Slow relaxation of the magnetization observed in mononuclear Ln-radical compounds with D<sub>4d</sub> geometry configurations.
Chen, Peng Yun; Wu, Ming Ze; Liu, Zhong Yi; Tian, Li; Zhang, Yi Quan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 558–565; doi:10.1039/c8dt03809k

data_7048260
_publ_section_title
;
 Slow relaxation of the magnetization observed in mononuclear Ln-radical
 compounds with D<sub>4d</sub> geometry configurations.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              558
_journal_page_last               565
_journal_paper_doi               10.1039/c8dt03809k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C25 H18 F18 N4 O8 Tb)'
_chemical_formula_sum            'C50 H36 F36 N8 O16 Tb2'
_chemical_formula_weight         2006.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2051js
_audit_creation_date             2018-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-22 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.609(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4759(11)
_cell_length_b                   17.6489(7)
_cell_length_c                   18.5888(9)
_cell_measurement_reflns_used    5392
_cell_measurement_temperature    135.00(10)
_cell_measurement_theta_max      73.4240
_cell_measurement_theta_min      3.4860
_cell_volume                     6988.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      135.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -114.00 -23.00   1.00    5.05    --  -41.11 -38.00-150.00   91
  2  \w    -95.00 -50.00   1.00    5.05    --  -41.11 125.00  60.00   45
  3  \w    -68.00  32.00   1.00    5.05    --  -41.11  57.00   0.00  100
  4  \w     81.00 111.00   1.00   25.20    --  107.08  45.00 120.00   30
  5  \w     82.00 127.00   1.00   25.20    --  107.08  30.00-150.00   45
  6  \w     30.00  77.00   1.00   25.20    --  107.08 -95.00-150.00   47
  7  \w     83.00 171.00   1.00   25.20    --  107.08  32.00  85.00   88
  8  \w     86.00 174.00   1.00   25.20    --  107.08  30.00  30.00   88
  9  \w    125.00 178.00   1.00   25.20    --  107.08  45.00 120.00   53
 10  \w     26.00  97.00   1.00   25.20    --  107.08 -95.00-120.00   71
 11  \w     35.00  84.00   1.00   25.20    --  107.08 -77.00 -90.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0544009000
_diffrn_orient_matrix_UB_12      0.0367100000
_diffrn_orient_matrix_UB_13      0.0627724000
_diffrn_orient_matrix_UB_21      -0.0413908000
_diffrn_orient_matrix_UB_22      0.0035202000
_diffrn_orient_matrix_UB_23      0.0521026000
_diffrn_orient_matrix_UB_31      0.0235244000
_diffrn_orient_matrix_UB_32      -0.0791144000
_diffrn_orient_matrix_UB_33      0.0315334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25840
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       block
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.923
_refine_diff_density_min         -3.770
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         12378
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.1074
_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^)+(0.1726P)^2^+72.9543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2835
_refine_ls_wR_factor_ref         0.3215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7941
_reflns_number_total             12378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03809k2.cif
_cod_data_source_block           a171113d
_cod_depositor_comments
'Adding full bibliography for 7048260--7048262.cif.'
_cod_database_code               7048260
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F22-C40 = F22'-C40 = F24-C40 = F24'-C40 = F23-C40 = F23'-C40
 1.35 with sigma of 0.01
 F22-F24 \\sim F24-F23
 with sigma of 0.005
 F23-F22 \\sim F22-F24
 with sigma of 0.005
 F22'-F24' \\sim F24'-F23'
 with sigma of 0.005
 F23'-F22' \\sim F22'-F24'
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(F23') \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22')
\\sim Ueq, Uanis(F24') \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F18) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F3)
\\sim Ueq, Uanis(F26) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(F10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(F22) = Uanis(F22')
Uanis(F23') = Uanis(F23)
Uanis(F24') = Uanis(F24)
4. Others
 Sof(F22')=Sof(F23')=Sof(F24')=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N8(H8), N4(H4), C43(H43), C13(H13), C34(H34), C48(H48), C18(H18), C23(H23),
 C9(H9), C38(H38), C10(H10), C35(H35)
5.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C7(H7A,H7B,H7C), C5(H5A,H5B,H5C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C4(H4A,H4B,H4C), C32(H32A,H32B,H32C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              56705
_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 6.249
_oxdiff_exptl_absorpt_empirical_full_min 0.357