Syntheses, structures and magnetic properties of three dinuclear, one-dimensional and two-dimensional dysprosium(iii) complexes based on naphthalene diimide salicylic acid
Chen, Jia-Ting; Kuang, Xiao-Man; Li, You-Hong; Zhong, Yun-Jing; Zhang, Hui; Su, Jia-Yin; Chen, Wen-Bin; Dong, Wen; CrystEngComm 26 (2024) 5461–5468; doi:10.1039/D4CE00751D

data_7249289
_publ_section_title
;
 Syntheses, structures and magnetic properties of three dinuclear,
 one-dimensional and two-dimensional dysprosium(iii) complexes based on
 naphthalene diimide salicylic acid
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5461
_journal_page_last               5468
_journal_paper_doi               10.1039/D4CE00751D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C45 H33 Dy N4 O20, 3(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C54 H58 Dy N7 O25'
_chemical_formula_weight         1367.57
_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             2023-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                83.0210(10)
_cell_angle_beta                 74.564(2)
_cell_angle_gamma                84.6300(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5540(2)
_cell_length_b                   12.8863(2)
_cell_length_c                   19.4414(3)
_cell_measurement_reflns_used    18621
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.4680
_cell_measurement_theta_min      2.4120
_cell_volume                     2763.83(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(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 0.974
_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    -40.00  18.00   0.50    0.36    --  -46.85  37.00 150.00  116
  2  \w     -7.00  20.00   0.50    0.36    --  -46.85  19.00   0.00   54
  3  \w    -29.00  24.00   0.50    0.36    --  -46.85  37.00-150.00  106
  4  \w     83.00 169.00   0.50    0.78    --   99.00  61.00   0.00  172
  5  \w     96.00 170.00   0.50    0.78    --   99.00  45.00 -30.00  148
  6  \w     83.00 166.00   0.50    0.78    --   99.00  61.00 -60.00  166
  7  \w    147.00 172.00   0.50    0.78    --   99.00  85.00-105.00   50
  8  \w     86.00 140.00   0.50    0.78    --   99.00 125.00-180.00  108
  9  \w     86.00 126.00   0.50    0.78    --   99.00  85.00-105.00   80
 10  \w    -14.00  21.00   0.50    0.36    --   46.85 -19.00-150.00   70
 11  \w     26.00  52.00   0.50    0.78    --   99.00 -61.00-120.00   52
 12  \w     28.00  67.00   0.50    0.78    --   99.00 -61.00  30.00   78
 13  \w     27.00  52.00   0.50    0.78    --   99.00 -45.00 120.00   50
 14  \w     27.00  52.00   0.50    0.78    --   99.00 -45.00 150.00   50
 15  \w     52.00  77.00   0.50    0.78    --   99.00 -85.00 134.00   50
 16  \w     29.00 110.00   0.50    0.78    --   99.00-125.00 120.00  162
 17  \w     69.00 110.00   0.50    0.78    --   99.00-125.00  60.00   82
 18  \w     29.00 109.00   0.50    0.78    --   99.00-125.00 -60.00  160
 19  \w     57.00 108.00   0.50    0.78    --   99.00-125.00 -90.00  102
 20  \w     27.00  62.00   0.50    0.78    --   99.00 -94.00-150.00   70
 21  \w     68.00 104.00   0.50    0.78    --   99.00-125.00-150.00   72
 22  \w    -20.00  63.00   0.50    0.36    --   46.85 -85.00 134.00  166
 23  \w    -58.00 -32.00   0.50    0.78    --  -99.00  77.00  90.00   52
 24  \w    -92.00 -66.00   0.50    0.78    --  -99.00  77.00 120.00   52
 25  \w    -96.00 -71.00   0.50    0.78    --  -99.00  77.00  90.00   50
 26  \w    -54.00 -27.00   0.50    0.78    --  -99.00  77.00   0.00   54
 27  \w   -101.00 -63.00   0.50    0.78    --  -99.00  77.00   0.00   76
 28  \w    -68.00 -27.00   0.50    0.78    --  -99.00  61.00-180.00   82
 29  \w    -69.00  24.00   0.50    0.36    --  -46.85  85.00-105.00  186
 30  \w   -109.00 -38.00   0.50    0.78    --  -99.00 125.00 -60.00  142
 31  \w   -108.00 -57.00   0.50    0.78    --  -99.00 111.00 -61.73  102
 32  \w    -96.00 -47.00   0.50    0.78    --  -99.00  85.00-105.00   98
 33  \w   -108.00 -27.00   0.50    0.78    --  -99.00 114.00   0.18  162
 34  \w   -126.00 -33.00   0.50    0.78    --  -99.00 144.00  59.84  186
 35  \w   -108.00 -40.00   0.50    0.78    --  -99.00 110.00 176.83  136
 36  \w   -163.00 -87.00   0.50    0.78    --  -99.00 -15.00-150.00  152
 37  \w   -109.00 -74.00   0.50    0.36    --  -46.85-125.00 -60.00   70
 38  \w   -119.00 -91.00   0.50    0.36    --  -46.85-125.00-120.00   56
 39  \w   -119.00 -75.00   0.50    0.36    --  -46.85-125.00-150.00   88
 40  \w   -113.00 -87.00   0.50    0.78    --  -99.00-125.00  30.00   52
 41  \w   -141.00 -86.00   0.50    0.78    --  -99.00 -85.00 134.00  110
 42  \w   -168.00-139.00   0.50    0.78    --  -99.00-125.00  30.00   58
;
_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      -0.0899665000
_diffrn_orient_matrix_UB_12      -0.0370206000
_diffrn_orient_matrix_UB_13      0.0707754000
_diffrn_orient_matrix_UB_21      0.0960892000
_diffrn_orient_matrix_UB_22      -0.0821103000
_diffrn_orient_matrix_UB_23      0.0180873000
_diffrn_orient_matrix_UB_31      0.0434233000
_diffrn_orient_matrix_UB_32      0.0803333000
_diffrn_orient_matrix_UB_33      0.0386103000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40597
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.610
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       needle
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         10870
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0768P)^2^+6.1154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9637
_reflns_number_total             10870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00751d2.cif
_cod_data_source_block           kuangxiaoman-0929-dycl3-2_auto
_cod_depositor_comments
'Adding full bibliography for 7249287--7249289.cif.'
_cod_database_code               7249289
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Dy'
_shelx_estimated_absorpt_t_max   0.565
_shelx_estimated_absorpt_t_min   0.378
_diffrn_oxdiff_digest_frames
;
01671c89050eb17066c1cfb00fbb01d89b00047ab43
;
_diffrn_oxdiff_digest_hkl
;
017c45b46bcf64e93f66cf6a65718a98919741
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C48) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C53) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
3. Others
 Fixed Sof: N4(0.6) N5(0.4) C43(0.6) H43(0.6) C44(0.6) H44A(0.6) H44B(0.6)
 H44C(0.6) C46(0.4) H46(0.4) C47(0.4) H47A(0.4) H47B(0.4) H47C(0.4) C48(0.4)
 H48A(0.4) H48B(0.4) H48C(0.4) C45(0.6) H45A(0.6) H45B(0.6) H45C(0.6)
4.a Riding coordinates:
 O20(H20A,H20B), O19(H19A,H19B), O18(H18A,H18B), O17(H17A,H17B), O25(H25A,
 H25B), O24(H24A,H24B), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C53(H53A,H53B,
 H53C)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C31(H31), C6(H6A), C41(H41), C30(H30), C25(H25), C20(H20),
 C24(H24), C12(H12), C18(H18), C17(H17), C11(H11), C37(H37), C38(H38), C49(H49),
  C55(H55), C52(H52), C43(H43), C46(H46)
4.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C44(H44A,H44B,
 H44C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O6(H6), O13(H13)
;
_shelx_res_checksum              26533
_shelx_hkl_checksum              96240
_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 1.758
_oxdiff_exptl_absorpt_empirical_full_min 0.593