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_7229245
_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 Dy2 F36 N8 O16'
_chemical_formula_sum            'C58 H40 Dy2 F36 N8 O16'
_chemical_formula_weight         2113.98
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1p6478
_audit_creation_date             2017-06-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-09 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8277(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9689(2)
_cell_length_b                   25.9221(5)
_cell_length_c                   12.3832(2)
_cell_measurement_reflns_used    5745
_cell_measurement_temperature    129(1)
_cell_measurement_theta_max      73.5400
_cell_measurement_theta_min      4.0280
_cell_volume                     3730.65(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      129(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -32.00  41.00   1.00    4.13    --   41.49 -38.00 -90.00   73
  2  \w     31.00  80.00   1.00    4.13    --   41.49 -99.00-150.00   49
  3  \w     26.00  68.00   1.00   16.54    --  107.08 -95.00 -60.00   42
  4  \w     50.00 108.00   1.00   16.54    --  107.08 -95.00   0.00   58
  5  \w     90.00 139.00   1.00   16.54    --  107.08 -77.00 120.00   49
  6  \w     88.00 147.00   1.00   16.54    --  107.08  30.00  60.00   59
  7  \w    111.00 177.00   1.00   16.54    --  107.08  45.00 150.00   66
  8  \w     47.00  73.00   1.00   16.54    --  107.08 -77.00 120.00   26
  9  \w     83.00 177.00   1.00   16.54    --  107.08  77.00-120.00   94
 10  \w     34.00  77.00   1.00   16.54    --  107.08 -95.00-180.00   43
 11  \w   -113.00  -1.00   1.00    4.13    --  -41.49 -19.00 120.00  112
;
_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      0.0570449000
_diffrn_orient_matrix_UB_12      0.0518115000
_diffrn_orient_matrix_UB_13      -0.0159340000
_diffrn_orient_matrix_UB_21      -0.1126924000
_diffrn_orient_matrix_UB_22      0.0180979000
_diffrn_orient_matrix_UB_23      -0.0795220000
_diffrn_orient_matrix_UB_31      -0.0402366000
_diffrn_orient_matrix_UB_32      0.0228578000
_diffrn_orient_matrix_UB_33      0.0991315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14100
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         4.053
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.937
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.118
_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     633
_refine_ls_number_reflns         6656
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+10.4805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5333
_reflns_number_total             6656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09192c2.cif
_cod_data_source_block           a170310b
_cod_database_code               7229245
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C27-C26 = C27-C28 = C22-C23 = C22-C21
 1.39 with sigma of 0.01
 C20'-C21 = C20-C21
 1.5 with sigma of 0.01
 F8'-C20' = F9'-C20' = F7'-C20'
 1.35 with sigma of 0.01
 C23-C24
 1.47 with sigma of 0.01
 C24'-C23 = C24-C23
 1.5 with sigma of 0.01
 F12'-C24' = F10'-C24' = F11'-C24'
 1.35 with sigma of 0.01
 C25-C26 = C25'-C26
 1.5 with sigma of 0.01
 F13'-C25' = F14'-C25' = F15'-C25'
 1.35 with sigma of 0.01
 C29-C28 = C29'-C28
 1.5 with sigma of 0.01
 F17'-C29' = F16'-C29' = F18'-C29'
 1.35 with sigma of 0.01
 C25-C26 = C29-C28 = C20-C21 = C19-C18 = C15-C16
 1.47 with sigma of 0.01
 F5-C19 = C19-F4 = C19-F6 = C15-F2 = C15-F1 = C15-F3 = C20-F8 = C20-F9 = F7-
 C20 = C24-F10 = C24-F12 = C24-F11 = C29-F16 = C29-F17 = C29-F18 = C25-F15 =
 F14-C25 = F13-C25
 1.35 with sigma of 0.01
 F4-F6 \\sim F6-F5
 with sigma of 0.001
 F5-F4 \\sim F4-F6
 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
 F9'-F7' \\sim F7'-F8'
 with sigma of 0.001
 F8'-F9' \\sim F9'-F7'
 with sigma of 0.001
 F10-F11 \\sim F11-F12
 with sigma of 0.001
 F12-F10 \\sim F10-F11
 with sigma of 0.001
 F12'-F10' \\sim F10'-F11'
 with sigma of 0.001
 F11'-F12' \\sim F12'-F10'
 with sigma of 0.001
 F15-F13 \\sim F13-F14
 with sigma of 0.001
 F14-F15 \\sim F15-F13
 with sigma of 0.001
 F13'-F14' \\sim F14'-F15'
 with sigma of 0.001
 F15'-F13' \\sim F13'-F14'
 with sigma of 0.001
 F14'-C26 \\sim C26-F13'
 with sigma of 0.001
 F13'-C26 \\sim C26-F15'
 with sigma of 0.001
 F15'-C26 \\sim C26-F14'
 with sigma of 0.001
 F16-F17 \\sim F17-F18
 with sigma of 0.001
 F18-F16 \\sim F16-F17
 with sigma of 0.001
 F18'-F16' \\sim F16'-F17'
 with sigma of 0.001
 F17'-F18' \\sim F18'-F16'
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C29) \\sim Ueq, Uanis(C29') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F6) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F14)
\\sim Ueq, Uanis(F14') \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(F8') \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F9') = Uanis(F9)
Uanis(F7) = Uanis(F7')
Uanis(C20') = Uanis(C20)
Uanis(F8) = Uanis(F8')
Uanis(C24) = Uanis(C24')
Uanis(F18) = Uanis(F18')
Uanis(F17') = Uanis(F17)
Uanis(F16') = Uanis(F16)
Uanis(C29') = Uanis(C29)
Uanis(C25') = Uanis(C25)
Uanis(C29) = Uanis(C29')
4. Others
 Sof(F10')=Sof(F11')=Sof(F12')=Sof(C24')=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C24)=FVAR(1)
 Sof(F16')=Sof(F17')=Sof(F18')=Sof(C29')=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C29)=FVAR(2)
 Sof(F13')=Sof(F14')=Sof(F15')=Sof(C25')=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(C25)=FVAR(3)
 Sof(F7')=Sof(F8')=Sof(F9')=Sof(C20')=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C20)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C11(H11), C13(H13), C14(H14), C17(H17), C22(H22), C27(H27)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_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 1.604
_oxdiff_exptl_absorpt_empirical_full_min 0.724