A family of multi-spin rare-earth complexes based on a triazole nitronyl nitroxide radical: synthesis, structure and magnetic properties
Chen, Peng Yun; Wu, Ming Ze; Shi, Xiu Juan; Tian, Li; RSC Advances 8 (2018) 15480–; doi:10.1039/C8RA02546K

data_7230554
_publ_section_title
;
 A family of multi-spin rare-earth complexes based on a triazole nitronyl
 nitroxide radical: synthesis, structure and magnetic properties
;
_journal_issue                   28
_journal_name_full               'RSC Advances'
_journal_page_first              15480
_journal_paper_doi               10.1039/C8RA02546K
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C25 H21 F18 N5 O9 Tb'
_chemical_formula_sum            'C25 H21 F18 N5 O9 Tb'
_chemical_formula_weight         1036.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1zgcqj
_audit_creation_date             2016-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                105.052(3)
_cell_angle_beta                 103.900(3)
_cell_angle_gamma                99.476(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9958(3)
_cell_length_b                   12.3076(4)
_cell_length_c                   16.1878(6)
_cell_measurement_reflns_used    7346
_cell_measurement_temperature    113.01(10)
_cell_measurement_theta_max      73.6970
_cell_measurement_theta_min      3.8270
_cell_volume                     1811.28(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      113.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -68.00  31.00   1.00    1.00    --  -41.49  51.00 -11.00   99
  2  \w    -70.00  32.00   1.00    1.00    --  -41.49  57.00  90.00  102
  3  \w    -70.00  32.00   1.00    1.00    --  -41.49  57.00 120.00  102
  4  \w   -116.00 -17.00   1.00    1.00    --  -41.49 -38.00-180.00   99
  5  \w     23.00  98.00   1.00    1.00    --   41.49-125.00-180.00   75
  6  \w     31.00 135.00   1.00    1.00    --  107.08 -30.00 -90.00  104
  7  \w     94.00 133.00   1.00    1.00    --  107.08 -45.00-180.00   39
  8  \w     42.00 117.00   1.00    1.00    --  107.08 -30.00  90.00   75
  9  \w     36.00  81.00   1.00    1.00    --  107.08 -45.00-180.00   45
 10  \w     43.00 121.00   1.00    1.00    --  107.08-125.00  90.00   78
 11  \w     98.00 178.00   1.00    1.00    --  107.08  45.00 -90.00   80
 12  \w     34.00  83.00   1.00    1.00    --  107.08 -95.00 150.00   49
 13  \w     35.00 142.00   1.00    1.00    --  107.08 -15.00 -90.00  107
 14  \w     55.00 119.00   1.00    1.00    --  107.08-125.00-120.00   64
 15  \w     56.00 140.00   1.00    1.00    --  107.08 -77.00-120.00   84
 16  \w    104.00 175.00   1.00    1.00    --  107.08 125.00-150.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0191863000
_diffrn_orient_matrix_UB_12      -0.1232065000
_diffrn_orient_matrix_UB_13      -0.0060610000
_diffrn_orient_matrix_UB_21      0.1520187000
_diffrn_orient_matrix_UB_22      0.0515563000
_diffrn_orient_matrix_UB_23      0.0642222000
_diffrn_orient_matrix_UB_31      -0.0574546000
_diffrn_orient_matrix_UB_32      0.0031213000
_diffrn_orient_matrix_UB_33      0.0805664000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13161
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.833
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.900
_exptl_crystal_description       block
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6434
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0701P)^2^+1.9294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5851
_reflns_number_total             6434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra02546k2.cif
_cod_data_source_block           a160122a
_cod_original_cell_volume        1811.27(12)
_cod_database_code               7230554
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 F9-C16 = F8-C16 = F7-C16
 1.34 with sigma of 0.001
 F9'-C16 = F7'-C16 = F8'-C16
 1.34 with sigma of 0.001
 C11'-C12 = C11-C12
 1.52 with sigma of 0.01
 F3'-C11' = F3-C11 = F1-C11 = F1'-C11' = F2-C11 = F2'-C11'
 1.34 with sigma of 0.001
 F9-F7 \\sim F7-F8
 with sigma of 0.001
 F7-F8 \\sim F8-F9
 with sigma of 0.001
 F9'-F7' \\sim F7'-F8'
 with sigma of 0.001
 F7'-F8' \\sim F8'-F9'
 with sigma of 0.001
 F3'-F1' \\sim F1'-F2'
 with sigma of 0.001
 F1'-F2' \\sim F2'-F3'
 with sigma of 0.001
 F3-F1 \\sim F1-F2
 with sigma of 0.001
 F1-F2 \\sim F2-F3
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F8) \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7')
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F15) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F16) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(F9') = Uanis(F9)
Uanis(F7') = Uanis(F7)
Uanis(F8') = Uanis(F8)
Uanis(F3') = Uanis(F3)
Uanis(F1) = Uanis(F1')
Uanis(F2) = Uanis(F2')
Uanis(C11) = Uanis(C11')
4. Others
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C11')=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C11)=FVAR(2)
5.a Rotating group:
 O9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C18(H18), C23(H23)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-22
_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 11.542
_oxdiff_exptl_absorpt_empirical_full_min 0.672