Exchange-driven slow relaxation of magnetization in NiII2LnIII2 (LnIII = Y, Gd, Tb and Dy) butterfly complexes: experimental and theoretical studies
Chakraborty, Amit; Ahmed, Naushad; Ali, Junaid; Moorthy, Shruti; Goura, Joydeb; Singh, Saurabh Kumar; Rogez, Guillaume; Chandrasekhar, Vadapalli; Dalton Transactions  (2022) –; doi:10.1039/D2DT00237J

data_7711255
_publ_section_title
;
 Exchange-driven slow relaxation of magnetization in NiII2LnIII2 (LnIII =
 Y, Gd, Tb and Dy) butterfly complexes: experimental and theoretical
 studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00237J
_journal_year                    2022
_chemical_formula_moiety         'C54 H56 N6 Ni2 O18 Y2'
_chemical_formula_sum            'C54 H56 N6 Ni2 O18 Y2'
_chemical_formula_weight         1372.25
_chemical_melting_point          195
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-07 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0051(7)
_cell_length_b                   24.3858(10)
_cell_length_c                   14.8468(8)
_cell_measurement_reflns_used    13320
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3310
_cell_measurement_theta_min      2.7070
_cell_volume                     5432.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -61.00 -34.00   0.50   15.39    --    7.20  15.00 166.00   54
  2  \w     -9.00  17.00   0.50   15.39    --   -7.60 -15.00  -3.00   52
  3  \w     50.00  75.00   0.50   15.39    --    7.20  77.00   0.00   50
  4  \w     12.00  95.00   0.50   15.39    --    7.20  57.00-120.00  166
  5  \w     51.00  89.00   0.50   15.39    --    7.20  77.00 -90.00   76
  6  \w    -20.00  96.00   0.50   15.39    --    7.20  57.00-180.00  232
  7  \w     18.00  75.00   0.50   15.39    --   -7.60  57.00-150.00  114
  8  \w    -16.00  32.00   0.50   15.39    --   -7.60 -77.00 -90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0135914000
_diffrn_orient_matrix_UB_12      0.0278361000
_diffrn_orient_matrix_UB_13      0.0014654000
_diffrn_orient_matrix_UB_21      0.0445035000
_diffrn_orient_matrix_UB_22      0.0080604000
_diffrn_orient_matrix_UB_23      0.0089597000
_diffrn_orient_matrix_UB_31      0.0080749000
_diffrn_orient_matrix_UB_32      0.0024270000
_diffrn_orient_matrix_UB_33      -0.0469541000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1332
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            59843
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.031
_diffrn_reflns_theta_min         2.715
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6699
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+2.2896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4617
_reflns_number_total             6699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00237j2.cif
_cod_data_source_block           aj1340
_cod_database_code               7711255
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHNONiY
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 C27-H9
 1.865353 with sigma of 0.02
 Ni1-H9
 2.58246 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C17(H17), C11(H11), C3(H3), C4(H4), C14(H14), C21(H21),
 C12(H12), C19(H19), C20(H20), C13(H13)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C00T(H00A,H00B,H00C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              10374
_shelx_hkl_checksum              62416
_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 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.680