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_7247419
_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
'C49.259 H48 Dy2 Mo N21.259 O10, 0.741(C N), 8(H2 O)'
_chemical_formula_sum            'C50 H64 Dy2 Mo N22 O18'
_chemical_formula_weight         1682.17
_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                 93.714(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9939(9)
_cell_length_b                   9.5351(3)
_cell_length_c                   24.0996(7)
_cell_measurement_reflns_used    7846
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      26.3630
_cell_measurement_theta_min      1.7340
_cell_volume                     6190.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (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    '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 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -10.27 349.73   0.50    8.00  74.14 -16.73  31.50    --   720
  2  \w    -67.05  21.45   0.50    8.00    --  -16.77  84.99  39.90  177
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8872
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.196
_exptl_absorpt_coefficient_mu    2.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       plate
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.766
_refine_diff_density_min         -2.249
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8872
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0547P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5251
_reflns_number_total             8872
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9877\% 
around [-0.07 0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
;
_cod_data_source_file            d3ce00720k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7247418--7247421.cif.'
_cod_database_code               7247419
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7575(7)
 0.2425(7)
2. 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
3. Restrained distances
 Dy1-H5A \\sim Dy1-H5B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2A) \\sim Ueq,
Uanis(N2A) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C1, C1A, C2, C2A, C3, Mo1, N1, N1A, N2, N2A, N3, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(C2A)=Sof(N1A)=Sof(N2A)=Sof(C3A)=Sof(N3A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(N1)=Sof(N2)=Sof(N3)=FVAR(1)
7.a Riding coordinates:
 O4(H4A,H4B), O9(H9A,H9B)
7.b Free rotating group:
 O5(H5A,H5B), O6(H6B,H6C), O7(H7A,H7B), O8(H8A,H8B)
7.c Rotating group:
 O2(H2B,H2A)
7.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)
7.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              25129
_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
;