Synthesis, Structures and Magnetic studies of Hexanuclear Lanthanide Complexes: SMM behavior in DyIII analogue and MCE properties in the GdIII analogue
Kumar, Pawan; Kalita, Pankaj; Palacios, Maria A.; Kumar, Vierandra; Acharya, Joydev; Colacio, Enrique; Chandrasekhar, Vadapalli; Dalton Transactions  (2023) –; doi:10.1039/D3DT01489D

data_7713411
_publ_section_title
;
 Synthesis, Structures and Magnetic studies of Hexanuclear Lanthanide
 Complexes: SMM behavior in DyIII analogue and MCE properties in the GdIII
 analogue
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01489D
_journal_year                    2023
_chemical_formula_moiety
'C92 H96 F12 N16 O26 Tb6, 2(N O3), 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C94 H108 F12 N18 O36 Tb6'
_chemical_formula_weight         3247.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-19 deposited with the CCDC.	2023-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.002(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8617(3)
_cell_length_b                   20.3171(4)
_cell_length_c                   19.5374(4)
_cell_measurement_reflns_used    30897
_cell_measurement_temperature    219.99(10)
_cell_measurement_theta_max      28.6550
_cell_measurement_theta_min      2.7580
_cell_volume                     5841.8(2)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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      219.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.898
_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    -41.00 -16.00   0.50  101.11    --    7.10 -38.00 114.00   50
  2  \w     25.00  50.00   0.50  101.11    --    7.10  38.00 -90.00   50
  3  \w     16.00  41.00   0.50  101.11    --   -7.50  38.00 -90.00   50
  4  \w    -32.00  -7.00   0.50  101.11    --   -7.50 -38.00 114.00   50
  5  \w     65.00  95.00   0.50  101.11    --    7.10  77.00 150.00   60
  6  \w     51.00  83.00   0.50  101.11    --    7.10  77.00 -60.00   64
  7  \w     50.00  95.00   0.50  101.11    --    7.10  77.00  90.00   90
  8  \w    -33.00  90.00   0.50  101.11    --    7.10  38.00  90.00  246
  9  \w    -31.00  20.00   0.50  101.11    --   -7.50 -82.00   0.00  102
 10  \w    -46.00 -20.00   0.50  101.11    --   -7.50 -82.00-150.00   52
 11  \w     -8.00  33.00   0.50  101.11    --   -7.50 -82.00  90.00   82
 12  \w    -47.00 -22.00   0.50  101.11    --   -7.50 -82.00  90.00   50
;
_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      0.0176495000
_diffrn_orient_matrix_UB_12      -0.0161394000
_diffrn_orient_matrix_UB_13      -0.0274576000
_diffrn_orient_matrix_UB_21      0.0425745000
_diffrn_orient_matrix_UB_22      -0.0034779000
_diffrn_orient_matrix_UB_23      0.0211086000
_diffrn_orient_matrix_UB_31      -0.0140706000
_diffrn_orient_matrix_UB_32      -0.0307677000
_diffrn_orient_matrix_UB_33      0.0120162000
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.922
_diffrn_reflns_theta_min         2.558
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73778
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.671
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         13851
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0449P)^2^+28.3292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11016
_reflns_number_total             13851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01489d2.cif
_cod_data_source_block           aj1920
_cod_database_code               7713411
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O F Tb '
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.666
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C1A-F3 \\sim C1A-F4 \\sim C1A-F5
 with sigma of 0.02
 C1C-F7 \\sim C1C-F8 \\sim C1C-F9
 with sigma of 0.02
 C1D-F10 \\sim C1D-F11 \\sim C1D-F12
 with sigma of 0.02
 C1B-F1 \\sim C1B-F2 \\sim C1B-F6
 with sigma of 0.02
 F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.03
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.03
 F1-F2 \\sim F2-F6 \\sim F6-F1
 with sigma of 0.03
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.03
3. Rigid body (RIGU) restrains
 C1D, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F6, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3, F4, F5, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(F7)=Sof(F8)=Sof(F9)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F6)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=FVAR(2)
5.a Riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,
 H1DC), O18(H18C,H18D)
5.b Rotating group:
 O13(H13A,H13B)
5.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7A), C10(H10), C11(H11), C12(H12),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C28(H28), C29(H29), C30(H30),
  C38(H38), C41(H41)
5.e Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
5.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7), O17(H17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53891
_shelx_hkl_checksum              40784
_shelx_fab_checksum              14675
_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 1.502
_oxdiff_exptl_absorpt_empirical_full_min 0.709