Modulating spin dynamics of binuclear LnIII‒radical complexes by using different indazole radicals
Chen, Peng Yun; Shi, Xiu Juan; Li, Ting; Tian, Li; Liu, Zhong Yi; Hua, Feng Zhen; Yu, Si Jia; Xu, Yuan Yuan; RSC Adv. 7 (2017) 45504–; doi:10.1039/C7RA09192C

data_7229243
_publ_section_title
;
 Modulating spin dynamics of binuclear LnIII--radical complexes by using
 different indazole radicals
;
_journal_issue                   72
_journal_name_full               'RSC Adv.'
_journal_page_first              45504
_journal_paper_doi               10.1039/C7RA09192C
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C58 H40 F36 Gd2 N8 O16'
_chemical_formula_sum            'C58 H40 F36 Gd2 N8 O16'
_chemical_formula_weight         2103.48
_chemical_name_systematic
;
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1p61pm
_audit_creation_date             2016-09-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.689(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9977(10)
_cell_length_b                   25.907(2)
_cell_length_c                   15.0221(10)
_cell_measurement_reflns_used    4344
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.36
_cell_measurement_theta_min      2.26
_cell_volume                     3744.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.572
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.8234.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.282
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7759
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+19.9325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5567
_reflns_number_total             7759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09192c2.cif
_cod_data_source_block           n151228b
_cod_database_code               7229243
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-F18' = C29-F16' = C29-F17'
 1.28 with sigma of 0.01
 F18'-F16' = F18'-F17' = F16'-F17'
 2.04 with sigma of 0.01
 C29-F18 = C29-F16 = C29-F17
 1.28 with sigma of 0.01
 F18-F16 = F18-F17 = F16-F17
 2.04 with sigma of 0.01
 C19-C18 = C19'-C18
 1.48 with sigma of 0.01
 C19'-F10' = C19'-F11' = C19'-F12'
 1.28 with sigma of 0.01
 F10'-F11' = F10'-F12' = F11'-F12'
 2.04 with sigma of 0.01
 C19-F10 = C19-F11 = C19-F12
 1.28 with sigma of 0.01
 F10-F11 = F10-F12 = F11-F12
 2.04 with sigma of 0.01
 C15-C16 = C15'-C16
 1.48 with sigma of 0.01
 C15'-F7' = C15'-F8' = C15'-F9'
 1.28 with sigma of 0.01
 F7'-F8' = F7'-F9' = F8'-F9'
 2.04 with sigma of 0.01
 C15-F7 = C15-F8 = C15-F9
 1.28 with sigma of 0.01
 F7-F8 = F7-F9 = F8-F9
 2.04 with sigma of 0.01
 C20-C21 = C20'-C21
 1.48 with sigma of 0.01
 C20'-F1' = C20'-F2' = C20'-F3'
 1.28 with sigma of 0.01
 F1'-F2' = F1'-F3' = F2'-F3'
 2.04 with sigma of 0.01
 C20-F1 = C20-F2 = C20-F3
 1.28 with sigma of 0.01
 F1-F2 = F1-F3 = F2-F3
 2.04 with sigma of 0.01
3. Rigid bond restraints
 F4, C24
 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(C18) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15') \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C19') \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F17')
\\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F16') \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F18') \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F7') \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F9') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(F18) = Uanis(F18')
Uanis(F17) = Uanis(F17')
Uanis(F16) = Uanis(F16')
Uanis(F12) = Uanis(F12')
Uanis(F11) = Uanis(F11')
Uanis(F10) = Uanis(F10')
Uanis(F9) = Uanis(F9')
Uanis(F8) = Uanis(F8')
Uanis(F7) = Uanis(F7')
Uanis(F3) = Uanis(F3')
Uanis(F2) = Uanis(F2')
Uanis(F1) = Uanis(F1')
Uanis(C19) = Uanis(C19')
Uanis(C15) = Uanis(C15')
Uanis(C20) = Uanis(C20')
5. Others
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C20')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C20)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=Sof(C15')=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C15)=FVAR(2)
 Sof(F10')=Sof(F11')=Sof(F12')=Sof(C19')=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C19)=FVAR(3)
 Sof(F16')=Sof(F17')=Sof(F18')=1-FVAR(4)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(4)
6.a Riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C12(H12), C13(H13), C14(H14), C17(H17), C22(H22), C27(H27)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'