Tuning the magnetization dynamics of Tb<sup>III</sup>-based single-chain magnets through substitution on the nitronyl nitroxide radical.
Liu, Xiaoqing; Wang, Yu-Xia; Han, Zongsu; Han, Tian; Shi, Wei; Cheng, Peng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8989–8994; doi:10.1039/c9dt01704f

data_7700008
_publ_section_title
;
 Tuning the magnetization dynamics of Tb<sup>III</sup>-based single-chain
 magnets through substitution on the nitronyl nitroxide radical.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8989
_journal_page_last               8994
_journal_paper_doi               10.1039/c9dt01704f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '0.5(C64 H44 F36 N4 O16 S2 Tb2)'
_chemical_formula_sum            'C32 H22 F18 N2 O8 S Tb'
_chemical_formula_weight         1095.49
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-10
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.8845(9)
_cell_length_b                   17.2985(7)
_cell_length_c                   29.7057(11)
_cell_measurement_reflns_used    6834
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      29.2117
_cell_measurement_theta_min      2.9168
_cell_volume                     8257.6(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   39.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  178.0000   90.0000 54

  2 omega  -95.00  -36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6622 -178.0000  150.0000 59

  3 omega  -95.00  -39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6622 -178.0000  -30.0000 56

  4 omega   17.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6622   37.0000  120.0000 32

  5 omega  -56.00    3.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6622  -57.0000  120.0000 59
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0098778000
_diffrn_orient_matrix_UB_12      -0.0362159000
_diffrn_orient_matrix_UB_13      0.0106499000
_diffrn_orient_matrix_UB_21      0.0304382000
_diffrn_orient_matrix_UB_22      -0.0044729000
_diffrn_orient_matrix_UB_23      0.0157392000
_diffrn_orient_matrix_UB_31      -0.0116610000
_diffrn_orient_matrix_UB_32      0.0186716000
_diffrn_orient_matrix_UB_33      0.0245683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            36659
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       plate
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1185
_refine_ls_number_reflns         14526
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11283
_reflns_number_total             14526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01704f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7700008--7700009.cif.'
_cod_database_code               7700008
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C1H1N1O1TB1
_chemical_oxdiff_usercomment     TBL11A
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.703
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-F30A
 1.31 with sigma of 0.02
 C59-F28B
 1.31 with sigma of 0.02
 C59-F29B
 1.31 with sigma of 0.02
 F30A-F29B
 2.2 with sigma of 0.02
 F29B-F28B
 2.2 with sigma of 0.02
 F28B-F30A
 2.2 with sigma of 0.02
 C59-F30B
 1.31 with sigma of 0.02
 C59-F28A
 1.31 with sigma of 0.02
 C59-F29A
 1.31 with sigma of 0.02
 F30B-F29A
 2.2 with sigma of 0.02
 F29A-F28A
 2.2 with sigma of 0.02
 F28A-F30B
 2.2 with sigma of 0.02
 C58-F27A
 1.31 with sigma of 0.02
 C58-F26B
 1.31 with sigma of 0.02
 C58-F25A
 1.31 with sigma of 0.02
 F25A-F26B
 2.2 with sigma of 0.02
 F26B-F27A
 2.2 with sigma of 0.02
 F27A-F25A
 2.2 with sigma of 0.02
 C63-F32B
 1.32 with sigma of 0.02
 C63-F33A
 1.32 with sigma of 0.02
 C63-F31B
 1.32 with sigma of 0.02
 F32B-F33A
 2.13 with sigma of 0.02
 F33A-F31B
 2.13 with sigma of 0.02
 F31B-F32B
 2.13 with sigma of 0.02
 C63-F32A
 1.32 with sigma of 0.02
 C63-F33B
 1.32 with sigma of 0.02
 C63-F31A
 1.32 with sigma of 0.02
 F32A-F33B
 2.13 with sigma of 0.02
 F33B-F31A
 2.13 with sigma of 0.02
 F31A-F32A
 2.13 with sigma of 0.02
 C58-F27B
 1.31 with sigma of 0.02
 C58-F26A
 1.31 with sigma of 0.02
 C58-F25B
 1.31 with sigma of 0.02
 F25B-F26A
 2.2 with sigma of 0.02
 F26A-F27B
 2.2 with sigma of 0.02
 F27B-F25B
 2.2 with sigma of 0.02
3. Rigid bond restraints
 F31B, F32B, F33A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F32A, F33B, F31A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F32B \\sim F33A \\sim F31B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F32A \\sim F33B \\sim F31A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(F28A) \\sim Ueq, Uanis(F28B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F32B) \\sim Ueq, Uanis(F33A) \\sim Ueq, Uanis(F31B) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F32A) \\sim Ueq, Uanis(F33B) \\sim Ueq, Uanis(F31A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F27B) \\sim Ueq, Uanis(F25B) \\sim Ueq, Uanis(F26A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F27A) \\sim Ueq, Uanis(F26B) \\sim Ueq, Uanis(F25A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F31B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F30B) = Uanis(F29A) = Uanis(F28A)
Uanis(F28B) = Uanis(F29B) = Uanis(F30A)
5. Others
 Sof(F28B)=Sof(F29B)=Sof(F30A)=1-FVAR(1)
 Sof(F28A)=Sof(F29A)=Sof(F30B)=FVAR(1)
 Sof(F25B)=Sof(F26A)=Sof(F27B)=1-FVAR(2)
 Sof(F25A)=Sof(F26B)=Sof(F27A)=FVAR(2)
 Sof(F31B)=Sof(F32B)=Sof(F33A)=1-FVAR(3)
 Sof(F31A)=Sof(F32A)=Sof(F33B)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C19(H19),
 C24(H24), C29(H29), C35(H35), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
  C43(H43), C51(H51), C56(H56), C61(H61)
6.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,
 H17c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C49(H49a,
 H49b,H49c)
;
_shelx_res_checksum              42718
_shelx_fab_checksum              38733
_olex2_submission_special_instructions 'No special instructions were received'