Zero-Field Slow Magnetic Relaxation Behavior of Zn2Dy in a Family of Trinuclear Near Linear Zn2Ln Complexes: Synthesis, Experimental and Theoretical Investigations
Ahmed, Naushad; Ansari, Kamal Uddin; Dalton Transactions  (2022) –; doi:10.1039/D2DT00926A

data_7710254
_publ_section_title
;
 Zero-Field Slow Magnetic Relaxation Behavior of Zn2Dy in a Family of
 Trinuclear Near Linear Zn2Ln Complexes: Synthesis, Experimental and
 Theoretical Investigations
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00926A
_journal_year                    2022
_chemical_formula_moiety
'C62 H59 N4 O14 Tb Zn2, 2(N O3), 2(C H4 O), 1(C H4 O)'
_chemical_formula_sum            'C65 H71 N6 O23 Tb Zn2'
_chemical_formula_weight         1593.99
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-09 deposited with the CCDC.	2022-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                85.513(4)
_cell_angle_beta                 87.341(4)
_cell_angle_gamma                61.328(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7840(16)
_cell_length_b                   13.1615(17)
_cell_length_c                   22.061(3)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.48
_cell_volume                     3246.6(7)
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            93955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.942
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.83702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         11448
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0344P)^2^+3.7817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9410
_reflns_number_total             11448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00926a2.cif
_cod_data_source_block           Zn2Tb
_cod_database_code               7710254
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.693
_olex2_refinement_description
;
1. Restrained distances
 O53-H53
 0.85 with sigma of 0.01
 O33-H33
 0.85 with sigma of 0.01
 N2-O3 = N2-O5
 1.25 with sigma of 0.02
 N2-O1
 1.24 with sigma of 0.02
 N4-O4
 1.24 with sigma of 0.02
 N4-O2 = N4-O6
 1.25 with sigma of 0.02
 C64-H53
 1.896626 with sigma of 0.02
 C44-H33
 1.882775 with sigma of 0.02
 Zn2-H53
 2.964808 with sigma of 0.02
 Zn1-H33
 3.017247 with sigma of 0.02
 N2-O3 \\sim N2-O1 \\sim N2-O5
 with sigma of 0.02
 O3-O1 \\sim O1-O5 \\sim O5-O3
 with sigma of 0.04
 N2-O5 \\sim N2-O5A
 with sigma of 0.02
 N2-O3 \\sim N2-O3A
 with sigma of 0.02
 N2-O1 \\sim N2-O1A
 with sigma of 0.02
 N4-O2 \\sim N4-O4 \\sim N4-O6
 with sigma of 0.02
 O2-O4 \\sim O4-O6 \\sim O6-O2
 with sigma of 0.04
2. Restrained planarity
 N2, O3, O1, O5
 with sigma of 0.1
 N4, O2, O4, O6
 with sigma of 0.1
3. Rigid bond restraints
 O3, N2, O3A, O1, O1A, O5, O5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N2 \\sim O3 \\sim O1 \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O5A \\sim O3 \\sim O3A \\sim O1 \\sim O1A \\sim O5 \\sim N2: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N4 \\sim O2 \\sim O4 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N2, O3, O1, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5A, O3, N2, O3A, O1, O5, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, O2, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1A)=Sof(O3A)=Sof(O5A)=1-FVAR(1)
 Sof(O3)=Sof(O1)=Sof(O5)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C44(H44A,H44B), C84(H84A,H84B), C64(H64A,H64B)
7.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C20(H20), C19(H19), C17(H17), C14(H14), C13(H13A),
 C12(H12), C42(H42), C41(H41), C40(H40), C39(H39), C37(H37), C32(H32),
 C33(H33A), C34(H34), C52(H52), C53(H53A), C54(H54), C82(H82), C81(H81),
 C80(H80), C79(H79), C77(H77), C72(H72), C73(H73A), C74(H74), C59(H59),
 C60(H60), C61(H61), C62(H62), C57(H57)
7.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C85(H85A,H85B,H85C), C65(H65A,H65B,
 H65C), C92(H92A,H92B,H92C)
7.d Idealised tetrahedral OH refined as rotating group:
 O13(H13), O73(H73)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 105 electrons were 
found in a volume of 427\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 2[CH4O], 1[CH4O] per Formula Unit 
which account for 108 electrons per unit cell.
;
_shelx_res_checksum              30110
_shelx_hkl_checksum              41429
_shelx_fab_checksum              41634
_olex2_submission_special_instructions 'No special instructions were received'