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_7710255
_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 Sm Zn2, 2(N O3), 2(C H3 O H), 2(H2 O)'
_chemical_formula_sum            'C64 H71 N6 O24 Sm Zn2'
_chemical_formula_weight         1589.51
_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                85.982(6)
_cell_angle_beta                 87.403(5)
_cell_angle_gamma                61.234(9)
_cell_formula_units_Z            2
_cell_length_a                   12.7211(10)
_cell_length_b                   13.1975(11)
_cell_length_c                   21.9778(12)
_cell_measurement_reflns_used    7800
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.1780
_cell_measurement_theta_min      1.7600
_cell_volume                     3226.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -349.73  10.27   0.50    3.00   6.61  -9.84 -31.50    --   720
  2  \w    -60.89   0.11   0.50    3.00    --  -14.77  94.56 -34.84  122
  3  \w    -65.46   0.04   0.50    3.00    --  -19.34  94.56 145.16  131
  4  \w   -100.81  15.69   0.50    3.00    --   -9.84 -59.25 164.08  233
  5  \w    -65.46   0.04   0.50    3.00    --  -19.34  94.56  73.16  131
  6  \f    -10.27 349.73   0.50    3.00  81.02  -9.84  31.50    --   720
  7  \w    -65.46   0.04   0.50    3.00    --  -19.34  94.56   1.16  131
  8  \w   -100.81  15.69   0.50    3.00    --   -9.84 -59.25 -51.92  233
  9  \f   -339.92  20.08   0.50    3.00  15.81  -9.84 -59.25    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0062918000
_diffrn_orient_matrix_UB_12      0.0559147000
_diffrn_orient_matrix_UB_13      -0.0070269000
_diffrn_orient_matrix_UB_21      0.0571230000
_diffrn_orient_matrix_UB_22      -0.0182000000
_diffrn_orient_matrix_UB_23      0.0125809000
_diffrn_orient_matrix_UB_31      0.0272756000
_diffrn_orient_matrix_UB_32      -0.0176870000
_diffrn_orient_matrix_UB_33      -0.0289697000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1933
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            141092
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.763
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         11347
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7632
_reflns_number_total             11347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00926a2.cif
_cod_data_source_block           Zn2Sm
_cod_database_code               7710255
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Sm Zn'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Restrained distances
 O13-H13
 0.87 with sigma of 0.01
 O00H-H00H
 0.87 with sigma of 0.01
 C24-H13
 1.923631 with sigma of 0.02
 Zn1-H13
 2.937036 with sigma of 0.02
 C01W-H00H
 1.918062 with sigma of 0.02
 Zn2-H00H
 2.973499 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C01W(H01E,H01G), C64(H64A,H64B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C00Z(H00Z), C017(H017), C37(H37), C14(H14), C01A(H01A), C57(H57),
 C01F(H01F), C52(H52), C41(H41), C12(H12), C34(H34), C32(H32), C54(H54),
 C39(H39), C42(H42), C01Q(H01Q), C33(H33A), C19(H19), C40(H40), C01Z(H01Z),
 C22(H22), C53(H53A), C13(H13A), C20(H20), C61(H61), C027(H027), C028(H028),
 C62(H62), C21(H21), C60(H60), C59(H59)
2.c Idealised Me refined as rotating group:
 C01S(H01B,H01C,H01D), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C65(H65A,H65B,
 H65C), C91(H91A,H91B,H91C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 117 electrons were 
found in a volume of 424\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1.5[CH4O, H2O], 0.5[CH4O, H2O] per Formula Unit 
which account for 112 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18150
_shelx_hkl_checksum              19686
_shelx_fab_checksum              37888
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.406
_oxdiff_exptl_absorpt_empirical_full_min 0.405