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_7700009
_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         'C64 H44 F36 N4 O16 S2 Tb2'
_chemical_formula_sum            'C64 H44 F36 N4 O16 S2 Tb2'
_chemical_formula_weight         2190.99
_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)
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_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.913(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1897(5)
_cell_length_b                   20.9619(7)
_cell_length_c                   23.0457(8)
_cell_measurement_reflns_used    12362
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      29.2117
_cell_measurement_theta_min      2.4744
_cell_volume                     8225.0(5)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -1.00   57.40   0.8000   98.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   37.0000   30.0000 73

  2 omega   27.00   74.20   0.8000   98.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000   30.0000 59

  3 omega  -75.00  -43.80   0.8000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  123.0000  -91.0000 39

  4 omega  -80.00    5.60   0.8000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  -37.0000  150.0000 107
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0017501000
_diffrn_orient_matrix_UB_12      -0.0247026000
_diffrn_orient_matrix_UB_13      0.0207592000
_diffrn_orient_matrix_UB_21      0.0041826000
_diffrn_orient_matrix_UB_22      0.0228788000
_diffrn_orient_matrix_UB_23      0.0229344000
_diffrn_orient_matrix_UB_31      -0.0414358000
_diffrn_orient_matrix_UB_32      0.0032486000
_diffrn_orient_matrix_UB_33      -0.0028516000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.769
_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         0.587
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1293
_refine_ls_number_reflns         14485
_refine_ls_number_restraints     504
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+2.6543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11500
_reflns_number_total             14485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01704f2.cif
_cod_data_source_block           p101229e
_cod_depositor_comments
'Adding full bibliography for 7700008--7700009.cif.'
_cod_database_code               7700009
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12TB1
_chemical_oxdiff_usercomment     TBL3
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.702
_reflns_odcompleteness_completeness 99.87
_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
 F7-F8 = F8-F9 = F7-F9 = F7'-F8' = F8'-F9' = F7'-F9'
 2.12 with sigma of 0.02
 C38-F7 = C38-F7' = C38-F8 = C38-F8' = C38-F9 = C38-F9'
 1.38 with sigma of 0.01
 F10-F11 = F11-F12 = F10-F12 = F10'-F11' = F11'-F12' = F10'-F12'
 2.12 with sigma of 0.02
 C39-F10 = C39-F10' = C39-F11 = C39-F11' = C39-F12 = C39-F12'
 1.38 with sigma of 0.01
 F13-F14 = F14-F15 = F13-F15 = F13'-F14' = F14'-F15' = F13'-F15'
 2.12 with sigma of 0.02
 C49-F13 = C49-F14 = C49-F15 = C49-F13' = C49-F14' = C49-F15'
 1.38 with sigma of 0.01
 F16-F17 = F17-F18 = F16-F18 = F16'-F17' = F17'-F18' = F16'-F18'
 2.12 with sigma of 0.02
 C48-F16 = C48-F17 = C48-F18 = C48-F16' = C48-F17' = C48-F18'
 1.38 with sigma of 0.01
 F25-F26 = F26-F27 = F25-F27 = F25'-F26' = F26'-F27' = F25'-F27'
 2.12 with sigma of 0.02
 C54-F25 = C54-F26 = C54-F27 = C54-F25' = C54-F26' = C54-F27'
 1.38 with sigma of 0.01
 F28-F29 = F29-F30 = F28-F30 = F28'-F29' = F29'-F30' = F28'-F30'
 2.12 with sigma of 0.02
 C53-F28 = C53-F29 = C53-F30 = C53-F28' = C53-F29' = C53-F30'
 1.38 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7' \\sim F8' \\sim F9': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F10 \\sim F11 \\sim F12 \\sim F10' \\sim F11' \\sim F12': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F13 \\sim F14 \\sim F15 \\sim F13' \\sim F14' \\sim F15': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F16 \\sim F17 \\sim F18 \\sim F16' \\sim F17' \\sim F18': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F25 \\sim F26 \\sim F27 \\sim F25' \\sim F26' \\sim F27': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F28 \\sim F29 \\sim F30 \\sim F28' \\sim F29' \\sim F30': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F25)
\\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F29) \\sim Ueq,
Uanis(F28) \\sim Ueq, Uanis(F30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim
Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq,
Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F16') \\sim Ueq, Uanis(F17') \\sim Ueq, Uanis(F18') \\sim Ueq,
Uanis(F25') \\sim Ueq, Uanis(F26') \\sim Ueq, Uanis(F27') \\sim Ueq,
Uanis(F29') \\sim Ueq, Uanis(F28') \\sim Ueq, Uanis(F30') \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F7') \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F10')
\\sim Ueq, Uanis(F11') \\sim Ueq, Uanis(F12') \\sim Ueq, Uanis(F13') \\sim Ueq,
Uanis(F14') \\sim Ueq, Uanis(F15') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(F13')=Sof(F14')=Sof(F15')=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(F16')=Sof(F17')=Sof(F18')=1-FVAR(4)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(4)
 Sof(F25')=Sof(F26')=Sof(F27')=1-FVAR(5)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(5)
 Sof(F28')=Sof(F29')=Sof(F30')=1-FVAR(6)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(6)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C20(H20),
 C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C36(H36), C41(H41),
  C46(H46), C51(H51), C56(H56), C61(H61)
5.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C17(H17a,H17b,
 H17c), C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C34(H34a,
 H34b,H34c)
;
_shelx_res_checksum              74792
_shelx_fab_checksum              67712
_olex2_submission_special_instructions 'No special instructions were received'