Solvent-dependent Ln(III) clusters assembled by immobilization of CO<sub>2</sub> in air: zero-field single-molecule magnets and magnetic refrigerant materials.
Liu, Cai-Ming; Hao, Xiang; Hu, Zhao-Bo; Wen, He-Rui; Dalton transactions (Cambridge, England : 2003) 54 (2024) 96–107; doi:10.1039/d4dt02310b

data_7717437
_publ_section_title
;
 Solvent-dependent Ln(III) clusters assembled by immobilization of
 CO<sub>2</sub> in air: zero-field single-molecule magnets and magnetic
 refrigerant materials.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              96
_journal_page_last               107
_journal_paper_doi               10.1039/d4dt02310b
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C66 H54 Dy5 F5 N20 O22, 3(C H4 O), 3.5(H2 O)'
_chemical_formula_sum            'C69 H73 Dy5 F5 N20 O28.5'
_chemical_formula_weight         2545.95
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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             2024-10-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-31 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                105.243(2)
_cell_angle_beta                 102.278(2)
_cell_angle_gamma                100.5150(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4896(3)
_cell_length_b                   17.1556(3)
_cell_length_c                   19.5110(5)
_cell_measurement_reflns_used    30709
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      30.9710
_cell_measurement_theta_min      1.6660
_cell_volume                     4423.73(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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                 'CCD plate'
_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    -44.00 -17.00   0.50    7.50    --    5.00  45.00 168.64   54
  2  \w    -14.00  77.00   0.50    7.50    --  -10.70  45.00  77.28  182
  3  \w     -3.00  23.00   0.50    7.50    --  -10.70  45.00  30.00   52
  4  \w    -94.00 -62.00   0.50    7.50    --  -10.70  45.00 -19.89   64
  5  \w     22.00  64.00   0.50    7.50    --  -10.70  45.00 -19.89   84
  6  \w    -55.00 -29.00   0.50    7.50    --  -10.70  45.00  30.00   52
  7  \w    -99.00 -15.00   0.50    7.50    --  -10.70  45.00 150.00  168
  8  \w    -99.00 -34.00   0.50    7.50    --  -10.70  45.00  77.28  130
  9  \w    -91.00  78.00   0.50    7.50    --  -10.70  45.00 171.72  338
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120580000
_diffrn_orient_matrix_UB_12      0.0436401000
_diffrn_orient_matrix_UB_13      0.0181785000
_diffrn_orient_matrix_UB_21      -0.0502498000
_diffrn_orient_matrix_UB_22      -0.0015564000
_diffrn_orient_matrix_UB_23      -0.0044747000
_diffrn_orient_matrix_UB_31      0.0032963000
_diffrn_orient_matrix_UB_32      -0.0074114000
_diffrn_orient_matrix_UB_33      0.0344266000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.530
_diffrn_reflns_theta_max         24.530
_diffrn_reflns_theta_min         1.599
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
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    1.910
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         14744
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0628P)^2^+27.7934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12858
_reflns_number_total             14744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02310b2.cif
_cod_data_source_block           new
_cod_depositor_comments
'Adding full bibliography for 7717437--7717440.cif.'
_cod_original_cell_volume        4423.73(17)
_cod_original_formula_sum        'C69 H73 Dy5 F5 N20 O28.50'
_cod_database_code               7717437
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFDy
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Restrained distances
 O19-H19A
 0.85 with sigma of 0.01
 O20-H20
 0.85 with sigma of 0.01
 O21-C65
 1.43 with sigma of 0.01
 O21-H21
 0.85 with sigma of 0.01
 C71-O27
 1.43 with sigma of 0.01
 Dy4-H19A
 2.840214 with sigma of 0.02
 C66-H20
 1.891717 with sigma of 0.02
 Dy4-H20
 2.887304 with sigma of 0.02
 C64-H19A
 1.895834 with sigma of 0.02
 Dy4-H21
 2.872157 with sigma of 0.02
 C65-H21
 1.858101 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O3W) \\sim Ueq, Uanis(O7W) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C4) \\sim Ueq, Uanis(O4WB) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O4WA)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4WB) = Uanis(O4W) = Uanis(O4WA)
3. Others
 Fixed Sof: O3W(0.5) H3WA(0.5) H3WB(0.5) O7W(0.5) H7WA(0.5) H7WB(0.5) O6W(0.5)
 H6WA(0.5) H6WB(0.5) O4W(0.3333) O4WA(0.3333) O4WB(0.3333)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O17(H17A), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O7W(H7WA,H7WB),
 O6W(H6WA,H6WB)
4.b Ternary CH refined with riding coordinates:
 O18(H18)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14),
 C16(H16), C17(H17), C19(H19), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28),
  C29(H29), C31(H31), C34(H34), C35(H35), C36(H36), C38(H38), C40(H40),
 C41(H41), C43(H43), C46(H46), C47(H47), C48(H48), C50(H50), C52(H52), C53(H53),
  C55(H55), C58(H58), C59(H59), C60(H60)
4.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C)
4.e Idealised tetrahedral OH refined as rotating group:
 O22(H22A), O24(H24A), O27(H27)
;
_shelx_res_checksum              6321
_shelx_hkl_checksum              93580
_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 1.661
_oxdiff_exptl_absorpt_empirical_full_min 0.701