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_7708158
_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         'C27 H18 Dy N15 O12, 3(H2 O)'
_chemical_formula_sum            'C27 H24 Dy N15 O15'
_chemical_formula_weight         961.11
_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'
_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                90
_cell_angle_beta                 110.0249(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.96209(10)
_cell_length_b                   16.44139(8)
_cell_length_c                   17.20872(11)
_cell_measurement_reflns_used    27230
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0640
_cell_measurement_theta_min      3.3700
_cell_volume                     3711.54(4)
_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)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -64.00  27.00   0.50    0.21    --  -45.62  96.00 -79.00  182
  2  \w    -22.00  60.00   0.50    0.21    --   45.62 -96.00 170.00  164
  3  \w    -92.00 -67.00   0.50    0.90    -- -102.00  96.00 -79.00   50
  4  \w   -123.00 -97.00   0.50    0.90    -- -102.00 -96.00 170.00   52
  5  \w     48.00  74.00   0.50    0.90    --  106.06 -96.00 170.00   52
  6  \w     93.00 149.00   0.50    0.90    --  106.06  96.00 -79.00  112
  7  \w    -13.00  30.00   0.50    0.21    --  -45.62  19.00 -60.00   86
  8  \w    -17.00  28.00   0.50    0.21    --  -45.62  37.00  30.00   90
  9  \w    -93.00 -68.00   0.50    0.21    --  -45.62 125.00 120.00   50
 10  \w    -23.00  30.00   0.50    0.21    --  -45.62  19.00 -90.00  106
 11  \w    -22.00  29.00   0.50    0.21    --  -45.62  19.00-180.00  102
 12  \w    -62.00 -14.00   0.50    0.21    --  -45.62 125.00 120.00   96
 13  \w     19.00  46.00   0.50    0.21    --   45.62-125.00 120.00   54
 14  \w     69.00  94.00   0.50    0.21    --   45.62-125.00 120.00   50
 15  \w    -67.00 -30.00   0.50    0.90    -- -102.00  61.00  30.00   74
 16  \w   -175.00-150.00   0.50    0.90    -- -102.00 -15.00-120.00   50
 17  \w    -69.00 -31.00   0.50    0.90    -- -102.00 125.00  30.00   76
 18  \w   -138.00 -85.00   0.50    0.90    -- -102.00 -15.00-120.00  106
 19  \w   -108.00 -80.00   0.50    0.90    -- -102.00 125.00  30.00   56
 20  \w    -67.00 -36.00   0.50    0.90    -- -102.00  61.00  90.00   62
 21  \w   -107.00 -29.00   0.50    0.90    -- -102.00 108.00 112.83  156
 22  \w   -165.00-117.00   0.50    0.90    -- -102.00 -45.00-150.00   96
 23  \w   -108.00 -29.00   0.50    0.90    -- -102.00 109.00-104.99  158
 24  \w   -149.00 -79.00   0.50    0.90    -- -102.00 -77.00 -90.00  140
 25  \w   -127.00 -55.00   0.50    0.90    -- -102.00 147.00 -49.80  144
 26  \w    -68.00 -31.00   0.50    0.90    -- -102.00  61.00   0.00   74
 27  \w   -112.00 -44.00   0.50    0.90    -- -102.00 125.00-180.00  136
 28  \w   -107.00 -68.00   0.50    0.90    -- -102.00 106.00-151.51   78
 29  \w   -168.00 -33.00   0.50    0.90    -- -102.00   0.00 -90.00  270
 30  \w     93.00 118.00   0.50    0.90    --  106.06  15.00-150.00   50
 31  \w     40.00  96.00   0.50    0.90    --  106.06-125.00  90.00  112
 32  \w     43.00  71.00   0.50    0.90    --  106.06 -94.00-120.00   56
 33  \w     40.00  72.00   0.50    0.90    --  106.06 -61.00-180.00   64
 34  \w     36.00  79.00   0.50    0.90    --  106.06 -94.00-180.00   86
 35  \w     48.00  73.00   0.50    0.90    --  106.06 -61.00 150.00   50
 36  \w    134.00 175.00   0.50    0.90    --  106.06  15.00-150.00   82
 37  \w     40.00 105.00   0.50    0.90    --  106.06-125.00 -30.00  130
 38  \w    105.00 152.00   0.50    0.90    --  106.06 125.00-120.00   94
 39  \w     62.00 106.00   0.50    0.90    --  106.06-104.00 -49.49   88
 40  \w     35.00  68.00   0.50    0.90    --  106.06 -61.00   0.00   66
 41  \w     37.00 112.00   0.50    0.90    --  106.06-125.00 150.00  150
 42  \w     33.00  87.00   0.50    0.90    --  106.06 -94.00 -30.00  108
 43  \w     35.00  68.00   0.50    0.90    --  106.06 -61.00  60.00   66
;
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50442
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.821
_diffrn_reflns_theta_min         3.369
_exptl_absorpt_coefficient_mu    11.564
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67939
_exptl_absorpt_correction_type   multi-scan
_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    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.954
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         7632
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+5.3781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7322
_reflns_number_total             7632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02532e2.cif
_cod_data_source_block           121907-yehuajian
_cod_database_code               7708158
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H14A of O14B, All N(H) groups, All O(H,H) groups, All O(H,
  H,H,H) groups
 At 1.5 times of:
  H8 of O8, H2 of O2, H6 of O6, H10 of O10, H12 of O12, H4 of O4
2. Uiso/Uaniso restraints and constraints
H14C \\sim O14B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14A) = Uanis(O14B)
3. Others
 Sof(O14B)=Sof(H14A)=Sof(H14B)=1-FVAR(1)
 Sof(O14A)=Sof(H14C)=Sof(H14D)=FVAR(1)
 Fixed Sof: O13(0.5) H13A(0.5) H13B(0.5) O16(0.5) H16A(0.5) H16B(0.5) O17(0.5)
 H17A(0.5) H17B(0.5) O15(0.5) H15A(0.5) H15B(0.5)
4.a Riding coordinates:
 O14B(H14A), O14A(H14C), O13(H13A,H13B), O16(H16A,H16B), O17(H17A,H17B),
 O15(H15A,H15B), O15(H14D), O15(H14B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), N7(H7), N12(H12A), C1(H1), C7(H7A), C8(H8A), C10(H10A), C16(H16),
 C17(H17), C19(H19), C25(H25), C26(H26)
4.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O6(H6), O8(H8), O10(H10), O12(H12)
;
_shelx_res_checksum              97062
_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
;