Syntheses, structural modulation and slow magnetic relaxation of three dysprosium(III) complexes with mononuclear, dinuclear and one-dimensional structures
Ye, Hua-Jian; Zhang, Tian; Huang, Shu-Yuan; Liu, Xiao-Ling; Chen, Wen-Bin; Zhang, Yi-Quan; Tang, Jinkui; Dong, Wen; Dalton Transactions  (2021) –; doi:10.1039/D1DT02532E

data_7708160
_publ_section_title
;
 Syntheses, structural modulation&#x00A0;and slow magnetic relaxation of
 three dysprosium(III) complexes with mononuclear, dinuclear and
 one-dimensional structures
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02532E
_journal_year                    2021
_chemical_formula_moiety         'C16 H16 Dy N6 O8, 2(C3 H7 N O)'
_chemical_formula_sum            'C22 H30 Dy N8 O10'
_chemical_formula_weight         729.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                112.6490(10)
_cell_angle_beta                 100.3860(10)
_cell_angle_gamma                98.7410(10)
_cell_formula_units_Z            2
_cell_length_a                   10.56300(10)
_cell_length_b                   11.32340(10)
_cell_length_c                   12.71470(10)
_cell_measurement_reflns_used    14818
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9100
_cell_measurement_theta_min      3.8920
_cell_volume                     1338.83(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_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    127.00 174.00   0.50    0.12    --  106.06  36.00  38.00   94
  2  \w     94.00 123.00   0.50    0.12    --  106.06  36.00  38.00   58
  3  \w     31.00 115.00   0.50    0.05    --   46.00  36.00  38.00  168
  4  \w    138.00 164.00   0.50    0.12    --  106.06  30.00-180.00   52
  5  \w     92.00 134.00   0.50    0.12    --  106.06  30.00-180.00   84
  6  \w     36.00  85.00   0.50    0.05    --   46.00-125.00  60.00   98
  7  \w     35.00 112.00   0.50    0.12    --  106.06-125.00 150.00  154
  8  \w     34.00  80.00   0.50    0.12    --  106.06-125.00 120.00   92
  9  \w     36.00  62.00   0.50    0.12    --  106.06 -94.00 150.00   52
 10  \w     45.00 101.00   0.50    0.12    --  106.06 -94.00   0.00  112
 11  \w     42.00  92.00   0.50    0.12    --  106.06 -94.00  60.00  100
 12  \w     63.00  89.00   0.50    0.12    --  106.06 -94.00 -30.00   52
 13  \w     52.00  78.00   0.50    0.12    --  106.06 -94.00 -90.00   52
 14  \w     37.00 112.00   0.50    0.12    --  106.06-125.00-150.00  150
 15  \w     49.00  86.00   0.50    0.12    --  106.06 -94.00-180.00   74
 16  \w     35.00  73.00   0.50    0.12    --  106.06 -61.00-120.00   76
 17  \w     37.00  71.00   0.50    0.12    --  106.06 -61.00 -90.00   68
 18  \w     41.00  71.00   0.50    0.12    --  106.06 -61.00 -60.00   60
 19  \w     42.00  73.00   0.50    0.12    --  106.06 -61.00  60.00   62
 20  \w     19.00  68.00   0.50    0.05    --   46.00 -77.00-120.00   98
 21  \w    -22.00  43.00   0.50    0.05    --   46.00 -36.00-118.00  130
 22  \w    -20.00  13.00   0.50    0.05    --   46.00 -77.00-120.00   66
 23  \w    -24.00  44.00   0.50    0.05    --   46.00 -37.00 120.00  136
 24  \w   -108.00 -30.00   0.50    0.12    -- -102.00 110.00 -37.74  156
 25  \w    -69.00 -44.00   0.50    0.12    -- -102.00 125.00  90.00   50
 26  \w   -120.00 -38.00   0.50    0.12    -- -102.00 137.00  -2.92  164
 27  \w    -59.00 -29.00   0.50    0.12    -- -102.00 125.00-120.00   60
 28  \w   -108.00 -68.00   0.50    0.12    -- -102.00 125.00-120.00   80
 29  \w   -108.00 -60.00   0.50    0.12    -- -102.00 110.00-141.11   96
 30  \w    -69.00 -30.00   0.50    0.12    -- -102.00  61.00 -90.00   78
 31  \w    -69.00 -29.00   0.50    0.12    -- -102.00  61.00-120.00   80
 32  \w   -175.00 -87.00   0.50    0.12    -- -102.00 -36.00-118.00  176
 33  \w   -173.00-101.00   0.50    0.12    -- -102.00 -30.00-180.00  144
 34  \w   -119.00 -60.00   0.50    0.05    --  -46.00 -36.00-118.00  118
 35  \w   -174.00 -87.00   0.50    0.12    -- -102.00 -30.00 -30.00  174
 36  \w   -175.00-140.00   0.50    0.12    -- -102.00 -30.00 120.00   70
 37  \w   -128.00 -86.00   0.50    0.12    -- -102.00 -30.00 120.00   84
 38  \w    -12.00  14.00   0.50    0.05    --  -46.00  36.00  38.00   52
 39  \w   -114.00 -89.00   0.50    0.05    --  -46.00-125.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17175
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.674
_diffrn_reflns_theta_min         3.903
_exptl_absorpt_coefficient_mu    15.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5387
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0491P)^2^+0.3538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5222
_reflns_number_total             5387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02532e2.cif
_cod_data_source_block           exp_756
_cod_original_cell_volume        1338.83(2)
_cod_database_code               7708160
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O10-C22
 1.25 with sigma of 0.01
 O9-C22
 1.25 with sigma of 0.01
 C22-N8
 1.32 with sigma of 0.01
 O8-C18 \\sim O8A-C18A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.04
 N7-C17 \\sim N7A-C17A
 with sigma of 0.02
 N7-C18 \\sim N7A-C18A
 with sigma of 0.02
 N7-C19 \\sim N7A-C19A
 with sigma of 0.02
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 O8-N7 \\sim O8A-N7A
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C18A) = Uanis(C17)
Uanis(C19A) = Uanis(C19)
Uanis(C18) = Uanis(C17A)
Uanis(N7A) = Uanis(N7)
Uanis(O8A) = Uanis(O8)
4. Others
 Sof(N7A)=Sof(O8A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(O8)=Sof(N7)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Fixed Sof: H22(0.5) H22A(0.5) O9(0.6) O10(0.4)
5.a Rotating group:
 O7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C4(H4), C5(H5A), C9(H9), C12(H12), C13(H13), C14(H14), C18(H18),
 C22(H22), C22(H22A), C18A(H18A)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C17A(H17D,H17E,H17F),
 C19A(H19D,H19E,H19F)
5.d Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_shelx_res_checksum              54101
_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
;