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_7230553
_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
'C30 H34 Dy F12 N10 O8, C20 H4 Dy F24 O8, C H Cl3'
_chemical_formula_sum            'C51 H39 Cl3 Dy2 F36 N10 O16'
_chemical_formula_weight         2163.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1zgcrk
_audit_creation_date             2016-07-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.183(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4350(4)
_cell_length_b                   21.3325(7)
_cell_length_c                   23.0646(5)
_cell_measurement_reflns_used    10569
_cell_measurement_temperature    156.9(7)
_cell_measurement_theta_max      73.7690
_cell_measurement_theta_min      3.9550
_cell_volume                     8511.1(4)
_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_temperature      156.9(7)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.261
_diffrn_reflns_theta_min         3.649
_exptl_absorpt_coefficient_mu    11.432
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         16830
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0739
_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^)+(0.1159P)^2^+14.0975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13016
_reflns_number_total             16830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra02546k2.cif
_cod_data_source_block           a160629f_sqd
_cod_original_cell_volume        8511.2(4)
_cod_database_code               7230553
_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
 F10-C30 = F10'-C30 = F11-C30 = F11'-C30 = F12-C30 = F12'-C30
 1.33 with sigma of 0.01
 F5-C25 = F5'-C25 = F4-C25 = F4'-C25 = F6-C25 = F6'-C25
 1.33 with sigma of 0.01
 F10'-F11' \\sim F11'-F12'
 with sigma of 0.001
 F11'-F12' \\sim F12'-F10'
 with sigma of 0.001
 F11-F12 \\sim F12-F10
 with sigma of 0.001
 F12-F10 \\sim F10-F11
 with sigma of 0.001
 F4'-F6' \\sim F6'-F5'
 with sigma of 0.001
 F6'-F5' \\sim F5'-F4'
 with sigma of 0.001
 F6-F5 \\sim F5-F4
 with sigma of 0.001
 F5-F4 \\sim F4-F6
 with sigma of 0.001
3. Rigid bond restraints
 F2, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F34, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F35, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(F28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F4') \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F5)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6') \\sim Ueq, Uanis(F11') \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F10') \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12')
\\sim Ueq, Uanis(F12) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(F3) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F32)
\\sim Ueq, Uanis(F35) \\sim Ueq, Uanis(F27) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.002
Uanis(F16) \\sim Ueq, Uanis(F30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F6') = Uanis(F6)
Uanis(F5') = Uanis(F5)
Uanis(F4) = Uanis(F4')
5. Others
 Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C51(H51)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C23(H23), C28(H28), C33(H33), C38(H38), C43(H43), C48(H48)
6.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), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20