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_7710718
_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 Ce Cl3 O4 P4'
_chemical_formula_sum            'C60 H48 Ce Cl3 O4 P4'
_chemical_formula_weight         1203.33
_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   geom
_audit_creation_date             2022-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-09 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                98.4460(10)
_cell_angle_beta                 94.3080(10)
_cell_angle_gamma                114.7660(10)
_cell_formula_units_Z            2
_cell_length_a                   11.32160(10)
_cell_length_b                   12.4712(2)
_cell_length_c                   22.4085(2)
_cell_measurement_reflns_used    21711
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.6460
_cell_measurement_theta_min      3.9760
_cell_volume                     2808.71(6)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.955
_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    -56.00  27.00   0.50    0.40    --  -46.62  37.00  30.00  166
  2  \w    -56.00 -30.00   0.50    1.00    -- -102.00  30.00 -90.00   52
  3  \w    -60.00 -32.00   0.50    1.00    -- -102.00  77.00-180.00   56
  4  \w    -72.00 -33.00   0.50    1.00    -- -102.00 125.00-120.00   78
  5  \w    -67.00 -33.00   0.50    1.00    -- -102.00  30.00-180.00   68
  6  \w   -107.00 -80.00   0.50    1.00    -- -102.00  77.00-180.00   54
  7  \w   -115.00 -89.00   0.50    1.00    -- -102.00 125.00-120.00   52
  8  \w    -71.00  20.00   0.50    0.40    --  -46.62  86.00  42.00  182
  9  \w     31.00  58.00   0.50    0.40    --   46.62 -86.00 -76.00   54
 10  \w     34.00 117.00   0.50    1.00    --  107.00-125.00-180.00  166
 11  \w     68.00 107.00   0.50    1.00    --  107.00 -86.00 -76.00   78
 12  \w     43.00 115.00   0.50    1.00    --  107.00-125.00-120.00  144
 13  \w     46.00  79.00   0.50    1.00    --  107.00 -45.00 -60.00   66
 14  \w     39.00 131.00   0.50    1.00    --  107.00 -77.00 -60.00  184
 15  \w     36.00  79.00   0.50    1.00    --  107.00 -45.00 120.00   86
 16  \w     68.00  97.00   0.50    1.00    --  107.00 -94.00 150.00   58
 17  \w     82.00 116.00   0.50    1.00    --  107.00-125.00 120.00   68
 18  \w     53.00  78.00   0.50    1.00    --  107.00-125.00 120.00   50
 19  \w     35.00 116.00   0.50    1.00    --  107.00-125.00  60.00  162
 20  \w     35.00  71.00   0.50    1.00    --  107.00 -30.00 150.00   72
 21  \w     38.00  68.00   0.50    1.00    --  107.00 -45.00  90.00   60
 22  \w    -23.00  21.00   0.50    0.40    --   46.62 -86.00 -76.00   88
 23  \w    -22.00  62.00   0.50    0.40    --   46.62 -37.00-180.00  168
 24  \w     34.00 125.00   0.50    1.00    --  107.00 -15.00-120.00  182
 25  \w    152.00 178.00   0.50    1.00    --  107.00  86.00  42.00   52
 26  \w     82.00 142.00   0.50    1.00    --  107.00  86.00  42.00  120
 27  \w     36.00  69.00   0.50    1.00    --  107.00 -30.00-150.00   66
 28  \w     32.00  69.00   0.50    1.00    --  107.00 -30.00-120.00   74
 29  \w     37.00  66.00   0.50    1.00    --  107.00 -30.00 -90.00   58
 30  \w     35.00 109.00   0.50    1.00    --  107.00 -94.00-120.00  148
 31  \w    -79.00 -54.00   0.50    1.00    -- -102.00  86.00  42.00   50
 32  \w    -87.00 -30.00   0.50    1.00    -- -102.00 125.00  60.00  114
 33  \w    -57.00 -32.00   0.50    1.00    -- -102.00  30.00 150.00   50
 34  \w    -63.00 -29.00   0.50    1.00    -- -102.00  30.00  90.00   68
 35  \w   -116.00 -89.00   0.50    1.00    -- -102.00 125.00  60.00   54
 36  \w   -145.00-118.00   0.50    1.00    -- -102.00 -77.00-120.00   54
 37  \w   -105.00 -78.00   0.50    1.00    -- -102.00 -77.00-120.00   54
 38  \w   -119.00 -72.00   0.50    0.40    --  -46.62-125.00 -30.00   94
 39  \w   -116.00 -71.00   0.50    0.40    --  -46.62-125.00  30.00   90
 40  \w   -111.00 -84.00   0.50    0.40    --  -46.62-125.00  60.00   54
 41  \w   -117.00 -90.00   0.50    0.40    --  -46.62-125.00 150.00   54
 42  \w   -112.00 -85.00   0.50    1.00    -- -102.00 -94.00  30.00   54
 43  \w   -165.00-140.00   0.50    1.00    -- -102.00 -94.00  30.00   50
 44  \w   -165.00 -88.00   0.50    1.00    -- -102.00 -86.00 -76.00  154
;
_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      0.0298930000
_diffrn_orient_matrix_UB_12      0.0462083000
_diffrn_orient_matrix_UB_13      -0.0597916000
_diffrn_orient_matrix_UB_21      -0.0546002000
_diffrn_orient_matrix_UB_22      0.0922580000
_diffrn_orient_matrix_UB_23      0.0185951000
_diffrn_orient_matrix_UB_31      0.1382528000
_diffrn_orient_matrix_UB_32      0.0927765000
_diffrn_orient_matrix_UB_33      0.0320042000
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36815
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.356
_diffrn_reflns_theta_min         4.094
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61493
_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    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1218
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.425
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0484P)^2^+3.3636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10851
_reflns_number_total             11409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00766e2.cif
_cod_data_source_block           yrc112709_cecl3(dppb)2_sq
_cod_original_cell_volume        2808.70(6)
_cod_database_code               7710718
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C32 H32 O32 P32 Cl32 Ce32 '
_shelx_estimated_absorpt_t_max   0.466
_shelx_estimated_absorpt_t_min   0.345
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a 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              70838
_shelx_fab_checksum              3414
_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 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.685