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_1564116
_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
'C48 H47 Br4 Dy N5 O14 Zn2, N O3, C H2 Cl2, 2(C H4 O)'
_chemical_formula_sum            'C51 H57 Br4 Cl2 Dy N6 O19 Zn2'
_chemical_formula_weight         1741.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.489(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.847(3)
_cell_length_b                   12.3745(11)
_cell_length_c                   32.761(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    153
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.29
_cell_volume                     12107.7(19)
_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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30587
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         1.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.812
_exptl_absorpt_correction_T_max  0.214
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1179 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.4387.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             6856
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.725
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11032
_refine_ls_number_restraints     1480
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1017P)^2^+90.5646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8268
_reflns_number_total             11032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex1.cif
_cod_data_source_block           1
_cod_database_code               1564116
_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
 O19-C51
 1.45 with sigma of 0.01
 Cl1-C49 = Cl2-C49
 1.75 with sigma of 0.01
 O18-C50
 1.45 with sigma of 0.01
 O18-Cl1
 2.3 with sigma of 0.01
 H18-Cl1
 1.83493 with sigma of 0.01
 H19-O17
 1.83493 with sigma of 0.01
3. Rigid bond restraints
 Cl1, Cl2, C49, C50, O19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim O19 \\sim Cl1 \\sim C17 \\sim C21 \\sim C5 \\sim C1 \\sim C38 \\sim
C18 \\sim C33 \\sim C25 \\sim C3 \\sim C2 \\sim C4 \\sim C34 \\sim C24 \\sim
C13 \\sim C39 \\sim C6 \\sim C16 \\sim C27 \\sim C12 \\sim C37 \\sim C41 \\sim
C26 \\sim C20 \\sim C42 \\sim C7 \\sim C47 \\sim C36 \\sim C29 \\sim C15 \\sim
C22 \\sim C14 \\sim C35 \\sim C19 \\sim C31 \\sim C28 \\sim C8 \\sim C30 \\sim
C32 \\sim C23 \\sim C40 \\sim C48 \\sim C11 \\sim C9 \\sim C10 \\sim C43 \\sim
C44 \\sim C46 \\sim C45 \\sim C50 \\sim C49 \\sim C51: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C28(H28A,H28B), C8(H8A,H8B), C30(H30A,H30B),
 C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B), C49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C34(H34), C24(H24), C16(H16), C27(H27), C12(H12), C7(H7),
 C36(H36), C22(H22), C14(H14), C32(H32), C43(H43), C44(H44), C46(H46), C45(H45)
5.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C40(H40A,H40B,
 H40C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
5.d Idealised tetrahedral OH refined as rotating group:
 O18(H18), O19(H19)
;
_shelx_res_checksum              88887
_shelx_hkl_checksum              84820
_shelx_fab_checksum              90383
_shelx_shelxl_version_number     2014/7