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_7229244
_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.cc1p5yg8
_audit_creation_date             2016-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.167(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9723(4)
_cell_length_b                   24.1441(9)
_cell_length_c                   12.9349(5)
_cell_measurement_reflns_used    7047
_cell_measurement_temperature    111.07(15)
_cell_measurement_theta_max      28.8170
_cell_measurement_theta_min      3.5590
_cell_volume                     3680.3(2)
_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      111.07(15)
_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    -16.00  98.00   1.00    1.59    --   11.08   0.00 -60.00  114
  2  \w    -10.00  17.00   1.00    1.59    --  -11.24 -99.00  30.00   27
  3  \w    -16.00  36.00   1.00    1.59    --   11.08 -57.00 -60.00   52
  4  \w     35.00  60.00   1.00    1.59    --   11.08-178.00  30.00   25
;
_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      0.0190838000
_diffrn_orient_matrix_UB_12      0.0278344000
_diffrn_orient_matrix_UB_13      0.0058038000
_diffrn_orient_matrix_UB_21      0.0156768000
_diffrn_orient_matrix_UB_22      -0.0040288000
_diffrn_orient_matrix_UB_23      0.0549645000
_diffrn_orient_matrix_UB_31      0.0548736000
_diffrn_orient_matrix_UB_32      -0.0085369000
_diffrn_orient_matrix_UB_33      -0.0069198000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18113
_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         3.458
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78456
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.739
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0426P)^2^+16.6480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5392
_reflns_number_total             6476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09192c2.cif
_cod_data_source_block           a160406d
_cod_database_code               7229244
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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-C28
 1.53 with sigma of 0.01
 F16'-C29 = F16-C29 = F17'-C29 = F17-C29 = F18'-C29 = F18-C29
 1.35 with sigma of 0.001
 F16-F18 \\sim F18-F17
 with sigma of 0.001
 F17-F16 \\sim F16-F18
 with sigma of 0.001
 F18-F17 \\sim F17-F16
 with sigma of 0.001
 F17-F16 \\sim F16-F18
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F11) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F16) \\sim Ueq, Uanis(F16') \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F18')
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F17') \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(F16') = Uanis(F16)
Uanis(F18) = Uanis(F18')
Uanis(F17') = Uanis(F17)
4. Others
 Sof(F17')=Sof(F16')=Sof(F18')=1-FVAR(1)
 Sof(F18)=Sof(F17)=Sof(F16)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C14(H14), C13(H13), C9(H9), C10(H10), C22(H22), C27(H27), C17(H17)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-06
_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 1.457
_oxdiff_exptl_absorpt_empirical_full_min 0.785