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_7710717
_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 Cl3 O4 P4 Sm'
_chemical_formula_sum            'C60 H48 Cl3 O4 P4 Sm'
_chemical_formula_weight         1213.56
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-02 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                98.8240(10)
_cell_angle_beta                 93.9410(10)
_cell_angle_gamma                114.9520(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3010(2)
_cell_length_b                   12.4404(2)
_cell_length_c                   22.2903(2)
_cell_measurement_reflns_used    26947
_cell_measurement_temperature    100(8)
_cell_measurement_theta_max      76.4680
_cell_measurement_theta_min      3.9780
_cell_volume                     2776.32(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_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    -28.00  23.00   0.50    0.08    --   46.62 -10.00  57.00  102
  2  \w     35.00  69.00   0.50    0.40    --  106.69 -61.00  30.00   68
  3  \w     41.00 108.00   0.50    0.40    --  106.69 -94.00  90.00  134
  4  \w     77.00 115.00   0.50    0.40    --  106.69-125.00  90.00   76
  5  \w     54.00 116.00   0.50    0.40    --  106.69-125.00  30.00  124
  6  \w     79.00 105.00   0.50    0.40    --  106.69-125.00 -60.00   52
  7  \w     86.00 113.00   0.50    0.40    --  106.69-125.00-150.00   54
  8  \w     38.00  94.00   0.50    0.08    --   46.62-125.00   0.00  112
  9  \w     35.00  73.00   0.50    0.40    --  106.69 -61.00   0.00   76
 10  \w     34.00 108.00   0.50    0.40    --  106.69 -77.00 -60.00  148
 11  \w     79.00 108.00   0.50    0.08    --   46.62  10.00-129.00   58
 12  \w    105.00 176.00   0.50    0.40    --  106.69  10.00-129.00  142
 13  \w    144.00 177.00   0.50    0.40    --  106.69  61.00 -90.00   66
 14  \w    130.00 156.00   0.50    0.40    --  106.69  45.00 -30.00   52
 15  \w    103.00 149.00   0.50    0.40    --  106.69  45.00 -90.00   92
 16  \w     97.00 177.00   0.50    0.40    --  106.69  45.00 -60.00  160
 17  \w     91.00 175.00   0.50    0.40    --  106.69 125.00 -60.00  168
 18  \w     91.00 141.00   0.50    0.40    --  106.69  61.00 -90.00  100
 19  \w     91.00 174.00   0.50    0.40    --  106.69  30.00   0.00  166
 20  \w     35.00  80.00   0.50    0.40    --  106.69-125.00-150.00   90
 21  \w     39.00 105.00   0.50    0.40    --  106.69 -77.00-150.00  132
 22  \w     36.00  71.00   0.50    0.40    --  106.69 -61.00-150.00   70
 23  \w     34.00  59.00   0.50    0.40    --  106.69 -61.00-180.00   50
 24  \w     24.00  74.00   0.50    0.08    --   46.62  10.00-129.00  100
 25  \w     39.00  83.00   0.50    0.40    --  106.69 -77.00   0.00   88
 26  \w     37.00  63.00   0.50    0.40    --  106.69 -61.00 120.00   52
 27  \w      5.00  78.00   0.50    0.08    --   46.62 -99.00-120.00  146
 28  \w    -22.00  28.00   0.50    0.08    --  -46.62  10.00-129.00  100
 29  \w    -24.00   7.00   0.50    0.08    --  -46.62  19.00 -90.00   62
 30  \w    -40.00 -13.00   0.50    0.08    --  -46.62  37.00 -60.00   54
 31  \w    -58.00 -29.00   0.50    0.40    -- -102.00 125.00  60.00   58
 32  \w    -63.00 -29.00   0.50    0.40    -- -102.00  61.00 150.00   68
 33  \w    -68.00 -43.00   0.50    0.40    -- -102.00  61.00  60.00   50
 34  \w    -99.00 -62.00   0.50    0.40    -- -102.00  77.00 150.00   74
 35  \w   -117.00 -92.00   0.50    0.40    -- -102.00 125.00  60.00   50
 36  \w    -93.00 -67.00   0.50    0.40    -- -102.00  77.00 -90.00   52
 37  \w    -57.00 -32.00   0.50    0.40    -- -102.00 125.00 -90.00   50
 38  \w   -114.00 -62.00   0.50    0.40    -- -102.00 125.00 -90.00  104
 39  \w   -122.00 -25.00   0.50    0.08    --  -46.62 -10.00  57.00  194
 40  \w   -110.00 -71.00   0.50    0.08    --  -46.62-125.00  60.00   78
 41  \w   -171.00 -83.00   0.50    0.40    -- -102.00 -10.00  57.00  176
;
_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      -0.1304742000
_diffrn_orient_matrix_UB_12      0.0113896000
_diffrn_orient_matrix_UB_13      -0.0078747000
_diffrn_orient_matrix_UB_21      0.0780613000
_diffrn_orient_matrix_UB_22      0.1378429000
_diffrn_orient_matrix_UB_23      0.0060586000
_diffrn_orient_matrix_UB_31      -0.0014460000
_diffrn_orient_matrix_UB_32      -0.0177541000
_diffrn_orient_matrix_UB_33      -0.0700286000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_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       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36235
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.820
_diffrn_reflns_theta_min         4.059
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (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    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0401P)^2^+2.1812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10909
_reflns_number_total             11244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00766e2.cif
_cod_data_source_block           yrc022501_smcl3(dppbo)_sq
_cod_original_cell_volume        2776.32(7)
_cod_database_code               7710717
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Sm C H O Cl P'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C59(H59), C58(H58), C39(H39), C33(H33), C24(H24), C56(H56),
 C47(H47), C41(H41), C57(H57), C44(H44), C36(H36), C10(H10), C38(H38), C46(H46),
  C60(H60), C50(H50), C29(H29), C28(H28), C20(H20), C51(H51), C40(H40),
 C30(H30), C32(H32), C11(H11), C35(H35), C26(H26), C54(H54), C8(H8), C34(H34),
 C9(H9), C45(H45), C52(H52), C17(H17), C12(H12), C14(H14), C22(H22), C53(H53),
 C15(H15), C27(H27), C16(H16), C21(H21), C23(H23), C2(H2), C6(H6), C4(H4),
 C5(H5), C3(H3)
;
_shelx_res_checksum              26914
_shelx_fab_checksum              66339
_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 1.683
_oxdiff_exptl_absorpt_empirical_full_min 0.713