Bis-pyrazolone-based dysprosium(III) complexes: zero-field single-molecule magnet behavior in the [2 × 2] grid DyIII4 cluster
Ashebr, Tesfay; Li, Xiao-Lei; Zhao, Chen; Yang, Qianqian; Tang, Jinkui; CrystEngComm  (2022) –; doi:10.1039/D2CE01067D

data_7245388
_publ_section_title
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 Bis-pyrazolone-based dysprosium(III) complexes: zero-field
 single-molecule magnet behavior in the [2 \\times 2] grid DyIII4 cluster
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01067D
_journal_year                    2022
_chemical_formula_moiety         'C100 H100 Dy4 N34 O14, 2(C H4 O)'
_chemical_formula_sum            'C102 H108 Dy4 N34 O16'
_chemical_formula_weight         2716.22
_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   mixed
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.894(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8689(16)
_cell_length_b                   31.487(3)
_cell_length_c                   21.8015(16)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      2.26
_cell_volume                     12164.1(18)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            116732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.384
_diffrn_reflns_theta_min         1.981
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.500
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0836 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.8335.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.024
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.055
_refine_diff_density_min         -4.122
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         16372
_refine_ls_number_restraints     795
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.2100
_refine_ls_R_factor_gt           0.1410
_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^)+(0.1307P)^2^+1146.8345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3459
_refine_ls_wR_factor_ref         0.4093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9324
_reflns_number_total             16372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01067d2.cif
_cod_data_source_block           lix_sq
_cod_original_cell_volume        12164.2(17)
_cod_database_code               7245388
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C3 \\sim C11 \\sim C23 \\sim C45 \\sim C47 \\sim C49: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3.8A
2. Rigid body (RIGU) restrains
 Dy1, Dy2, O1, O2, O3, O9, O5, O6, O7, N1, N2, N3, O4, N5, N6, N7, N8, N9, N10,
  N11, N12, N13, N14, N15, N16, N17, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10,
 C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C26, C27,
  C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39, C40, C41, C42,
 C43, C44, C45, C46, C47, C48, C49, C50, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Everything fixed:
 O2, H2, O7, H7, O8, H8
3.b Riding coordinates:
 C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C42(H42A,H42B,
 H42C)
3.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N14(H14), N15(H15), C2(H2A), C11(H11), C45(H45), C23(H23),
 C47(H47), C49(H49), C22(H22), C27(H27), C33(H33), C35(H35), C19(H19), C39(H39),
  C5(H5A), C41(H41), C21(H21), C44(H44), C46(H46), C48(H48), C51(H51), C13(H13)
3.d Fitted hexagon refined as free rotating group:
 C11(C45,C23,C47,C3,C49), C37(C19,C39,C5,C41,C21), C44(C46,C48,C50,C51,C13)
3.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C43(H43A,H43B,
 H43C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              22210
_shelx_hkl_checksum              35313
_shelx_fab_checksum              33135
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'