Boosting mono-axial crystal field in stable high-coordinate Dy(III) single-ion magnets by substitution of phenoxy axial ligand
Zhang, Ben; Zhou, Yang; Dong, Chang; Xiang, Yi; Shi, Yanbo; Zhang, Chennan; Yuan, Aihua; Zheng, Shaojun; Li, Zhaoyang; Zhang, Yi-Quan; Yang, Yong; Chen, Lei; Dalton Transactions  (2023) –; doi:10.1039/D3DT01318A

data_7713406
_publ_section_title
;
 Boosting mono-axial crystal field in stable high-coordinate Dy(III)
 single-ion magnets by substitution of phenoxy axial ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01318A
_journal_year                    2023
_chemical_formula_moiety         'C39 H40 Dy N7 O, 2(C24 H20 B), 0.85(C H2 Cl2)'
_chemical_formula_sum            'C87.85 H81.7 B2 Cl1.7 Dy N7 O'
_chemical_formula_weight         1495.989
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-05-22
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.03.24 svn.rc9df729e for OlexSys, GUI svn.r6758)
;
_audit_update_record
;
2023-06-21 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.308(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.136(8)
_cell_length_b                   13.581(5)
_cell_length_c                   27.587(11)
_cell_measurement_reflns_used    18295
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.142
_cell_measurement_theta_min      2.533
_cell_volume                     7542(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            85247
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9989
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             3085.488
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.5451
_refine_diff_density_min         -0.5128
_refine_diff_density_rms         0.0919
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             8.7760
_refine_ls_goodness_of_fit_ref   1.0501
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    153
_refine_ls_number_parameters     912
_refine_ls_number_reflns         14796
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.0498
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+2.1824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                11589
_reflns_number_total             14796
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt01318a2.cif
_cod_data_source_block           '[Dy(BPATPA)(dimethylPhO)]'
_cod_database_code               7713406
_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
2. Rigid bond restraints
 C84, C85
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C84 \\sim C85: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Others
 Fixed Sof: C88(0.85) H88a(0.85) H88b(0.85) Cl1(0.85) Cl2(0.85)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b), C13(H13a,H13b), C19(H19a,H19b), C20(H20a,H20b),
 C26(H26a,H26b), C88(H88a,H88b)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
 C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68),
  C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77),
 C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86),
  C87(H87)
5.c Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c), C39(H39a,H39b,H39c)
;
_olex2_submission_special_instructions 'No special instructions were received'