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_7713412
_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 Dy6 F12 N16 O26, 2(N O3), 2(C H4 O)'
_chemical_formula_sum            'C96 H108 Dy6 F12 N18 O34'
_chemical_formula_weight         3261.00
_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     iterative
_audit_creation_date             2023-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-19 deposited with the CCDC.	2023-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.266(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9080(4)
_cell_length_b                   20.2610(6)
_cell_length_c                   19.5143(6)
_cell_measurement_reflns_used    21082
_cell_measurement_temperature    119.98(10)
_cell_measurement_theta_max      29.0520
_cell_measurement_theta_min      2.8740
_cell_volume                     5833.1(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 (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_environment      N~2~
_diffrn_ambient_temperature      119.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.879
_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     57.00  96.00   0.50   15.00    --    7.10  77.00  90.00   78
  2  \w     50.00  94.00   0.50   15.00    --    7.10  77.00-180.00   88
  3  \w    -17.00  44.00   0.50   15.00    --    7.10 -38.00  90.00  122
  4  \w    -82.00 -33.00   0.50   15.00    --    7.10 -38.00  90.00   98
  5  \w    -13.00  33.00   0.50   15.00    --   -7.50 -82.00  30.00   92
  6  \w    -40.00 -15.00   0.50   15.00    --   -7.50 -77.00-150.00   50
  7  \w    -59.00  -9.00   0.50   15.00    --   -7.50 -82.00 -60.00  100
  8  \w     -2.00  31.00   0.50   15.00    --   -7.50 -77.00-150.00   66
;
_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      -0.0189663000
_diffrn_orient_matrix_UB_12      0.0313047000
_diffrn_orient_matrix_UB_13      -0.0098002000
_diffrn_orient_matrix_UB_21      -0.0363271000
_diffrn_orient_matrix_UB_22      -0.0064654000
_diffrn_orient_matrix_UB_23      0.0188498000
_diffrn_orient_matrix_UB_31      0.0251335000
_diffrn_orient_matrix_UB_32      0.0142552000
_diffrn_orient_matrix_UB_33      0.0299782000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56046
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.008
_diffrn_reflns_theta_min         2.682
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43690
_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    1.857
_exptl_crystal_description       block
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.307
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         13654
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0537P)^2^+30.8981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10801
_reflns_number_total             13654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01489d2.cif
_cod_data_source_block           aj1851
_cod_database_code               7713412
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyCHNOF
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.611
_reflns_odcompleteness_completeness 99.66
_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
 C1A-F10 \\sim C1A-F11 \\sim C1A-F12
 with sigma of 0.02
 O13-C43 \\sim O13-C43A
 with sigma of 0.02
 C1D-F1 \\sim C1D-F2 \\sim C1D-F6
 with sigma of 0.02
 C1C-F7 \\sim C1C-F8 \\sim C1C-F9
 with sigma of 0.02
 F1-F2 \\sim F2-F6 \\sim F6-F1
 with sigma of 0.03
 C1B-F3 \\sim C1B-F4 \\sim C1B-F5
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.03
 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
3. Uiso/Uaniso restraints and constraints
O13 \\sim C43: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F7 \\sim F8 \\sim F9 \\sim C1C: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.004
F1 \\sim F2 \\sim F6 \\sim C1D: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.004
F3 \\sim F4 \\sim F5 \\sim C1B: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.004
Uanis(C43A) = Uanis(C43)
4. Rigid body (RIGU) restrains
 O13, C43
 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
 F1, F2, F6, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3, F4, F5, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(H13a)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C43A)=
 Sof(H43d)=Sof(H43e)=Sof(H43f)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(H13)=Sof(H1Ca)=Sof(H1Cb)=Sof(H1Cc)=Sof(C43)=
 Sof(H43a)=Sof(H43b)=Sof(H43c)=FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F6)=Sof(H1Da)=Sof(H1Db)=Sof(H1Dc)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=FVAR(2)
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),
  C41(H41), C38(H38)
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              12987
_shelx_hkl_checksum              69389
_shelx_fab_checksum              98317
_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 1.820
_oxdiff_exptl_absorpt_empirical_full_min 0.695