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_7710252
_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 Ce N4 O14 Zn2, 2(N O3), C H4 O, 2(C H4 O)'
_chemical_formula_sum            'C65 H71 Ce N6 O23 Zn2'
_chemical_formula_weight         1575.18
_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             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                86.0000(10)
_cell_angle_beta                 87.6080(10)
_cell_angle_gamma                61.616(6)
_cell_formula_units_Z            2
_cell_length_a                   12.693(3)
_cell_length_b                   13.251(3)
_cell_length_c                   21.930(6)
_cell_measurement_reflns_used    10243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      3.1
_cell_volume                     3237.0(14)
_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      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku saturn 724 + mode (4*4 bin mode)'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44546
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.069
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   numerical
_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    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         14085
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0170P)^2^+5.6982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11875
_reflns_number_total             14085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00926a2.cif
_cod_data_source_block           Zn2Ce
_cod_database_code               7710252
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Restrained distances
 O13-H13A
 0.87 with sigma of 0.01
 O33-H33A
 0.87 with sigma of 0.01
 O53-H53A
 0.87 with sigma of 0.01
 O73-H73A
 0.87 with sigma of 0.01
 C24-H13A
 1.923908 with sigma of 0.02
 Zn1-H13A
 2.91996 with sigma of 0.02
 C44-H33A
 1.9237 with sigma of 0.02
 Zn1-H33A
 2.915748 with sigma of 0.02
 C64-H53A
 1.91807 with sigma of 0.02
 Zn2-H53A
 2.859133 with sigma of 0.02
 C84-H73A
 1.914527 with sigma of 0.02
 Zn2-H73A
 2.946129 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C1S \\sim O1S: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C44(H44A,H44B), C64(H64A,H64B), C84(H84A,H84B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C17(H17), C19(H19), C20(H20), C21(H21),
 C22(H22), C32(H32), C33(H33), C34(H34), C37(H37), C39(H39), C40(H40), C41(H41),
  C42(H42), C52(H52), C53(H53), C54(H54), C57(H57), C59(H59), C60(H60),
 C61(H61), C62(H62), C72(H72), C73(H73), C74(H74), C77(H77), C79(H79), C80(H80),
  C81(H81), C82(H82)
3.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C65(H65A,H65B,H65C), C85(H85A,H85B,
 H85C), C92(H92A,H92B,H92C), C1S(H1SA,H1SB,H1SC)
3.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 67 electrons were 
found in a volume of 306\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[CH4O] per Formula Unit 
which account for 72 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91917
_shelx_hkl_checksum              90992
_shelx_fab_checksum              73218
_olex2_submission_special_instructions 'No special instructions were received'