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_7717438
_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         'C73 H79 Cl F5 Gd5 N20 O20'
_chemical_formula_sum            'C73 H79 Cl F5 Gd5 N20 O20'
_chemical_formula_weight         2537.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-09-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.760(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6636(5)
_cell_length_b                   17.1881(3)
_cell_length_c                   44.8621(10)
_cell_measurement_reflns_used    18497
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      30.0760
_cell_measurement_theta_min      1.4560
_cell_volume                     17644.7(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  66.26   0.38   13.00    --   -8.90  45.00 104.79  227
  2  \w    -61.00  69.34   0.38   13.00    --   -8.90  45.00   0.00  343
  3  \w    -91.00 -41.98   0.38   13.00    --   -8.90  45.00 104.79  129
;
_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      0.0200590000
_diffrn_orient_matrix_UB_12      -0.0058108000
_diffrn_orient_matrix_UB_13      -0.0091519000
_diffrn_orient_matrix_UB_21      0.0023773000
_diffrn_orient_matrix_UB_22      0.0408584000
_diffrn_orient_matrix_UB_23      -0.0015497000
_diffrn_orient_matrix_UB_31      0.0235351000
_diffrn_orient_matrix_UB_32      0.0008125000
_diffrn_orient_matrix_UB_33      0.0134441000
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            52103
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         1.482
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19591
_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    1.835
_exptl_crystal_description       plate
_exptl_crystal_F_000             9400
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.096
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         14640
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0586P)^2^+79.1062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12089
_reflns_number_total             14640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02310b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7717437--7717440.cif.'
_cod_database_code               7717438
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFGe
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C68-O19
 1.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C63) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C69)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O15(H15), O16(H16A), O17(H17A), O18(H18A), O19(H19A), O20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C64(H64A,H64B), C66(H66A,H66B), C68(H68A,H68B), C70(H70A,H70B)
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), N18(H18)
4.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C69(H69A,H69B,
 H69C), C71(H71A,H71B,H71C)
;
_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 1 ethanol molecule, 3 water molcules in one unit cell, which is 
consistent with the number of masked electrons.
;
_shelx_res_checksum              45738
_shelx_hkl_checksum              47892
_shelx_fab_checksum              30988
_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 5.491
_oxdiff_exptl_absorpt_empirical_full_min 0.444