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_7249288
_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         'C28 H15 Dy N2 O12, 2(H2 O)'
_chemical_formula_sum            'C28 H19 Dy N2 O14'
_chemical_formula_weight         769.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.789(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8770(3)
_cell_length_b                   37.7347(9)
_cell_length_c                   8.9024(4)
_cell_measurement_reflns_used    14951
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9370
_cell_measurement_theta_min      2.6840
_cell_volume                     2588.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  81.00   0.50    8.54    --    6.35  19.00 150.00  114
  2  \w    -16.00  68.00   0.50    8.54    --    6.35  77.00-150.00  168
  3  \w     -8.00  74.00   0.50    8.54    --    6.35  57.00   0.00  164
  4  \w      1.00  69.00   0.50    8.54    --    6.35  37.00 120.00  136
  5  \w    -14.00  33.00   0.50    8.54    --    6.35 -99.00   0.00   94
  6  \w    -34.00  10.00   0.50    8.54    --    6.35 -37.00-180.00   88
  7  \w    -34.00  -9.00   0.50    8.54    --    6.35 -57.00   0.00   50
;
_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      0.0005012000
_diffrn_orient_matrix_UB_12      -0.0167000000
_diffrn_orient_matrix_UB_13      -0.0363776000
_diffrn_orient_matrix_UB_21      -0.0433287000
_diffrn_orient_matrix_UB_22      0.0075725000
_diffrn_orient_matrix_UB_23      -0.0840187000
_diffrn_orient_matrix_UB_31      0.0812134000
_diffrn_orient_matrix_UB_32      0.0041482000
_diffrn_orient_matrix_UB_33      0.0071293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34502
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.648
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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    1.976
_exptl_crystal_description       plate
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.922
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0107P)^2^+14.0707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5113
_reflns_number_total             5955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00751d2.cif
_cod_data_source_block           xiaoman-erwei-dycl3-1_auto
_cod_depositor_comments
'Adding full bibliography for 7249287--7249289.cif.'
_cod_original_cell_volume        2587.99(19)
_cod_database_code               7249288
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Dy Cl'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.842
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C16(H16), C17(H17), C23(H23),
 C26(H26), C27(H27)
2.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              57832
_shelx_hkl_checksum              1745
_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 1.735
_oxdiff_exptl_absorpt_empirical_full_min 0.636