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_7713410
_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         'C94 H100 Er6 F12 N16 O26, 2(N O3), 2(C H4 O)'
_chemical_formula_sum            'C96 H108 Er6 F12 N18 O34'
_chemical_formula_weight         3289.56
_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                 97.575(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8051(4)
_cell_length_b                   20.1675(5)
_cell_length_c                   19.4036(5)
_cell_measurement_reflns_used    20294
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.8700
_cell_measurement_theta_min      2.6180
_cell_volume                     5743.0(3)
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.886
_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    -23.00  93.00   0.50   72.24    --    7.10  57.00  60.00  232
  2  \w     51.00  93.00   0.50   72.24    --    7.10  77.00-120.00   84
  3  \w     63.00  96.00   0.50   72.24    --    7.10  77.00 150.00   66
  4  \w    -36.00   5.00   0.50   72.24    --   -7.50  57.00-120.00   82
  5  \w    -96.00 -33.00   0.50   72.24    --   -7.50 -19.00-150.00  126
  6  \w    -10.00  30.00   0.50   72.24    --   -7.50 -19.00-150.00   80
  7  \w     19.00  44.00   0.50   72.24    --   -7.50  57.00-120.00   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      -0.0470605000
_diffrn_orient_matrix_UB_12      0.0017940000
_diffrn_orient_matrix_UB_13      -0.0128440000
_diffrn_orient_matrix_UB_21      0.0027623000
_diffrn_orient_matrix_UB_22      -0.0311774000
_diffrn_orient_matrix_UB_23      -0.0165098000
_diffrn_orient_matrix_UB_31      -0.0106206000
_diffrn_orient_matrix_UB_32      -0.0161497000
_diffrn_orient_matrix_UB_33      0.0303970000
_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  0.0481
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56351
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.942
_diffrn_reflns_theta_min         2.580
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.438
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60586
_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    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.521
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         13457
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0598P)^2^+99.3054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9918
_reflns_number_total             13457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01489d2.cif
_cod_data_source_block           aj1860
_cod_database_code               7713410
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFEr
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.556
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O17-C44
 1.43 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
 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
 F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.03
 F7-F8 \\sim F8-F9 \\sim F9-F7
 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
 O13-C43 \\sim O13-C43A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F3 \\sim F4 \\sim F5 \\sim C1A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.002 within 1.7A
F7 \\sim F8 \\sim F9 \\sim C1C: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.002 within 1.7A
F10 \\sim F11 \\sim F12 \\sim C1D: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.002 within 1.7A
Uanis(C43) = Uanis(C43A)
4. Rigid body (RIGU) restrains
 F3, F4, F5, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10, F11, F12, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F8, F9, C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F6)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=FVAR(2)
 Sof(H13A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(3)
 Sof(H13)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(3)
6.a Riding coordinates:
 O13(H13A), O13(H13), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,
 H1CC), C1D(H1DA,H1DB,H1DC)
6.b 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)
6.c 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)
6.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C43A(H43D,H43E,H43F), C44(H44A,H44B,H44C)
6.e Idealised tetrahedral OH refined as rotating group:
 O7(H7), O17(H17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54791
_shelx_hkl_checksum              55000
_shelx_fab_checksum              63034
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.617