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_7710251
_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 La N4 O14 Zn2, 2(N O3), C H4 O, 2[CH4O], 1[C4H8O]'
_chemical_formula_sum            'C69 H79 La N6 O24 Zn2'
_chemical_formula_weight         1646.07
_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     iterative
_audit_creation_date             2022-04-30
_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                85.739(4)
_cell_angle_beta                 87.260(4)
_cell_angle_gamma                61.849(6)
_cell_formula_units_Z            2
_cell_length_a                   12.6542(8)
_cell_length_b                   13.2334(8)
_cell_length_c                   21.8815(9)
_cell_measurement_reflns_used    17397
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7770
_cell_measurement_theta_min      2.0370
_cell_volume                     3221.5(4)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku saturn 724 mode 4'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42177
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.062
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.80754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          .037
_exptl_crystal_size_mid          .027
_exptl_crystal_size_min          .021
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         13160
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0624P)^2^+2.3727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10431
_reflns_number_total             13160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00926a2.cif
_cod_data_source_block           Zn2La
_cod_database_code               7710251
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 O73-H73
 0.85 with sigma of 0.01
 O33-H33
 0.85 with sigma of 0.01
 O13-H13
 0.85 with sigma of 0.01
 O74-H74
 0.85 with sigma of 0.01
 C84-H73
 1.893005 with sigma of 0.02
 Zn2-H73
 2.837977 with sigma of 0.02
 C44-H33
 1.899201 with sigma of 0.02
 Zn1-H33
 2.891688 with sigma of 0.02
 C24-H13
 1.893238 with sigma of 0.02
 Zn1-H13
 2.892918 with sigma of 0.02
 C64-H74
 1.888406 with sigma of 0.02
 Zn2-H74
 2.914714 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C44(H44A,H44B), C64(H64A,H64B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C54(H54), C37(H37), C13(H13A), C39(H39), C77(H77), C53(H53), C15(H15),
 C17(H17), C40(H40), C14(H14), C55(H55), C73(H73A), C41(H41), C75(H75),
 C20(H20), C81(H81), C22(H22), C79(H79), C80(H80), C19(H19), C35(H35), C61(H61),
  C62(H62), C33(H33A), C82(H82), C74(H74A), C60(H60), C57(H57), C42(H42),
 C34(H34), C21(H21), C59(H59)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C92(H92A,H92B,H92C), C65(H65A,H65B,H65C), C85(H85A,H85B,
 H85C), C45(H45A,H45B,H45C), C1S(H1SA,H1SB,H1SC)
2.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 318\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[CH4O,0.5C4H8O] per Formula Unit 
which account for 156 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2550
_shelx_hkl_checksum              9470
_shelx_fab_checksum              38220
_olex2_submission_special_instructions 'No special instructions were received'