Mononuclear and Trinuclear DyIII SMMs with Schiff-base Ligands Modified by Nitro- Group: First Triangular Complex with N-N Pathway
Cheng, Li-Wei; Zhang, Chi-Lung; Wei, Jun-Yu; Lin, Po-Heng; Dalton Transactions  (2019) –; doi:10.1039/C9DT02646K

data_7701463
_publ_section_title
;
 Mononuclear and Trinuclear DyIII SMMs with Schiff-base Ligands Modified
 by Nitro- Group: First Triangular Complex with N-N Pathway
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02646K
_journal_year                    2019
_chemical_formula_moiety         'C28 H26 Dy N8 O12, N O3, 2(C2 H5 O)'
_chemical_formula_sum            'C32 H36 Dy N9 O17'
_chemical_formula_weight         981.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-16
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2019-08-20 deposited with the CCDC.    2019-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.566(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6293(5)
_cell_length_b                   13.9322(7)
_cell_length_c                   13.7379(7)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.843
_cell_measurement_theta_min      3.336
_cell_volume                     1878.68(16)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            99732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         34.917
_diffrn_reflns_theta_min         2.924
_exptl_absorpt_coefficient_mu    2.078
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0686 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.8435.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Gold
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       Block
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         8203
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.9169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6981
_reflns_number_total             8203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02646k2.cif
_cod_data_source_block           mo_wcy_3_025_0m
_cod_database_code               7701463
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Sof(H15A)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(H15)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
4.a Rotating group:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C4(H4), C3(H3), C13(H13), C2(H2A), C1(H1), C11(H11), C15(H15),
  C15(H15A)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F)
4.d Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'