Slow magnetic relaxation of mononuclear complexes based on uncommon Kramers lanthanide ions CeIII, SmIII and YbIII
Leng, Ji-Dong; Hua, Qiu-Yan; Liu, Wen-Ting; Tao, Ze-Xian; Tan, Nai-Wen; Wang, Yu-Fei; Lin, Wei-Quan; Dalton Transactions  (2022) –; doi:10.1039/D2DT00766E

data_7710719
_publ_section_title
;
 Slow magnetic relaxation of mononuclear complexes based on uncommon
 Kramers lanthanide ions CeIII, SmIII and YbIII
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00766E
_journal_year                    2022
_chemical_formula_moiety
'C60 H48 Cl2 O4 P4 Yb, Cl H0.783 O0.392, C4 H8 O, 1.608(H2 O)'
_chemical_formula_sum            'C64 H60 Cl3 O7 P4 Yb'
_chemical_formula_weight         1344.39
_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     dual
_audit_creation_date             2022-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-19 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                91.4607(3)
_cell_angle_beta                 101.8219(3)
_cell_angle_gamma                95.1610(3)
_cell_formula_units_Z            2
_cell_length_a                   13.50187(5)
_cell_length_b                   14.30058(5)
_cell_length_c                   15.59805(6)
_cell_measurement_reflns_used    67410
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.4700
_cell_measurement_theta_min      2.8810
_cell_volume                     2932.929(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_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    -85.00 -33.00   0.50    0.05    --  -46.37 -23.00 145.00  104
  2  \w    -61.00  30.00   0.50    0.05    --  -46.37  23.00 -49.00  182
  3  \w    -16.00  42.00   0.50    0.05    --   46.37 -23.00 145.00  116
  4  \w     33.00  74.00   0.50    0.05    --   46.37  23.00 -49.00   82
  5  \w    -64.00 -38.00   0.50    0.10    -- -102.00  23.00 -49.00   52
  6  \w   -156.00-131.00   0.50    0.10    -- -102.00 -23.00 145.00   50
  7  \w     39.00  65.00   0.50    0.10    --  107.00 -23.00 145.00   52
  8  \w    135.00 176.00   0.50    0.10    --  107.00  23.00 -49.00   82
  9  \w    -94.00 -11.00   0.50    0.05    --  -46.37 125.00  30.00  166
 10  \w    -57.00 -32.00   0.50    0.05    --  -46.37 -42.00   5.67   50
 11  \w     62.00  88.00   0.50    0.05    --   46.37  57.00-120.00   52
 12  \w     23.00  68.00   0.50    0.05    --   46.37  77.00-150.00   90
 13  \w     23.00 115.00   0.50    0.05    --   46.37  77.00  90.00  184
 14  \w     23.00  76.00   0.50    0.05    --   46.37  77.00 150.00  106
 15  \w     23.00  69.00   0.50    0.05    --   46.37  77.00  60.00   92
 16  \w     23.00  82.00   0.50    0.05    --   46.37  77.00 -90.00  118
 17  \w     77.00 111.00   0.50    0.05    --   46.37  37.00  30.00   68
 18  \w     34.00  88.00   0.50    0.05    --   46.37  37.00-180.00  108
 19  \w     24.00 101.00   0.50    0.05    --   46.37  77.00 -60.00  154
 20  \w     23.00 117.00   0.50    0.05    --   46.37  77.00 -30.00  188
 21  \w     30.00  58.00   0.50    0.05    --   46.37  57.00-120.00   56
 22  \w     23.00  48.00   0.50    0.05    --   46.37  77.00  30.00   50
 23  \w     78.00 116.00   0.50    0.05    --   46.37  77.00 150.00   76
 24  \w     30.00  63.00   0.50    0.05    --   46.37  57.00  60.00   66
 25  \w     75.00 100.00   0.50    0.05    --   46.37  77.00-150.00   50
 26  \w     74.00 111.00   0.50    0.05    --   46.37  77.00  60.00   74
 27  \w     15.00  92.00   0.50    0.05    --   46.37-125.00  60.00  154
 28  \w     32.00  71.00   0.50    0.05    --   46.37  37.00  30.00   78
 29  \w   -146.00 -83.00   0.50    0.10    -- -102.00 -66.00 147.93  126
 30  \w   -145.00 -83.00   0.50    0.10    -- -102.00 -64.00 113.96  124
 31  \w   -128.00 -78.00   0.50    0.10    -- -102.00 -76.00-175.21  100
 32  \w   -154.00 -78.00   0.50    0.10    -- -102.00 -76.00 -24.35  152
 33  \w   -131.00 -85.00   0.50    0.10    -- -102.00 -58.00 114.24   92
 34  \w   -174.00-137.00   0.50    0.10    -- -102.00 -76.00-175.21   74
 35  \w   -173.00-132.00   0.50    0.10    -- -102.00 -63.00-159.86   82
 36  \w   -126.00-100.00   0.50    0.10    -- -102.00  77.00  90.00   52
 37  \w    -80.00 -37.00   0.50    0.10    -- -102.00  77.00  90.00   86
 38  \w   -171.00 -79.00   0.50    0.10    -- -102.00 -74.00-136.82  184
 39  \w   -174.00-109.00   0.50    0.10    -- -102.00 -76.00  28.85  130
 40  \w   -105.00 -78.00   0.50    0.10    -- -102.00 -77.00 120.00   54
 41  \w   -174.00-127.00   0.50    0.10    -- -102.00 -77.00 120.00   94
 42  \w   -104.00 -75.00   0.50    0.10    -- -102.00 -83.00-111.32   58
 43  \w   -169.00 -78.00   0.50    0.10    -- -102.00 -76.00 108.87  182
 44  \w   -174.00-113.00   0.50    0.10    -- -102.00 -83.00-111.32  122
 45  \w   -143.00 -78.00   0.50    0.10    -- -102.00 -77.00 -98.86  130
 46  \w   -175.00 -79.00   0.50    0.10    -- -102.00 -74.00 -15.79  192
 47  \w   -106.00 -78.00   0.50    0.10    -- -102.00 -78.00  17.63   56
 48  \w   -155.00-123.00   0.50    0.10    -- -102.00 -77.00  90.00   64
 49  \w   -105.00 -80.00   0.50    0.10    -- -102.00 -73.00 171.63   50
 50  \w   -116.00 -80.00   0.50    0.10    -- -102.00 -72.00-165.31   72
 51  \w   -169.00 -78.00   0.50    0.10    -- -102.00 -77.00 -30.00  182
 52  \w   -104.00 -78.00   0.50    0.10    -- -102.00 -77.00  90.00   52
 53  \w   -101.00 -76.00   0.50    0.10    -- -102.00 -81.00 107.15   50
 54  \w   -103.00 -75.00   0.50    0.10    -- -102.00 -83.00 -73.17   56
 55  \w   -174.00-149.00   0.50    0.10    -- -102.00 -77.00 -98.86   50
 56  \w   -175.00-142.00   0.50    0.10    -- -102.00 -72.00-165.31   66
 57  \w   -103.00 -78.00   0.50    0.10    -- -102.00 -77.00-150.00   50
 58  \w   -104.00 -78.00   0.50    0.10    -- -102.00 -76.00  28.85   52
 59  \w   -126.00 -79.00   0.50    0.10    -- -102.00 -74.00 -75.26   94
 60  \w   -119.00 -83.00   0.50    0.10    -- -102.00 -65.00-122.30   72
 61  \w   -173.00 -78.00   0.50    0.10    -- -102.00 -77.00 -60.00  190
 62  \w   -141.00 -84.00   0.50    0.10    -- -102.00 -61.00 -60.00  114
 63  \w   -103.00 -78.00   0.50    0.10    -- -102.00 -77.00 -90.00   50
 64  \w   -109.00 -84.00   0.50    0.10    -- -102.00 -63.00-159.86   50
 65  \w   -141.00 -83.00   0.50    0.10    -- -102.00 -65.00  68.59  116
 66  \w   -168.00-142.00   0.50    0.10    -- -102.00 -82.00-115.94   52
 67  \w   -101.00 -76.00   0.50    0.10    -- -102.00 -82.00-115.94   50
 68  \w   -138.00 -79.00   0.50    0.10    -- -102.00 -74.00 139.03  118
 69  \w   -157.00 -79.00   0.50    0.10    -- -102.00 -77.00  60.00  156
 70  \w   -104.00 -79.00   0.50    0.10    -- -102.00 -74.00 -50.24   50
 71  \w   -174.00-149.00   0.50    0.10    -- -102.00 -77.00-150.00   50
 72  \w   -103.00 -78.00   0.50    0.10    -- -102.00 -77.00   0.00   50
 73  \w   -108.00 -83.00   0.50    0.10    -- -102.00 -64.00  26.12   50
 74  \w   -169.00-143.00   0.50    0.10    -- -102.00 -64.00  26.12   52
 75  \w   -175.00 -80.00   0.50    0.10    -- -102.00 -73.00  49.99  190
 76  \w   -166.00-135.00   0.50    0.10    -- -102.00 -74.00 -75.26   62
 77  \w    -79.00 -30.00   0.50    0.10    -- -102.00 125.00-120.00   98
 78  \w   -116.00 -90.00   0.50    0.10    -- -102.00 125.00-120.00   52
 79  \w   -117.00 -76.00   0.50    0.10    -- -102.00 -81.00   9.75   82
 80  \w   -117.00 -35.00   0.50    0.10    -- -102.00 125.00   0.00  164
 81  \w   -104.00 -79.00   0.50    0.10    -- -102.00 -74.00 163.99   50
 82  \w   -105.00 -80.00   0.50    0.10    -- -102.00 -75.00 151.81   50
 83  \w   -113.00 -76.00   0.50    0.10    -- -102.00 -82.00  74.64   74
 84  \w     94.00 131.00   0.50    0.10    --  107.00 -77.00  30.00   74
 85  \w     58.00  87.00   0.50    0.10    --  107.00 -77.00  30.00   58
 86  \w     38.00 106.00   0.50    0.10    --  107.00 -94.00 -60.00  136
 87  \w     51.00 123.00   0.50    0.10    --  107.00-133.00-109.10  144
 88  \w     63.00 113.00   0.50    0.10    --  107.00-125.00-180.00  100
 89  \w     39.00 101.00   0.50    0.10    --  107.00 -94.00 150.00  124
 90  \w     39.00 115.00   0.50    0.10    --  107.00-125.00 120.00  152
 91  \w     35.00 107.00   0.50    0.10    --  107.00 -94.00-120.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0660964000
_diffrn_orient_matrix_UB_12      0.0865071000
_diffrn_orient_matrix_UB_13      -0.0208448000
_diffrn_orient_matrix_UB_21      0.0768964000
_diffrn_orient_matrix_UB_22      -0.0645936000
_diffrn_orient_matrix_UB_23      -0.0232993000
_diffrn_orient_matrix_UB_31      -0.0586272000
_diffrn_orient_matrix_UB_32      -0.0082353000
_diffrn_orient_matrix_UB_33      -0.0960494000
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            84890
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.081
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.671
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             1362
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.251
_refine_diff_density_min         -2.274
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0540P)^2^+7.0371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11701
_reflns_number_total             11944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00766e2.cif
_cod_data_source_block           yrc111314_ybcl-thf
_cod_original_cell_volume        2932.928(19)
_cod_database_code               7710719
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C124 H122 Cl4 O20 P8 Yb2 '
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(O7B)=Sof(H7BA)=Sof(H7BB)=1-FVAR(1)
 Sof(O7A)=Sof(H3A)=Sof(H7A)=FVAR(1)
4.a Free rotating group:
 O7A(H3A,H7A), O6(H6A,H6B), O7B(H7BA,H7BB)
4.b Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60)
;
_shelx_res_checksum              12867
_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 1.952
_oxdiff_exptl_absorpt_empirical_full_min 0.681