Elucidation of the two-step relaxation processes of a tetranuclear dysprosium molecular nanomagnet through magnetic dilution.
Fang, Yu; Ji, Xiao-Qin; Xiong, Jin; Li, Guanzheng; Ma, Fang; Sun, Hao-Ling; Zhang, Yi-Quan; Gao, Song; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11636–11644; doi:10.1039/c8dt01870g

data_7047140
_publ_section_title
;
 Elucidation of the two-step relaxation processes of a tetranuclear
 dysprosium molecular nanomagnet through magnetic dilution.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11636
_journal_page_last               11644
_journal_paper_doi               10.1039/c8dt01870g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H28 N4 O12 Y2'
_chemical_formula_sum            'C24 H28 N4 O12 Y2'
_chemical_formula_weight         742.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-09 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                111.052(15)
_cell_angle_beta                 104.623(12)
_cell_angle_gamma                105.043(13)
_cell_formula_units_Z            2
_cell_length_a                   10.7338(13)
_cell_length_b                   11.874(2)
_cell_length_c                   13.261(2)
_cell_measurement_reflns_used    2321
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6470
_cell_measurement_theta_min      4.3230
_cell_volume                     1406.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.949
_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     69.00  96.00   1.00    3.00    --   39.74  37.00 -90.00   27
  2  \w     37.00 135.00   1.00   22.00    --  107.52 -61.00-150.00   98
  3  \w     76.00 122.00   1.00   22.00    --  107.52-125.00 -90.00   46
  4  \w     60.00 100.00   1.00   22.00    --  107.52 -94.00 -30.00   40
  5  \w     43.00 133.00   1.00   22.00    --  107.52 -77.00  90.00   90
  6  \w     90.00 118.00   1.00   22.00    --  107.52-125.00 120.00   28
  7  \w     34.00 128.00   1.00   22.00    --  107.52 -45.00 -30.00   94
  8  \w    108.00 175.00   1.00   22.00    --  107.52  30.00  60.00   67
  9  \w    131.00 169.00   1.00   22.00    --  107.52  45.00   0.00   38
 10  \w     99.00 132.00   1.00   22.00    --  107.52 125.00 120.00   33
 11  \w     83.00 108.00   1.00   22.00    --  107.52  45.00   0.00   25
 12  \w     99.00 170.00   1.00   22.00    --  107.52  30.00 -60.00   71
 13  \w    144.00 174.00   1.00   22.00    --  107.52 125.00-180.00   30
 14  \w     71.00 121.00   1.00    3.00    --   39.74 178.00  90.00   50
 15  \w     31.00 133.00   1.00   22.00    --  107.52 -30.00  60.00  102
 16  \w     34.00  62.00   1.00   22.00    --  107.52-125.00 -90.00   28
 17  \w     14.00  74.00   1.00    3.00    --   39.74 -99.00-150.00   60
 18  \w     63.00 114.00   1.00    3.00    --   39.74-178.00-150.00   51
 19  \w   -128.00  48.00   1.00    3.00    --  -39.74   0.00  90.00  176
;
_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      0.0332620000
_diffrn_orient_matrix_UB_12      0.0027179000
_diffrn_orient_matrix_UB_13      -0.1057248000
_diffrn_orient_matrix_UB_21      0.0004144000
_diffrn_orient_matrix_UB_22      0.1388421000
_diffrn_orient_matrix_UB_23      0.0368036000
_diffrn_orient_matrix_UB_31      0.1574499000
_diffrn_orient_matrix_UB_32      0.0588474000
_diffrn_orient_matrix_UB_33      0.0750813000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9385
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.948
_diffrn_reflns_theta_min         3.868
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_preparation       none
_exptl_crystal_recrystallization_method none
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0903P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.2108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3620
_reflns_number_total             5419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01870g2.cif
_cod_data_source_block           20170725b
_cod_depositor_comments
'Adding full bibliography for 7047139--7047140.cif.'
_cod_original_cell_volume        1406.8(4)
_cod_database_code               7047140
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c1 h1 n1 o1 y1'
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.460
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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, All O(H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 C24-H8
 1.860416 with sigma of 0.02
 Y2-H8
 2.948682 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N1) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O1) \\sim
Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12)
\\sim Ueq, Uanis(Y1) \\sim Ueq, Uanis(Y2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C2(H2), C3(H3A), C4(H4A), C5(H5), C7(H7), C9(H9), C11(H11),
 C12(H12), C13(H13), C14(H14)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C)
;
_olex2_date_sample_data_collection 2017-07-25
_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 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.633