A seven-coordinated DyIII single-ion magnet with C2v symmetry constructed by a multidentate Schiff-base ligand
Wang, Ruirui; Yao, Binling; Bai, Feifei; Wang, Wen; Li, Licun; Ma, Yue; Wang, Qinglun; Zhao, Bin; Zhang, Yuanzhu; CrystEngComm 23 (2021) 1718–1722; doi:10.1039/D0CE01826K

data_7242160
_publ_section_title
;
 A seven-coordinated DyIII single-ion magnet with C2v symmetry constructed
 by a multidentate Schiff-base ligand
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1718
_journal_page_last               1722
_journal_paper_doi               10.1039/D0CE01826K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C28 H24 Cl3 Dy N2 O5'
_chemical_formula_sum            'C28 H24 Cl3 Dy N2 O5'
_chemical_formula_weight         737.34
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-19 deposited with the CCDC.	2021-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                101.510(3)
_cell_angle_beta                 90.312(3)
_cell_angle_gamma                97.846(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0382(3)
_cell_length_b                   12.2095(4)
_cell_length_c                   14.6675(6)
_cell_measurement_reflns_used    13103
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0500
_cell_measurement_theta_min      1.9970
_cell_volume                     1396.56(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_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   -115.00  65.00   0.25    5.00    --  -25.00  45.00   0.00  720
  2  \w   -115.00  65.00   0.25    5.00    --  -25.00  45.00  90.00  720
  3  \w   -115.00  65.00   0.25    5.00    --  -25.00  45.00 180.00  720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0484328000
_diffrn_orient_matrix_UB_12      -0.0119670000
_diffrn_orient_matrix_UB_13      0.0380128000
_diffrn_orient_matrix_UB_21      0.0329329000
_diffrn_orient_matrix_UB_22      0.0536408000
_diffrn_orient_matrix_UB_23      0.0269018000
_diffrn_orient_matrix_UB_31      -0.0671787000
_diffrn_orient_matrix_UB_32      0.0237691000
_diffrn_orient_matrix_UB_33      -0.0164223000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.866
_diffrn_reflns_theta_min         1.719
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_refine_diff_density_max         2.127
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         9384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7459
_reflns_number_total             9384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01826k2.cif
_cod_data_source_block           r20200101d
_cod_depositor_comments
'Adding full bibliography for 7242160--7242161.cif.'
_cod_original_cell_volume        1396.57(9)
_cod_database_code               7242160
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 90.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N10(H10), N9(H9), C10(H10a), C15(H15), C19(H19), C23(H23), C25(H25), C30(H30),
  C42(H42), C44(H44), C46(H46), C52(H52), C53(H53), C55(H55), C59(H59),
 C61(H61), C64(H64), C67(H67)
2.b Idealised Me refined as rotating group:
 C49(H49a,H49b,H49c), C65(H65a,H65b,H65c)
;
_shelx_res_checksum              79282
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.804