A novel oxime-derived 3d-4f single-molecule magnet exhibiting two single-ion magnetic relaxations.
Dong, Hui-Ming; Li, Yan; Liu, Zhong-Yi; Yang, En-Cui; Zhao, Xiao-Jun; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11876–11882; doi:10.1039/c6dt02003h

data_7039608
_publ_section_title
;
 A novel oxime-derived 3d-4f single-molecule magnet exhibiting two
 single-ion magnetic relaxations.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11876
_journal_page_last               11882
_journal_paper_doi               10.1039/c6dt02003h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C64 H62 Dy4 N48 Ni6 O18, 2(C H4 O), 2(Cl O4)'
_chemical_formula_sum            'C73 H88 Cl2 Dy4 N50 Ni6 O31'
_chemical_formula_weight         3235.09
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-18 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.960(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4709(7)
_cell_length_b                   26.2839(16)
_cell_length_c                   18.8993(10)
_cell_measurement_reflns_used    8828
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.36
_cell_volume                     5207.1(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29859
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.411
_exptl_absorpt_coefficient_mu    4.043
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0645 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.7854.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       block
_exptl_crystal_F_000             3180
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
The unit cell contains 6 methanol molecules and 4 acetoniteile molecules 
which have been treated as a diffuse contribution to 
the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         9178
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0315P)^2^+16.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7810
_reflns_number_total             9178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02003h2.cif
_cod_data_source_block           n150413d
_cod_depositor_comments          'Adding full bibliography for 7039608.cif.'
_cod_database_code               7039608
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.499
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C21-N18 = N18-C23 = C23-C24 = C24-N17 = N17-C22 = C22-C21
 1.38 with sigma of 0.01
 C21-C23 = N18-C24 = C23-N17 = C24-C22 = N17-C21 = C22-N18
 2.35 with sigma of 0.01
 C21-C24 = N18-N17 = C23-C22
 2.65 with sigma of 0.01
 C21'-N18' = N18'-C23' = C23'-C24' = C24'-N17'
 1.38 with sigma of 0.01
 N17'-C22' = C22'-C21'
 1.38 with sigma of 0.01
 C21'-C23' = N18'-C24' = C23'-N17' = C24'-C22'
 2.35 with sigma of 0.01
 N17'-C21' = C22'-N18'
 2.35 with sigma of 0.01
 C21'-C24' = N18'-N17' = C23'-C22'
 2.65 with sigma of 0.01
 C24-C25 = C24'-C25
 1.48 with sigma of 0.01
 O11'-O12' = O11'-O13' = O12'-O13'
 2.32 with sigma of 0.01
 O10'-O11' = O10'-O12' = O10'-O13'
 2.32 with sigma of 0.01
 Cl1'-O10' = Cl1'-O11' = Cl1'-O12' = Cl1'-O13'
 1.4 with sigma of 0.01
 O10-O11 = O10-O12 = O10-O13 = O11-O12 = O11-O13 = O12-O13
 2.32 with sigma of 0.01
 Cl1-O10 = Cl1-O11 = Cl1-O12 = Cl1-O13
 1.4 with sigma of 0.01
3. Restrained planarity
 N17, N18, C21, C22, C23, C24
 with sigma of 0.001
 N17', N18', C21', C22', C23', C24'
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C17 \\sim C1 \\sim C18 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15
\\sim C16 \\sim C19 \\sim C20 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29
\\sim C30 \\sim C31 \\sim C32 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C21' \\sim C22' \\sim C23' \\sim C24' \\sim C35: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
Uanis(C23') \\sim Ueq, Uanis(C22') \\sim Ueq, Uanis(C21') \\sim Ueq,
Uanis(N18') \\sim Ueq, Uanis(N17') \\sim Ueq, Uanis(C24') \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(O7) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N24) \\sim
Ueq, Uanis(O4) \\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(N11) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N18)
\\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C21) = Uanis(C21')
Uanis(N18) = Uanis(N18')
Uanis(N17) = Uanis(N17')
Uanis(C24) = Uanis(C24')
Uanis(C23) = Uanis(C23')
Uanis(C22) = Uanis(C22')
Uanis(O13) = Uanis(O13')
Uanis(O12) = Uanis(O12')
Uanis(O11) = Uanis(O11')
Uanis(O10) = Uanis(O10')
Uanis(Cl1) = Uanis(Cl1')
5. Others
 Sof(Cl1')=Sof(O10')=Sof(O11')=Sof(O12')=Sof(O13')=1-FVAR(1)
 Sof(Cl1)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(O13)=FVAR(1)
 Sof(N17')=Sof(N18')=Sof(C21')=Sof(H21')=Sof(C22')=Sof(H22')=Sof(C23')=
 Sof(H23')=Sof(C24')=1-FVAR(2)
 Sof(N17)=Sof(N18)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=
 Sof(C24)=FVAR(2)
6.a Riding coordinates:
 O1(H1)
6.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N12(H12), N20(H20), C17(H17), C1(H1A), C18(H18), C2(H2), C3(H3),
 C6(H6), C7(H7), C8(H8A), C11(H11), C12(H12A), C13(H13), C16(H16), C26(H26),
 C27(H27), C28(H28), C21(H21), C22(H22), C23(H23), C21'(H21'), C22'(H22'),
 C23'(H23')
6.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N16(H16A,H16B), N24(H24A,H24B)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C)
6.e Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20