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_7701462
_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         'C69 H81 Dy3 N24 O33'
_chemical_formula_sum            'C69 H81 Dy3 N24 O33'
_chemical_formula_weight         2262.07
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-24
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2019-10-28 deposited with the CCDC.    2019-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.811(4)
_cell_length_b                   28.811(4)
_cell_length_c                   28.811(4)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.91
_cell_volume                     23915(6)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.18
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            376587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.429
_diffrn_reflns_theta_min         2.828
_exptl_absorpt_coefficient_mu    1.926
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             9000
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.208
_refine_diff_density_max         2.246
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8203
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+284.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5144
_reflns_number_total             8203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02646k2.cif
_cod_data_source_block           wcy-dy
_cod_original_cell_volume        23915(10)
_cod_database_code               7701462
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C10 \\sim C9 \\sim C1 \\sim C11 \\sim C16 \\sim C7 \\sim C6 \\sim C2 \\sim C15
\\sim C12 \\sim C14 \\sim C13 \\sim C4 \\sim C3 \\sim C5 \\sim C17 \\sim C8
\\sim C21 \\sim C22 \\sim C23 \\sim C18 \\sim C20 \\sim C19: within -3.4A with
sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C10(H10), C7(H7), C12(H12), C14(H14), C3(H3), C5(H5), C21(H21),
 C18(H18)
3.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              23127
_shelx_fab_checksum              64989
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'