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_7230552
_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 Gd N5 O9'
_chemical_formula_sum            'C25 H21 F18 Gd N5 O9'
_chemical_formula_weight         1034.72
_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.cc1zgcph
_audit_creation_date             2016-01-19
_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                105.182(3)
_cell_angle_beta                 103.964(3)
_cell_angle_gamma                99.368(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0094(3)
_cell_length_b                   12.3115(4)
_cell_length_c                   16.2016(5)
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    113.00(10)
_cell_measurement_theta_max      28.0470
_cell_measurement_theta_min      3.8470
_cell_volume                     1814.67(11)
_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      113.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -12.00  84.00   1.00    2.85    --   11.08  38.00-120.00   96
  2  \w    -10.00  30.00   1.00    2.85    --  -11.24-107.00 -14.00   40
  3  \w     36.00  72.00   1.00    2.85    --   11.08-178.00  90.00   36
  4  \w     41.00  98.00   1.00    2.85    --   11.08-178.00  30.00   57
  5  \w    -13.00  85.00   1.00    2.85    --   11.08  38.00 150.00   98
;
_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      0.0306699000
_diffrn_orient_matrix_UB_12      -0.0163483000
_diffrn_orient_matrix_UB_13      0.0377661000
_diffrn_orient_matrix_UB_21      -0.0301806000
_diffrn_orient_matrix_UB_22      0.0385486000
_diffrn_orient_matrix_UB_23      0.0264781000
_diffrn_orient_matrix_UB_31      -0.0617267000
_diffrn_orient_matrix_UB_32      -0.0450629000
_diffrn_orient_matrix_UB_33      -0.0114562000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13737
_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         3.364
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75993
_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    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.836
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6381
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0314P)^2^+4.3088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5681
_reflns_number_total             6381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra02546k2.cif
_cod_data_source_block           a160119e
_cod_original_cell_volume        1814.66(10)
_cod_database_code               7230552
_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, All O(H,H) groups
2. Restrained distances
 F11-C20 = F3A-C20 = F12'-C20 = F10'-C20 = F10-C20 = F11'-C20
 1.34 with sigma of 0.01
 C15-C14 = C15'-C14
 1.56 with sigma of 0.01
 F4-C15 = F4'-C15' = F6'-C15' = F6-C15 = F5'-C15' = F5-C15
 1.34 with sigma of 0.01
 F4-F5 \\sim F5-F6
 with sigma of 0.001
 F5-F6 \\sim F6-F4
 with sigma of 0.001
 F4'-F5' \\sim F5'-F6'
 with sigma of 0.001
 F5'-F6' \\sim F6'-F4'
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F3A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11') \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F10') \\sim Ueq, Uanis(F12') \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(F11) = Uanis(F3A)
Uanis(F12') = Uanis(F10')
Uanis(F10) = Uanis(F11')
Uanis(F4) = Uanis(F4')
Uanis(F5) = Uanis(F5')
Uanis(F6) = Uanis(F6')
Uanis(C15) = Uanis(C15')
4. Others
 Sof(F3A)=Sof(F10')=Sof(F11')=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12')=FVAR(1)
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C15')=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C15)=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 2016-01-19
_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 1.374
_oxdiff_exptl_absorpt_empirical_full_min 0.699