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_7701461
_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 Gd3 N24 O33'
_chemical_formula_sum            'C69 H81 Gd3 N24 O33'
_chemical_formula_weight         2246.32
_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             2019-09-09
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2019-09-27 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                   28.897(4)
_cell_length_b                   28.897(4)
_cell_length_c                   28.897(4)
_cell_measurement_reflns_used    9418
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.345
_cell_measurement_theta_min      2.991
_cell_volume                     24130(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 2014/5 (Sheldrick, 2014)'
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            234187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.978
_diffrn_reflns_theta_max         24.978
_diffrn_reflns_theta_min         2.907
_exptl_absorpt_coefficient_mu    1.700
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6338
_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            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             8952
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.105
_refine_diff_density_max         2.064
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0264P)^2^+293.8480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5593
_reflns_number_total             7075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02646k2.cif
_cod_data_source_block           clw_gd_1
_cod_original_cell_volume        24130(10)
_cod_database_code               7701461
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.602
_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.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C10(H10), C7(H7), C12(H12), C21(H21), C14(H14), C5(H5), C3(H3),
 C18(H18)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C22(H22A,H22B,
 H22C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              88977
_shelx_fab_checksum              54574
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'