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_7247420
_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
'C29 H26 Dy Mo N15 O5, 2(C O), 6(H2 O), H O, 2.5(O)'
_chemical_formula_sum            'C31 H39 Dy Mo N15 O16.5'
_chemical_formula_weight         1144.21
_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
_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                92.524(2)
_cell_angle_beta                 95.871(2)
_cell_angle_gamma                108.109(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5532(9)
_cell_length_b                   11.6027(10)
_cell_length_c                   18.7684(16)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.28
_cell_volume                     2165.8(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SIR2004  (Burla et al.,  2007)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55238
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         2.226
_exptl_absorpt_coefficient_mu    2.088
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0869 before and 0.0541 after correction. The Ratio of minimum to maximum transmission is 0.8635. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic orangish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.119
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9861
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0320P)^2^+9.0784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8629
_reflns_number_total             9861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00720k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7247418--7247421.cif.'
_cod_original_formula_sum        'C31 H39 Dy Mo N15 O16.50'
_cod_database_code               7247420
_shelx_shelxl_version_number     2018/3
_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) groups, All O(H,H) groups
2. Restrained distances
 C30-O6
 1.42 with sigma of 0.02
 O18-O18_$2
 3 with sigma of 0.02
 O18_$2-O18
 2.6 with sigma of 0.02
 O14_$3-O18
 2.6 with sigma of 0.02
 O6-O18
 3 with sigma of 0.02
 O18-O14_$3
 2.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O12)=Sof(H12A)=Sof(H12B)=1-FVAR(1)
 Sof(O13)=Sof(H13A)=Sof(H13B)=FVAR(1)
 Fixed Sof: O14(0.5)
6.a Everything fixed:
 H20A, H9B, H9C
6.b Free rotating group:
 O10(H10B,H10C), O21(H21A,H21B), O15(H15A,H15B), O11(H11A,H11B), O12(H12A,
 H12B), O13(H13A,H13B)
6.c Rotating group:
 O2(H2A,H2B), O4(H4A,H4B), O5(H5A,H5B)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C18(H18), C19(H19), C20(H20), C26(H26),
 C27(H27), C28(H28), C29(H29), N9(H9A), N10(H10A), N15(H15)
6.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              29103
_olex2_submission_special_instructions 'No special instructions were received'