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_7717439
_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         'C118 H138.5 F8 Gd8 N32 Cl6 O51.25'
_chemical_formula_sum            'C118 H138.5 Cl6 F8 Gd8 N32 O51.25'
_chemical_formula_weight         4447.75
_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
_audit_creation_date             2024-10-22
_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                82.4240(10)
_cell_angle_beta                 79.9800(10)
_cell_angle_gamma                86.0980(10)
_cell_formula_units_Z            2
_cell_length_a                   18.6686(2)
_cell_length_b                   20.0759(2)
_cell_length_c                   21.9073(3)
_cell_measurement_reflns_used    59209
_cell_measurement_temperature    170.0(3)
_cell_measurement_theta_max      30.4470
_cell_measurement_theta_min      1.5520
_cell_volume                     8006.24(16)
_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_temperature      170.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_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    -50.00 -25.00   0.50    2.00    --    5.00  45.00 150.00   50
  2  \w    -82.00 -34.00   0.50    2.00    --   -8.90  45.00  90.00   96
  3  \w     -4.00  46.00   0.50    2.00    --   -8.90  45.00  90.00  100
  4  \w    -98.00  80.00   0.50    2.00    --   -8.90  45.00 164.41  356
  5  \w    -71.00 -40.00   0.50    2.00    --   -8.90  45.00  30.00   62
  6  \w     -3.00  80.00   0.50    2.00    --   -8.90  45.00  30.00  166
  7  \w     27.00  79.00   0.50    2.00    --   -8.90  45.00 -16.84  104
  8  \w    -40.00 -14.00   0.50    2.00    --   -8.90  45.00 -16.84   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            111623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.474
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48360
_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    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             3578
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.678
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1705
_refine_ls_number_reflns         37317
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0338P)^2^+6.8901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30279
_reflns_number_total             37317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02310b2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7717437--7717440.cif.'
_cod_original_formula_sum        'C118 H138.5 F8 Gd8 N32 Cl6 O51.25'
_cod_database_code               7717439
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Shared sites
{O29, O29W}
{O32, O32W}
3. Restrained distances
 O30-H30
 0.87 with sigma of 0.01
 O31-H31A
 0.87 with sigma of 0.01
 C101-O29
 1.42 with sigma of 0.01
 C102-O32
 1.42 with sigma of 0.02
 O32-C102
 1.42 with sigma of 0.01
 C103-H30
 1.896644 with sigma of 0.02
 Gd7-H30
 3.183875 with sigma of 0.02
 Gd5-H31A
 2.974604 with sigma of 0.02
 C104-H31A
 1.967465 with sigma of 0.02
4. Rigid bond restraints
 O29, C101
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O30, C103
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O31, C104
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O32, C102
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C101)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C102) \\sim Ueq, Uanis(O29) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O29) = Uanis(O29W)
Uanis(O32) = Uanis(O32W)
6. Others
 Fixed Sof: O29(0.5) C101(0.5) H10G(0.5) H10H(0.5) H10I(0.5) O29W(0.5)
 O32(0.5) C102(0.5) H10J(0.5) H10K(0.5) H10L(0.5) O32W(0.5)
7.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
7.b Me refined with riding coordinates:
 C104(H10D,H10E,H10F), C102(H10J,H10K,H10L)
7.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), C62(H62), C64(H64), C65(H65),
 C67(H67), C70(H70), C71(H71), C72(H72), C74(H74), C76(H76), C77(H77), C79(H79),
  C82(H82), C83(H83), C84(H84), C86(H86), C88(H88), C89(H89), C91(H91),
 C94(H94), C95(H95), C96(H96)
7.d Idealised Me refined as rotating group:
 C103(H10A,H10B,H10C), C101(H10G,H10H,H10I)
;
_smtbx_masks_special_details
;
Some solvents are disordered,and could not be modelled properly.Therefore
PLATON/SQUEEZE was used to remove the solvents,the solvents are estimated 
to be 12 methanol molecules,3 dichloromethane molecules, 3.25 water molcules
in one unit cell, which is consistent with the number of masked electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              304
_shelx_hkl_checksum              86357
_shelx_fab_checksum              1762
_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
;