 100.00   0.50    1.00    --  108.87-125.00 -30.00  130
 28  \w     37.00  70.00   0.50    1.00    --  108.87 -77.00  90.00   66
 29  \w     94.00 121.00   0.50    1.00    --  108.87  61.00-120.00   54
 30  \w     66.00 100.00   0.50    1.00    --  108.87-125.00-180.00   68
 31  \w     74.00  99.00   0.50    1.00    --  108.87-125.00 -60.00   50
 32  \w     34.00  59.00   0.50    1.00    --  108.87 -77.00 150.00   50
 33  \w    146.00 175.00   0.50    1.00    --  108.87 125.00  30.00   58
 34  \w     43.00  69.00   0.50    1.00    --  108.87-125.00 -60.00   52
 35  \w     89.00 158.00   0.50    1.00    --  108.87  30.00 -30.00  138
 36  \w    140.00 171.00   0.50    1.00    --  108.87  77.00   0.00   62
 37  \w     78.00 133.00   0.50    1.00    --  108.87  15.00 150.00  110
 38  \w    103.00 155.00   0.50    1.00    --  108.87  30.00-120.00  104
 39  \w     98.00 124.00   0.50    1.00    --  108.87  45.00  60.00   52
 40  \w     90.00 127.00   0.50    1.00    --  108.87  30.00 -90.00   74
 41  \w     99.00 131.00   0.50    1.00    --  108.87  77.00   0.00   64
 42  \w    102.00 170.00   0.50    1.00    --  108.87 125.00 -30.00  136
 43  \w     89.00 173.00   0.50    1.00    --  108.87  45.00 -90.00  168
 44  \w     95.00 149.00   0.50    1.00    --  108.87 125.00 120.00  108
 45  \w     38.00  99.00   0.50    1.00    --  108.87-125.00-150.00  122
 46  \w    103.00 135.00   0.50    1.00    --  108.87 125.00   0.00   64
 47  \w     32.00  84.00   0.50    1.00    --  108.87 -95.00  90.00  104
 48  \w    150.00 175.00   0.50    1.00    --  108.87 125.00  60.00   50
 49  \w     90.00 134.00   0.50    1.00    --  108.87 125.00  60.00   88
 50  \w     97.00 153.00   0.50    1.00    --  108.87  30.00  90.00  112
 51  \w     38.00  91.00   0.50    1.00    --  108.87 -95.00-150.00  106
 52  \w     32.00  84.00   0.50    1.00    --  108.87 -95.00  30.00  104
 53  \w     37.00  70.00   0.50    1.00    --  108.87 -77.00 -30.00   66
 54  \w    102.00 133.00   0.50    1.00    --  108.87  15.00  30.00   62
 55  \w     36.00  61.00   0.50    1.00    --  108.87-125.00-180.00   50
 56  \w     41.00  67.00   0.50    1.00    --  108.87 -77.00 120.00   52
 57  \w    128.00 161.00   0.50    1.00    --  108.87  30.00   0.00   66
 58  \w     96.00 122.00   0.50    1.00    --  108.87  30.00   0.00   52
 59  \w     32.00  82.00   0.50    1.00    --  108.87 -95.00  60.00  100
 60  \w     35.00  71.00   0.50    1.00    --  108.87 -77.00-120.00   72
 61  \w    103.00 129.00   0.50    1.00    --  108.87 125.00  30.00   52
 62  \w     39.00  70.00   0.50    1.00    --  108.87 -77.00 -60.00   62
 63  \w     64.00  90.00   0.50    1.00    --  108.87 -95.00 -90.00   52
 64  \w     89.00 162.00   0.50    1.00    --  108.87  30.00  60.00  146
;
_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      0.0379219000
_diffrn_orient_matrix_UB_12      -0.0305869000
_diffrn_orient_matrix_UB_13      0.0527680000
_diffrn_orient_matrix_UB_21      -0.0316180000
_diffrn_orient_matrix_UB_22      -0.0659778000
_diffrn_orient_matrix_UB_23      -0.0051029000
_diffrn_orient_matrix_UB_31      0.0212066000
_diffrn_orient_matrix_UB_32      -0.0437343000
_diffrn_orient_matrix_UB_33      -0.0292902000
_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  0.0871
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            82338
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        63.996
_diffrn_reflns_theta_max         63.996
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52015
_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    1.734
_exptl_crystal_description       plate
_exptl_crystal_F_000             7584
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.500
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         12462
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0865P)^2^+22.4158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8652
_reflns_number_total             12462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00214e1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7720400--7720402.cif.'
_cod_original_cell_volume        15030.7(7)
_cod_database_code               7720401
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFGd
_reflns_odcompleteness_completeness 99.93
_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
 H40B-H42
 2.2 with sigma of 0.02
 Gd3-H3WA \\sim Gd3-H3WB
 with sigma of 0.02
 Gd4-H4WA \\sim Gd4-H4WB
 with sigma of 0.02
 Gd2-H2WA \\sim Gd2-H2WB
 with sigma of 0.02
3.a Riding coordinates:
 C40(H40A,H40B,H40C), O1W(H1WA,H1WB), O3W(H3WA,H3WB)
3.b Free rotating group:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12), C16(H16), C17(H17),
 C18(H18), C21(H21), C24(H24), C25(H25), C29(H29), C30(H30), C31(H31), C34(H34),
  C37(H37), C38(H38), C42(H42), C43(H43), C44(H44), C47(H47), C50(H50), C51(H51)
3.d X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N10(H10A,H10B), N15(H15A,H15B), N20(H20A,H20B)
3.e 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              10654
_shelx_fab_checksum              50866
_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 3.237
_oxdiff_exptl_absorpt_empirical_full_min 0.465