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_7048261
_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         '2(C25 H18 Dy F18 N4 O8)'
_chemical_formula_sum            'C50 H36 Dy2 F36 N8 O16'
_chemical_formula_weight         2013.87
_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_block_doi                 10.5517/ccdc.csd.cc2051py
_audit_creation_date             2018-04-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.210(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3377(12)
_cell_length_b                   17.6000(7)
_cell_length_c                   18.5483(10)
_cell_measurement_reflns_used    7650
_cell_measurement_temperature    106.22(10)
_cell_measurement_theta_max      29.1170
_cell_measurement_theta_min      2.2280
_cell_volume                     6926.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      106.22(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_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     66.00  98.00   1.00    4.44    --   11.08-178.00 -30.00   32
  2  \w    -81.00  14.00   1.00    4.44    --  -11.24 -57.00  30.00   95
  3  \w    -86.00  -7.00   1.00    4.44    --  -11.24 -38.00 120.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0332967000
_diffrn_orient_matrix_UB_12      -0.0030140000
_diffrn_orient_matrix_UB_13      0.0134752000
_diffrn_orient_matrix_UB_21      0.0000223000
_diffrn_orient_matrix_UB_22      -0.0124511000
_diffrn_orient_matrix_UB_23      -0.0363708000
_diffrn_orient_matrix_UB_31      0.0026220000
_diffrn_orient_matrix_UB_32      0.0382293000
_diffrn_orient_matrix_UB_33      -0.0107991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32261
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.071
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       block
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.818
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.154
_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     1027
_refine_ls_number_reflns         12211
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0519P)^2^+35.0816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8348
_reflns_number_total             12211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03809k2.cif
_cod_data_source_block           a180328d
_cod_depositor_comments
'Adding full bibliography for 7048260--7048262.cif.'
_cod_original_cell_volume        6927.0(6)
_cod_database_code               7048261
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.95
_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
 F22A-C39 = F22-C39 = F23A-C39 = F23-C39 = F24A-C39 = F24-C39
 1.34 with sigma of 0.01
 F22-F23 \\sim F23-F24
 with sigma of 0.001
 F24-F22 \\sim F22-F23
 with sigma of 0.001
 F22A-F23A \\sim F23A-F24A
 with sigma of 0.001
 F24A-F22A \\sim F22A-F23A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F24) \\sim Ueq, Uanis(F24A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F23A)
\\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(F24) = Uanis(F24A)
Uanis(F22A) = Uanis(F22)
Uanis(F23A) = Uanis(F23)
4. Others
 Sof(F24A)=Sof(F22A)=Sof(F23A)=1-FVAR(1)
 Sof(F23)=Sof(F22)=Sof(F24)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C34(H34), N4(H4), N8(H8), C33(H33), C42(H42), C18(H18), C10(H10),
 C13(H13), C23(H23), C47(H47), C37(H37)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C)
;
_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 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.745