Imido Ligand Significantly Enhances The Effective Energy Barrier of Dysprosium(III) Single-Molecule Magnets
Liu, Bing-Cheng; Ge, Ning; Zhai, Yuan-Qi; Zhang, Tao; Ding, You-Song; Zheng, Yan-Zhen; Chemical Communications  (2019) –; doi:10.1039/C9CC04687A

data_7123802
_publ_section_title
;
 Imido Ligand Significantly Enhances The Effective Energy Barrier of
 Dysprosium(III) Single-Molecule Magnets
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04687A
_journal_year                    2019
_chemical_formula_moiety         'C39 H60 Cl2 Dy N3 O3, C4 H8 O'
_chemical_formula_sum            'C43 H68 Cl2 Dy N3 O4'
_chemical_formula_weight         924.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-19 deposited with the CCDC.    2019-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1852(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1751(16)
_cell_length_b                   12.3575(11)
_cell_length_c                   20.0341(17)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.400
_cell_measurement_theta_min      2.254
_cell_volume                     4473.4(7)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.663
_diffrn_reflns_theta_min         1.601
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.8383.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       stick
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         10355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0312P)^2^+2.1161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8044
_reflns_number_total             10355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04687a2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7123802
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.640
_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.a Ternary CH refined with riding coordinates:
 C8BA(H8BA), C3AA(H3AA), C9AA(H9AA), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C9BA(H9BA,H9BB), C0BA(H0BA,H0BB), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B),
 C6(H6A,H6B), C8(H8A,H8B), C15(H15A,H15B), C18(H18A,H18B), C1CA(H1CA,H1CB),
 C0CA(H0CA,H0CB), C2CA(H2CA,H2CB), C4CA(H4CA,H4CB), C3CA(H3CA,H3CB), C6AA(H6AA,
 H6AB), C5CA(H5CA,H5CB)
2.c Aromatic/amide H refined with riding coordinates:
 C4BA(H4BA), C2AA(H2AA), C4AA(H4AA), C8AA(H8AA), C7(H7), C12(H12), C13(H13),
 C14(H14)
2.d Idealised Me refined as rotating group:
 C2BA(H2BA,H2BB,H2BC), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C6BA(H6BA,H6BB,H6BC)
;
_shelx_res_checksum              45591
_olex2_submission_special_instructions 'No special instructions were received'