Slow relaxation of the magnetization observed in mononuclear Ln-radical compounds with D<sub>4d</sub> geometry configurations.
Chen, Peng Yun; Wu, Ming Ze; Liu, Zhong Yi; Tian, Li; Zhang, Yi Quan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 558–565; doi:10.1039/c8dt03809k

data_7048262
_publ_section_title
;
 Slow relaxation of the magnetization observed in mononuclear Ln-radical
 compounds with D<sub>4d</sub> geometry configurations.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              558
_journal_page_last               565
_journal_paper_doi               10.1039/c8dt03809k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C25 H18 F18 Gd N4 O8'
_chemical_formula_sum            'C25 H18 F18 Gd N4 O8'
_chemical_formula_weight         1001.68
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-19 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.425(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7171(4)
_cell_length_b                   17.7935(3)
_cell_length_c                   18.7601(4)
_cell_measurement_reflns_used    11174
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      78.8670
_cell_measurement_theta_min      3.6010
_cell_volume                     7151.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (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      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     26.00  89.00   0.50    1.50    --    0.00  57.00  60.00  126
  2  \w    -23.00   2.00   0.50    1.50    --    0.00  57.00  60.00   50
  3  \w     -8.00  19.00   0.50    1.50    --    0.00  82.00-180.00   54
  4  \w    -88.00  -1.00   0.50    1.50    --    0.00 -19.00 -60.00  174
  5  \w     54.00  87.00   0.50    1.50    --    0.00  57.00 -90.00   66
  6  \w     17.00  90.00   0.50    4.88    --  106.20 -45.00-180.00  146
  7  \w    120.00 146.00   0.50    4.88    --  106.20  82.00-150.00   52
  8  \w     78.00 189.00   0.50    4.88    --  106.20  45.00 -90.00  222
  9  \w     19.00 132.00   0.50    4.88    --  106.20 -77.00  90.00  226
 10  \w     73.00 139.00   0.50    4.88    --  106.20 -30.00 -60.00  132
 11  \w     80.00 151.00   0.50    4.88    --  106.20  77.00 -30.00  142
 12  \w    121.00 146.00   0.50    4.88    --  106.20  45.00  60.00   50
 13  \w     75.00 154.00   0.50    4.88    --  106.20  77.00 -90.00  158
 14  \w    157.00 183.00   0.50    4.88    --  106.20  77.00 -90.00   52
 15  \w    128.00 188.00   0.50    4.88    --  106.20  45.00 -60.00  120
 16  \w     78.00 126.00   0.50    4.88    --  106.20  61.00 -90.00   96
 17  \w     97.00 130.00   0.50    4.88    --  106.20 -45.00-180.00   66
 18  \w     19.00 119.00   0.50    4.88    --  106.20 -61.00  90.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0561618000
_diffrn_orient_matrix_UB_12      0.0163911000
_diffrn_orient_matrix_UB_13      -0.0714156000
_diffrn_orient_matrix_UB_21      -0.0211927000
_diffrn_orient_matrix_UB_22      0.0629608000
_diffrn_orient_matrix_UB_23      0.0423388000
_diffrn_orient_matrix_UB_31      0.0395766000
_diffrn_orient_matrix_UB_32      0.0571546000
_diffrn_orient_matrix_UB_33      -0.0261740000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49791
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9f (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    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         12771
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0765P)^2^+23.8380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9116
_reflns_number_total             12771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03809k2.cif
_cod_data_source_block           bizuo-gd
_cod_depositor_comments
'Adding full bibliography for 7048260--7048262.cif.'
_cod_database_code               7048262
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.175
_shelx_estimated_absorpt_t_min   0.135
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 F31-C46 = F30-C46 = F32-C46
 1.35 with sigma of 0.01
 F30A-C46 = F31A-C46 = F32A-C46
 1.35 with sigma of 0.01
 F30-F31 \\sim F31-F32
 with sigma of 0.001
 F32-F30 \\sim F30-F31
 with sigma of 0.001
 F31-F32 \\sim F32-F30
 with sigma of 0.001
 F30A-F32A \\sim F32A-F31A
 with sigma of 0.001
 F31A-F30A \\sim F30A-F32A
 with sigma of 0.001
 F32A-F31A \\sim F31A-F30A
 with sigma of 0.001
3. Rigid bond restraints
 F32, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F31, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F30, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C47
 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(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(F9) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F15) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F52) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F30) \\sim Ueq,
Uanis(F31) \\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C30)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(F26) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(C46) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(F30A) = Uanis(F30)
Uanis(F32) = Uanis(F32A)
Uanis(F31) = Uanis(F31A)
5. Others
 Sof(F32A)=Sof(F30A)=Sof(F31A)=1-FVAR(1)
 Sof(F30)=Sof(F31)=Sof(F32)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C9(H9), C10(H10), C13(H13), C18(H18), C23(H23), N6(H6), C34(H34),
 C35(H35), C38(H38), C43(H43), C48(H48)
6.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.764
_oxdiff_exptl_absorpt_empirical_full_min 0.539