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_7708159
_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         'C32 H28 Dy2 N10 O20, 5(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C36 H44 Dy2 N12 O25'
_chemical_formula_weight         1369.83
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-25
_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                103.705(2)
_cell_angle_beta                 90.636(2)
_cell_angle_gamma                106.159(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6507(3)
_cell_length_b                   11.3380(2)
_cell_length_c                   11.8034(4)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    105.88(10)
_cell_measurement_theta_max      75.7670
_cell_measurement_theta_min      3.8760
_cell_volume                     1201.07(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      105.88(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_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     24.00 117.00   0.50    0.05    --   45.87  77.00 -90.00  186
  2  \w     92.00 119.00   0.50    0.05    --   45.87  77.00-150.00   54
  3  \w     69.00  94.00   0.50    0.05    --   45.87 142.00-101.00   50
  4  \w     24.00  87.00   0.50    0.05    --   45.87  77.00-150.00  126
  5  \w     90.00 178.00   0.50    0.05    --  106.06  15.00 -30.00  176
  6  \w    117.00 164.00   0.50    0.05    --  106.06  45.00   0.00   94
  7  \w     95.00 120.00   0.50    0.05    --  106.06 142.00-101.00   50
  8  \w     85.00 128.00   0.50    0.05    --  106.06 127.00  88.00   86
  9  \w     37.00  73.00   0.50    0.05    --  106.06 -61.00-150.00   72
 10  \w     68.00 102.00   0.50    0.05    --  106.06 -94.00-150.00   68
 11  \w     92.00 123.00   0.50    0.05    --  106.06-142.00-157.00   62
 12  \w     55.00 111.00   0.50    0.05    --  106.06-125.00-120.00  112
 13  \w     58.00 112.00   0.50    0.05    --  106.06-125.00 -30.00  108
 14  \w     71.00  97.00   0.50    0.05    --  106.06 -94.00  30.00   52
 15  \w     46.00 112.00   0.50    0.05    --  106.06-127.00  12.00  132
 16  \w     53.00  93.00   0.50    0.05    --   45.87-127.00  12.00   80
 17  \w     36.00 111.00   0.50    0.05    --  106.06-125.00  30.00  150
 18  \w     34.00  66.00   0.50    0.05    --  106.06 -94.00  30.00   64
 19  \w     33.00  69.00   0.50    0.05    --  106.06 -61.00  30.00   72
 20  \w     34.00  73.00   0.50    0.05    --  106.06 -61.00 150.00   78
 21  \w     40.00  73.00   0.50    0.05    --  106.06 -61.00-120.00   66
 22  \w     33.00  67.00   0.50    0.05    --  106.06 -77.00-150.00   68
 23  \w     47.00  87.00   0.50    0.05    --  106.06-142.00-157.00   80
 24  \w     35.00 100.00   0.50    0.05    --   45.87-142.00-157.00  130
 25  \w    -55.00 -29.00   0.50    0.05    -- -102.00  61.00 120.00   52
 26  \w    -68.00 -30.00   0.50    0.05    -- -102.00  61.00  60.00   76
 27  \w    -88.00 -38.00   0.50    0.05    --  -45.87 127.00  88.00  100
 28  \w    -63.00 -31.00   0.50    0.05    -- -102.00  61.00-150.00   64
 29  \w    -86.00 -61.00   0.50    0.05    --  -45.87 142.00-101.00   50
 30  \w   -124.00 -98.00   0.50    0.05    -- -102.00 142.00-101.00   52
 31  \w   -111.00 -35.00   0.50    0.05    -- -102.00 127.00  88.00  152
 32  \w    -97.00 -29.00   0.50    0.05    -- -102.00  77.00 120.00  136
 33  \w   -141.00 -93.00   0.50    0.05    -- -102.00 -30.00  60.00   96
 34  \w   -104.00 -78.00   0.50    0.05    --  -45.87-127.00  12.00   52
 35  \w   -101.00 -76.00   0.50    0.05    --  -45.87-125.00  30.00   50
 36  \w   -111.00 -86.00   0.50    0.05    --  -45.87-125.00  90.00   50
 37  \w   -110.00 -85.00   0.50    0.05    -- -102.00-127.00  12.00   50
 38  \w   -145.00-112.00   0.50    0.05    -- -102.00 -77.00 -60.00   66
 39  \w   -117.00 -63.00   0.50    0.05    --  -45.87-142.00-157.00  108
 40  \w   -142.00-116.00   0.50    0.05    -- -102.00-142.00-157.00   52
 41  \w   -172.00 -29.00   0.50    0.05    -- -102.00   0.00-180.00  286
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1133099000
_diffrn_orient_matrix_UB_12      -0.0130545000
_diffrn_orient_matrix_UB_13      0.0855329000
_diffrn_orient_matrix_UB_21      -0.0819719000
_diffrn_orient_matrix_UB_22      0.0481737000
_diffrn_orient_matrix_UB_23      0.1039214000
_diffrn_orient_matrix_UB_31      -0.0908461000
_diffrn_orient_matrix_UB_32      -0.1373102000
_diffrn_orient_matrix_UB_33      -0.0075151000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.391
_diffrn_reflns_theta_min         3.868
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.092
_refine_diff_density_max         2.654
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0827P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4539
_reflns_number_total             4814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02532e2.cif
_cod_data_source_block           exp_646
_cod_database_code               7708159
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Dy'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H9A,H9B} of O9, H13B of O13, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, H5 of O5, {H10A,H10B} of O10, H1 of O1,
  {H11A,H11B} of O11, {H12A,H12B} of O12, H13A of O13
2. Restrained distances
 O9-H9B
 0.85 with sigma of 0.02
 H10B-H9B
 3 with sigma of 0.02
 H9B-H9A
 1.38 with sigma of 0.02
 O10-H9B
 3 with sigma of 0.02
3. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B)
4.b Free rotating group:
 O11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 N5(H5A), C4(H4), C5(H5B), C9(H9), C13(H13), C14(H14), C15(H15)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O5(H5), O8(H8)
;
_shelx_res_checksum              3997
_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 4.136
_oxdiff_exptl_absorpt_empirical_full_min 0.448