Dinuclear and trinuclear cyano-bridged {DyIIIMIV} (M = W, Mo) single-ion magnets supported by pentadentate Schiff-base ligands
Mao, Pan-Dong; Sun, Hui-Ying; Yan, Fei-Fei; Zhang, Shi-Hui; Li, Xin-Feng; Zhou, Ren-He; Zhang, Yi-Quan; Meng, Yin-Shan; Liu, Tao; CrystEngComm 25 (2023) 6030–6038; doi:10.1039/D3CE00720K

data_7247418
_publ_section_title
;
 Dinuclear and trinuclear cyano-bridged {DyIIIMIV} (M = W, Mo) single-ion
 magnets supported by pentadentate Schiff-base ligands
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6030
_journal_page_last               6038
_journal_paper_doi               10.1039/D3CE00720K
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C49.108 H48 Dy2 N21.108 O10 W, 0.892(C N), 8(H2 O)'
_chemical_formula_sum            'C50 H64 Dy2 N22 O18 W'
_chemical_formula_weight         1770.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-11
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.820(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0713(11)
_cell_length_b                   9.5260(3)
_cell_length_c                   24.0085(10)
_cell_measurement_reflns_used    8081
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      29.9120
_cell_measurement_theta_min      2.3080
_cell_volume                     6177.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.887
_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    -78.00  47.00   0.50   12.50    --    8.80 -77.00 150.00  250
  2  \w     22.00  53.00   0.50   12.50    --   -8.90  57.00 -60.00   62
  3  \w    -17.00  10.00   0.50   12.50    --   -8.90 -77.00-180.00   54
  4  \w    -38.00 -13.00   0.50   12.50    --   -8.90  57.00 -60.00   50
  5  \w     -3.00  64.00   0.50   12.50    --   -8.90  82.00-180.00  134
  6  \w    -45.00 -16.00   0.50   12.50    --   -8.90  82.00-180.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25571
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.979
_diffrn_reflns_theta_min         2.404
_exptl_absorpt_coefficient_mu    4.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic orangish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       plate
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7986
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0269P)^2^+30.3141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6002
_reflns_number_total             7986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00720k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7247418--7247421.cif.'
_cod_database_code               7247418
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.647
_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, All O(H,H) groups
2. Restrained distances
 H19B_$1-H7A
 2.1 with sigma of 0.02
 H7A-H8B
 2.2 with sigma of 0.02
 H4A-H6C
 2.2 with sigma of 0.02
 H8B-H9A
 2.2 with sigma of 0.02
 H7A-H19B_$1
 2.3 with sigma of 0.02
 C3-W1
 2.2 with sigma of 0.02
 H7A-H24_$2
 2.2 with sigma of 0.02
 H7B-O7
 0.9 with sigma of 0.01
 H7A-O7
 0.9 with sigma of 0.01
 Dy1-H5A \\sim Dy1-H5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C2A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N1A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C2, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C2A, N2, N2A, W1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C1A, N1, N1A, W1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3A, N3A, C3, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C2)=Sof(N2)=Sof(C3)=Sof(N3)=1-FVAR(1)
 Sof(C2A)=Sof(C3A)=Sof(N2A)=Sof(N3A)=FVAR(1)
 Sof(C1A)=Sof(N1A)=1-FVAR(2)
 Sof(C1)=Sof(N1)=FVAR(2)
6.a Riding coordinates:
 O8(H8A,H8B), O6(H6B,H6C), O9(H9A,H9B)
6.b Free rotating group:
 O5(H5A,H5B)
6.c Rotating group:
 O2(H2A,H2B), O4(H4A,H4B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C22(H22),
 C23(H23), C24(H24), C25(H25), N6(H6A)
6.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              82647
_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
;