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_7710253
_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 H57 Dy N4 O14 Zn2, 2(N O3), 1.5(H2 O), 1[CH4O]'
_chemical_formula_sum            'C63 H64 Dy N6 O22.5 Zn2'
_chemical_formula_weight         1558.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 111.889(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6246(16)
_cell_length_b                   12.9505(6)
_cell_length_c                   24.2392(15)
_cell_measurement_reflns_used    8682
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.5280
_cell_measurement_theta_min      1.8860
_cell_volume                     6590.1(8)
_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_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -1.73 182.27   0.50    2.00   6.61  -9.84 -31.50    --   368
  2  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25  92.08  233
  3  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25-123.92  233
  4  \f   -130.56  85.44   0.50    2.00  81.02  -9.84  31.50    --   432
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56161
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.848
_exptl_absorpt_coefficient_mu    1.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61507
_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    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5801
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0847P)^2^+12.7352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4591
_reflns_number_total             5801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00926a2.cif
_cod_data_source_block           zn2dy
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Yellow' was changed
to 'yellow' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C63 H64 Dy N6 O22.50 Zn2'
_cod_database_code               7710253
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Restrained distances
 O13-H13
 0.87 with sigma of 0.01
 C4-H13
 1.91458 with sigma of 0.02
 Zn1-H13
 2.992945 with sigma of 0.02
 O103-O104 \\sim O2-O3
 with sigma of 0.04
 N101-O103 \\sim N1-O2
 with sigma of 0.02
 O104-O102 \\sim O3-O1
 with sigma of 0.04
 O103-O102 \\sim O2-O1
 with sigma of 0.04
 N101-O102 \\sim N1-O1
 with sigma of 0.02
 N101-O104 \\sim N1-O3
 with sigma of 0.02
2. Restrained planarity
 O1, N1, O2, O3
 with sigma of 0.001
3. Others
 Fixed Sof: H92A(0.5) H92B(0.5) H92C(0.5) N101(0.75) O103(0.75) O104(0.75)
 O102(0.75) O1(0.25) N1(0.25) O2(0.25) O3(0.25) O4(0.25) H4C(0.25) H4D(0.25)
 O5(0.25) H5A(0.25) H5B(0.25) O6(0.25) H6A(0.25) H6B(0.25)
 Fixed Uiso: O1(0.12) N1(0.12) O2(0.12) O3(0.12)
4.a Riding coordinates:
 O4(H4C,H4D), O5(H5A,H5B), O6(H6A,H6B)
4.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C12(H12), C32(H32), C39(H39), C17(H17), C42(H42), C14(H14),
 C13(H13A), C2(H2), C34(H34), C40(H40), C19(H19), C41(H41), C33(H33), C1(H1),
 C20(H20)
4.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C92(H92A,H92B,H92C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 72 electrons were 
found in a volume of 272\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[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              15013
_shelx_hkl_checksum              31102
_shelx_fab_checksum              80877
_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
;