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_7245389
_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         'C152 H136 Dy2 N34 O12, 2(C6 H15 N)'
_chemical_formula_sum            'C164 H166 Dy2 N36 O12'
_chemical_formula_weight         3158.32
_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     dual
_audit_creation_date             2022-01-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.510(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.329(3)
_cell_length_b                   16.6830(14)
_cell_length_c                   30.194(2)
_cell_measurement_reflns_used    7078
_cell_measurement_temperature    180.00
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.32
_cell_volume                     17229(2)
_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      180.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1414
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            66146
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.177
_diffrn_reflns_theta_max         25.177
_diffrn_reflns_theta_min         2.047
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0904 before and 0.0753 after correction.
The Ratio of minimum to maximum transmission is 0.7530.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             6520
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.856
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         15339
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+140.4843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8461
_reflns_number_total             15339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01067d2.cif
_cod_data_source_block           1
_cod_original_cell_volume        17228(2)
_cod_database_code               7245389
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C81-C5
 1.5 with sigma of 0.02
 O6-N18
 3.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C65 \\sim C37 \\sim C39 \\sim C77 \\sim C19 \\sim C73: within 3.8A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 3.8A
C64 \\sim C74 \\sim C35 \\sim C9 \\sim C69 \\sim C79 \\sim C55 \\sim C21:
within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.01 within 3.8A
N1 \\sim C81 \\sim C5: within 3.8A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 3.8A
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C33(H33A,H33B), C67(H67A,H67B)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N3(H3), N13(H13), N14(H14), C20(H20), C30(H30), C34(H34), C40(H40),
 C44(H44), C48(H48), C60(H60), C62(H62), C66(H66), C70(H70), C72(H72), C76(H76),
  C78(H78), C80(H80), C82(H82), C41(H41), C21(H21), C43(H43), C11(H11),
 C45(H45), C49(H49), C25(H25), C51(H51), C13(H13A), C27(H27), C55(H55), C7(H7),
 C59(H59), C31(H31), C35(H35), C9(H9), C73(H73), C37(H37), C19(H19), C77(H77),
 C39(H39)
3.c Tetrahedral OH refined with riding coordinates:
 O6(H6)
3.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C3(H3A,H3B,H3C), C53(H53A,H53B,H53C), C57(H57A,H57B,
 H57C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C2(H2A,H2B,H2C), C17(H17A,
 H17B,H17C), C71(H71A,H71B,H71C), C75(H75A,H75B,H75C), C79(H79A,H79B,H79C),
 C5(H5A,H5B,H5C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 286 electrons were 
found in a volume of 3400\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[CH3CN] per Asymmetric Unit 
which account for 264 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16346
_shelx_hkl_checksum              61885
_shelx_fab_checksum              84580
_olex2_submission_special_instructions 'No special instructions were received'