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_7123801
_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         'C45 H51 Cl2 Dy O4'
_chemical_formula_sum            'C45 H51 Cl2 Dy O4'
_chemical_formula_weight         889.26
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-12-19 deposited with the CCDC.    2019-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.395(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.722(18)
_cell_length_b                   8.732(4)
_cell_length_c                   21.661(9)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.566
_cell_measurement_theta_min      2.179
_cell_volume                     8057(6)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.975
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35943
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.803
_diffrn_reflns_theta_min         1.886
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             3624
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9308
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0378
_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^+30.0926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7358
_reflns_number_total             9308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04687a2.cif
_cod_data_source_block           1
_cod_database_code               7123801
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 O00G-C01F
 1.42 with sigma of 0.01
 O00G-C01D
 1.42 with sigma of 0.01
3. Rigid bond restraints
 O00G, C01D, C016, C01F
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O005, C01A, C4, C01G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O00G \\sim C01F \\sim C01D \\sim C016: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O00G \\sim C01F \\sim C0AA \\sim C016 \\sim C01D: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O005 \\sim C01A \\sim C4 \\sim C01G: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(O2)=1-FVAR(1)
 Sof(O00G)=Sof(C016)=Sof(H01H)=Sof(H01I)=Sof(C01D)=Sof(H01M)=Sof(H01N)=
 Sof(C01F)=Sof(H01O)=Sof(H01P)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C00C(H00C), C00P(H00P)
6.b Secondary CH2 refined with riding coordinates:
 C00K(H00D,H00E), C00O(H00F,H00G), C00W(H00K,H00M), C010(H01A,H01B), C012(H01C,
 H01D), C016(H01H,H01I), C01A(H01J,H01K), C01D(H01M,H01N), C01F(H01O,H01P),
 C01G(H01Q,H01R), C4(H4A,H4B), C0AA(H0AA,H0AB), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C6(H6A,H6B)
6.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00H(H00H), C00I(H00I), C00J(H00J), C00L(H00L),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C014(H014), C015(H015),
 C017(H017), C018(H018), C019(H019), C01B(H01L)
6.d Idealised Me refined as rotating group:
 C013(H01E,H01F,H01G)
;
_shelx_res_checksum              4687
_olex2_submission_special_instructions 'No special instructions were received'