Experimental and theoretical interpretation of the magnetic behavior of two Dy(iii) single-ion magnets constructed through β-diketonate ligands with different substituent groups (‒Cl/‒OCH3)
Zhang, Sheng; Mo, Wenjiao; Zhang, Jiangwei; Wu, Haipeng; Li, Min; Lü, Xingqiang; Yin, Bing; Yang, Desuo; RSC Advances 8 (2018) 29513–; doi:10.1039/C8RA06240D

data_7231393
_publ_section_title
;
 Experimental and theoretical interpretation of the magnetic behavior of
 two Dy(iii) single-ion magnets constructed through \b-diketonate ligands
 with different substituent groups (--Cl/--OCH3)
;
_journal_issue                   52
_journal_name_full               'RSC Advances'
_journal_page_first              29513
_journal_paper_doi               10.1039/C8RA06240D
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C42 H23 Cl3 Dy F9 N2 O6'
_chemical_formula_sum            'C42 H23 Cl3 Dy F9 N2 O6'
_chemical_formula_weight         1091.47
_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   geom
_audit_creation_date             2018-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                98.652(7)
_cell_angle_beta                 100.231(8)
_cell_angle_gamma                102.305(8)
_cell_formula_units_Z            2
_cell_length_a                   11.5704(11)
_cell_length_b                   12.1367(11)
_cell_length_c                   15.4949(13)
_cell_measurement_reflns_used    1774
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9430
_cell_measurement_theta_min      3.7940
_cell_volume                     2051.6(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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -72.00   7.00   1.00    1.00    --  -56.18  61.00 -60.00   79
  2  \w     12.00  49.00   1.00    1.00    --    0.00  57.00 -30.00   37
  3  \w    -20.00   6.00   1.00    1.00    --    0.00  57.00 -30.00   26
  4  \w     -4.00  23.00   1.00    1.00    --    0.00 -57.00-180.00   27
  5  \w    -71.00 -28.00   1.00    1.00    --    0.00 -57.00-180.00   43
  6  \w     21.00 110.00   1.00    1.00    --   56.18-125.00-120.00   89
  7  \w     70.00 101.00   1.00    1.00    --  112.35-111.00-180.00   31
  8  \w     94.00 141.00   1.00    1.00    --  112.35 -91.00-120.00   47
  9  \w    139.00 176.00   1.00    1.00    --  112.35  25.00-180.00   37
 10  \w    113.00 178.00   1.00    1.00    --  112.35 111.00-120.00   65
 11  \w    115.00 174.00   1.00    1.00    --  112.35 111.00-150.00   59
 12  \w     96.00 174.00   1.00    1.00    --  112.35  50.00-120.00   78
 13  \w    100.00 162.00   1.00    1.00    --  112.35 111.00-180.00   62
 14  \w     92.00 177.00   1.00    1.00    --  112.35  37.00 -30.00   85
 15  \w     77.00 131.00   1.00    1.00    --  112.35 -63.00  60.00   54
 16  \w     53.00 112.00   1.00    1.00    --  112.35-111.00  60.00   59
 17  \w     46.00  72.00   1.00    1.00    --   56.18 -77.00  30.00   26
 18  \w     39.00 145.00   1.00    1.00    --  112.35 -37.00 150.00  106
 19  \w     49.00 116.00   1.00    1.00    --  112.35 -37.00 -90.00   67
 20  \w     68.00 121.00   1.00    1.00    --  112.35  25.00-180.00   53
 21  \w     49.00 118.00   1.00    1.00    --  112.35 -63.00-150.00   69
 22  \w     46.00 113.00   1.00    1.00    --  112.35-111.00-120.00   67
 23  \w    -14.00  16.00   1.00    1.00    --   56.18 -77.00  30.00   30
 24  \w    -76.00  -7.00   1.00    1.00    --  -56.18  61.00  90.00   69
 25  \w    -77.00 -31.00   1.00    1.00    --  -56.18  61.00  30.00   46
 26  \w    -80.00 -42.00   1.00    1.00    --    0.00 178.00  60.00   38
 27  \w   -118.00 -26.00   1.00    1.00    --  -56.18 -77.00 120.00   92
 28  \w   -118.00 -80.00   1.00    1.00    --  -56.18 -94.00  90.00   38
 29  \w   -119.00 -80.00   1.00    1.00    --  -56.18 -94.00   0.00   39
 30  \w   -129.00 -83.00   1.00    1.00    --  -56.18 -94.00  60.00   46
 31  \w   -123.00 -84.00   1.00    1.00    --  -56.18 -94.00-150.00   39
 32  \w   -120.00 -95.00   1.00    1.00    --  -56.18-125.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1126625000
_diffrn_orient_matrix_UB_12      -0.0708235000
_diffrn_orient_matrix_UB_13      0.0242692000
_diffrn_orient_matrix_UB_21      0.0793170000
_diffrn_orient_matrix_UB_22      -0.0682810000
_diffrn_orient_matrix_UB_23      0.0490862000
_diffrn_orient_matrix_UB_31      0.0224958000
_diffrn_orient_matrix_UB_32      0.0887341000
_diffrn_orient_matrix_UB_33      0.0872662000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_unetI/netI     0.1673
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11224
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        59.999
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_min         4.335
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.367
_exptl_absorpt_correction_T_max  0.428
_exptl_absorpt_correction_T_min  0.421
_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            ad
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     1887
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3381
_reflns_number_total             6059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra06240d2.cif
_cod_data_source_block           exp_8484
_cod_database_code               7231393
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.478
_shelx_estimated_absorpt_t_min   0.438
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
3. Others
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C12(H12), C13(H13), C15(H15),
 C16(H16), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C31(H31),
  C32(H32), C33(H33), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_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 2.056
_oxdiff_exptl_absorpt_empirical_full_min 0.723