Lanthanide(III) Dodecanuclear Structure with Acylyhydrazone Schiff-base Ligand: Slow Magnetic Relaxation and Magnetocaloric Effects
Wang, Wei; Zhang, Jing; Zhao, Ji-Hai; He, Yuan-Chun; Li, Meng-Ting; Yu, Yang; CrystEngComm  (2020) –; doi:10.1039/D0CE01339K

data_7241359
_publ_section_title
;
 Lanthanide(III) Dodecanuclear Structure with Acylyhydrazone Schiff-base
 Ligand: Slow Magnetic Relaxation and Magnetocaloric Effects
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01339K
_journal_year                    2020
_chemical_formula_moiety         'C114 H101 Dy12 N20 O58'
_chemical_formula_sum            'C114 H101 Dy12 N20 O58'
_chemical_formula_weight         4629.14
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-14 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.142(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8431(4)
_cell_length_b                   44.1352(7)
_cell_length_c                   27.1376(6)
_cell_measurement_reflns_used    48349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7840
_cell_measurement_theta_min      2.4640
_cell_volume                     19277.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.3a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.3a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.3a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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   -105.00  75.00   0.50   10.00    --  -15.00  45.00   0.00  360
  2  \w   -105.00  75.00   0.50   10.00    --  -15.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0029405000
_diffrn_orient_matrix_UB_12      -0.0038912000
_diffrn_orient_matrix_UB_13      -0.0247586000
_diffrn_orient_matrix_UB_21      -0.0056594000
_diffrn_orient_matrix_UB_22      -0.0155050000
_diffrn_orient_matrix_UB_23      0.0050391000
_diffrn_orient_matrix_UB_31      -0.0435965000
_diffrn_orient_matrix_UB_32      0.0017355000
_diffrn_orient_matrix_UB_33      -0.0104408000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            68574
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.571
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86708
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.3a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             8724
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         16740
_refine_ls_number_restraints     804
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0668P)^2^+49.1857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14516
_reflns_number_total             16740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01339k2.cif
_cod_data_source_block           1
_cod_database_code               7241359
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 82.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C33 \\sim C28 \\sim C52 \\sim C29 \\sim C50 \\sim C34 \\sim C14 \\sim C9 \\sim
C35 \\sim C20 \\sim C32 \\sim C31 \\sim C15 \\sim C44 \\sim C41 \\sim C13 \\sim
C46 \\sim C12 \\sim C49 \\sim C25 \\sim C30 \\sim C26 \\sim C22 \\sim C36 \\sim
C11 \\sim C21 \\sim C27 \\sim C10 \\sim C025 \\sim C48 \\sim C42 \\sim C8 \\sim
C19 \\sim C16 \\sim C54 \\sim C7 \\sim C3 \\sim C6 \\sim C23 \\sim C56 \\sim C4
\\sim C55 \\sim C2 \\sim C5 \\sim C1 \\sim C24 \\sim C53 \\sim C57 \\sim C47
\\sim C43 \\sim C40 \\sim C18 \\sim C39 \\sim C37 \\sim C51 \\sim C17 \\sim C38
\\sim C45: within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H49A(0.5) H49B(0.5) H49C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N9(H9), N4(H4), C14(H14), C35(H35), C32(H32), C31(H31), C12(H12), C25(H25),
 C30(H30), C22(H22), C11(H11), C27(H27), C10(H10), C19(H19), C16(H16), C7(H7),
 C3(H3), C23(H23), C4(H4A), C2(H2), C5(H5), C24(H24), C40(H40), C18(H18),
 C39(H39), C37(H37), C17(H17), C38(H38)
4.b Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C55(H55A,H55B,H55C), C53(H53A,H53B,H53C), C57(H57A,H57B,
 H57C), C47(H47A,H47B,H47C), C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              6845
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.180
_oxdiff_exptl_absorpt_empirical_full_min 0.878