Two heteronuclear ZnII/CdII-DyIII complexes based on open-chain ether schiff base ligand: Synthesis, structures, fluorescence and antioxidation activity
Xu, Jianhua; Xia, Xinzhao; Zhang, Geng; Wu, Huilu; Qu, Yao; Xia, Lixian; Han, Xintong; Inorganica Chimica Acta 512 (2020) 119918–; doi:10.1016/j.ica.2020.119918

data_1564117
_publ_section_title
;
 Two heteronuclear ZnII/CdII-DyIII complexes based on open-chain ether
 schiff base ligand: Synthesis, structures, fluorescence and antioxidation
 activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119918
_journal_paper_doi               10.1016/j.ica.2020.119918
_journal_volume                  512
_journal_year                    2020
_chemical_formula_moiety         'C29 H31 Br2 Cd Dy N4 O13, 3(C H2 Cl2)'
_chemical_formula_sum            'C32 H37 Br2 Cd Cl6 Dy N4 O13'
_chemical_formula_weight         1333.07
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.091(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.794(9)
_cell_length_b                   14.886(8)
_cell_length_c                   19.153(10)
_cell_measurement_reflns_used    6053
_cell_measurement_temperature    153
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.58
_cell_volume                     4500(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1292
_diffrn_reflns_av_unetI/netI     0.1574
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14589
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.881
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.315
_exptl_absorpt_correction_T_max  0.404
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1162 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.6643.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0653
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3645
_reflns_number_total             8234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P  21/c '
_cod_database_code               1564117
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C32-Cl5 = C32-Cl6 = C30-Cl1 = C30-Cl2 = C31-Cl3 = C31-Cl4
 1.75 with sigma of 0.01
 H16-H19A
 2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C11(H11A,H11B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C16(H16), C24(H24), C26(H26), C12(H12), C14(H14), C7(H7), C4(H4),
 C23(H23), C25(H25)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C)
4.d Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_shelx_res_checksum              22778
_shelx_hkl_checksum              20614