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_7717440
_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         'C78 H58 Cl2 Dy6 F6 N24 O22, 6(C2 H6 O)'
_chemical_formula_sum            'C90 H94 Cl2 Dy6 F6 N24 O28'
_chemical_formula_weight         3119.79
_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             2024-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-22 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                79.7510(10)
_cell_angle_beta                 86.8820(10)
_cell_angle_gamma                75.0230(10)
_cell_formula_units_Z            2
_cell_length_a                   14.69440(10)
_cell_length_b                   17.5692(2)
_cell_length_c                   21.4760(2)
_cell_measurement_reflns_used    110284
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      40.7330
_cell_measurement_theta_min      1.6590
_cell_volume                     5270.42(9)
_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   -105.00  65.00   0.50    1.50    --  -20.00  45.00   0.00  340
  2  \w   -105.00  65.00   0.50    1.50    --  -20.00  45.00  90.00  340
  3  \w   -105.00  65.00   0.50    1.50    --  -20.00  45.00 180.00  340
  4  \w    -97.00  73.00   0.50    1.50    --   -8.00  45.00 270.00  340
  5  \w   -125.00  45.00   0.50    1.50    --  -40.00  45.00   0.00  340
  6  \w   -125.00  45.00   0.50    1.50    --  -40.00  45.00  45.00  340
  7  \w   -125.00  45.00   0.50    1.50    --  -40.00  45.00 135.00  340
  8  \w   -125.00  45.00   0.50    1.50    --  -40.00  45.00 205.00  340
;
_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      0.0334019000
_diffrn_orient_matrix_UB_12      -0.0060909000
_diffrn_orient_matrix_UB_13      0.0241925000
_diffrn_orient_matrix_UB_21      0.0024157000
_diffrn_orient_matrix_UB_22      -0.0414963000
_diffrn_orient_matrix_UB_23      0.0056887000
_diffrn_orient_matrix_UB_31      0.0370865000
_diffrn_orient_matrix_UB_32      -0.0062763000
_diffrn_orient_matrix_UB_33      -0.0225596000
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            150534
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.300
_diffrn_reflns_theta_min         1.676
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65779
_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    1.966
_exptl_crystal_description       block
_exptl_crystal_F_000             3020
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1473
_refine_ls_number_reflns         21374
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      4.098
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+8.6062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19662
_reflns_number_total             21374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02310b2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7717437--7717440.cif.'
_cod_database_code               7717440
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOClDy
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O18-O19
 0.85 with sigma of 0.01
 O19-H19A
 0.87 with sigma of 0.01
 C91'-O26'
 1.43 with sigma of 0.01
 C92'-C91'
 1.53 with sigma of 0.01
 C91-O26
 1.43 with sigma of 0.01
 C91-C92
 1.53 with sigma of 0.01
 C79A-C21A = C79-C21
 1.54 with sigma of 0.02
 O21-C21 = O21A-C21A
 1.4 with sigma of 0.02
 C79-C21
 1.54 with sigma of 0.02
 Dy4-O19
 2.868868 with sigma of 0.02
 Dy4-H19A
 2.875827 with sigma of 0.02
 C87-H19A
 1.92001 with sigma of 0.02
 H26'-C21 \\sim H26'-C21A
 with sigma of 0.02
 H26'-O21 \\sim H26'-C79A
 with sigma of 0.04
 H26'-C79 \\sim H26'-O21A
 with sigma of 0.04
 O21-C79 \\sim C79A-O21A
 with sigma of 0.04
 Dy2-H1WA \\sim Dy2-H1WB
 with sigma of 0.02
3. Rigid bond restraints
 Dy2, O1W
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
4. Uiso/Uaniso restraints and constraints
C79 \\sim C79A \\sim C21A \\sim C21 \\sim O21A \\sim O21: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C92' \\sim C92: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Dy2 \\sim O1W: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01 within 2A
Uanis(O26) \\sim Ueq, Uanis(O26') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O22) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.005
5. Others
 Sof(O26')=Sof(H26')=Sof(C91')=Sof(H91C)=Sof(H91D)=Sof(C92')=Sof(H92D)=
 Sof(H92E)=Sof(H92F)=1-FVAR(1)
 Sof(O26)=Sof(H26)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=
 Sof(H92C)=FVAR(1)
 Sof(O21A)=Sof(H21C)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(C79A)=Sof(H79D)=
 Sof(H79E)=Sof(H79F)=1-FVAR(2)
 Sof(O21)=Sof(H21)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=FVAR(2)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O22(H22A), O23(H23A)
6.b Rotating group:
 O2W(H2WA,H2WB)
6.c Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C77(H77A,H77B), C81(H81A,H81B), C83(H83A,H83B), C85(H85A,
 H85B), C87(H87A,H87B), C91(H91A,H91B), C91'(H91C,H91D), C21(H21A,H21B),
 C21A(H21D,H21E)
6.d Me refined with riding coordinates:
 C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C92(H92A,H92B,H92C), C92'(H92D,H92E,H92F),
 C79(H79A,H79B,H79C), C79A(H79D,H79E,H79F)
6.e 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), 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), C62(H62), C64(H64), C65(H65), C67(H67),
 C70(H70), C71(H71), C72(H72), C89(H89)
6.f Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C)
6.g Idealised tetrahedral OH refined as rotating group:
 O20(H20), O24(H24A), O25(H25), O26(H26), O26'(H26'), O21(H21), O21A(H21C)
;
_shelx_res_checksum              71121
_shelx_hkl_checksum              41501
_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 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.651