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_7229246
_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
_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.cc1p5yf7
_audit_creation_date             2016-04-07
_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                 100.293(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0292(4)
_cell_length_b                   24.1953(12)
_cell_length_c                   12.9431(5)
_cell_measurement_reflns_used    7427
_cell_measurement_temperature    110.5(2)
_cell_measurement_theta_max      28.8230
_cell_measurement_theta_min      3.8850
_cell_volume                     3706.5(3)
_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      110.5(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     -1.00  69.00   1.00    3.94    --   11.08  19.00 -90.00   70
  2  \w     60.00  86.00   1.00    3.94    --   11.08 178.00-180.00   26
  3  \w    -52.00  10.00   1.00    3.94    --   11.08 -38.00 120.00   62
  4  \w     46.00  72.00   1.00    3.94    --   11.08-178.00 -90.00   26
  5  \w     53.00  97.00   1.00    3.94    --   11.08-178.00  90.00   44
;
_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      -0.0355904000
_diffrn_orient_matrix_UB_12      -0.0135096000
_diffrn_orient_matrix_UB_13      -0.0420409000
_diffrn_orient_matrix_UB_21      0.0164795000
_diffrn_orient_matrix_UB_22      0.0191905000
_diffrn_orient_matrix_UB_23      -0.0358630000
_diffrn_orient_matrix_UB_31      0.0453125000
_diffrn_orient_matrix_UB_32      -0.0175791000
_diffrn_orient_matrix_UB_33      -0.0068443000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18959
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60534
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.174
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         6501
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0334P)^2^+18.5913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5454
_reflns_number_total             6501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09192c2.cif
_cod_data_source_block           a160407a
_cod_database_code               7229246
_reflns_odcompleteness_completeness 99.74
_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
 F8-C20 = F9-C20 = F7-C20
 1.35 with sigma of 0.01
 F8'-C20 = F9'-C20 = F7'-C20
 1.35 with sigma of 0.001
 F9-F7 \\sim F7-F8
 with sigma of 0.001
 F7-F8 \\sim F8-F9
 with sigma of 0.001
 F9'-F8' \\sim F8'-F7'
 with sigma of 0.001
 F8'-F7' \\sim F7'-F9'
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F9') \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7') \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F3) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F15)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(F8') = Uanis(F8)
Uanis(F9') = Uanis(F9)
Uanis(F7') = Uanis(F7)
4. Others
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C12(H12), C13(H13), C14(H14), C17(H17), C22(H22), C27(H27)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-07
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.708