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_7701460
_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         'C20 H25 Dy N8 O13, C3 H7 N O'
_chemical_formula_sum            'C23 H32 Dy N9 O14'
_chemical_formula_weight         821.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-11
_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                 115.989(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.480(4)
_cell_length_b                   15.745(5)
_cell_length_c                   15.510(5)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.290
_cell_measurement_theta_min      2.922
_cell_volume                     3178.5(17)
_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 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            87705
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.448
_diffrn_reflns_theta_min         2.567
_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1084 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.7874.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0394P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5168
_reflns_number_total             6482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02646k2.cif
_cod_data_source_block           wcy-3-020
_cod_database_code               7701460
_shelx_estimated_absorpt_t_max   0.218
_shelx_estimated_absorpt_t_min   0.348
_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:
 N2(H2), C15(H15), C13(H13), C7(H7), C11(H11), C18(H18), C4(H4), C3(H3),
 C21(H21), C1(H1), C2(H2A)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'