Structurally characterized homo-trinuclear ZnII and hetero-pentanuclear [ZnII4LnIII] complexes constructed from an octadentate bis(Salamo)-based ligand: Hirshfeld surfaces, fluorescence and catalytic properties
Li, Xiao-Yan; Kang, Quan-Peng; Liu, Chang; Zhang, Yang; Dong, Wen-Kui; New Journal of Chemistry 43 (2019) 4605–; doi:10.1039/C9NJ00014C

data_7058173
_publ_section_title
;
 Structurally characterized homo-trinuclear ZnII and hetero-pentanuclear
 [ZnII4LnIII] complexes constructed from an octadentate bis(Salamo)-based
 ligand: Hirshfeld surfaces, fluorescence and catalytic properties
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4605
_journal_paper_doi               10.1039/C9NJ00014C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety
'C72 H64 Eu N10 O24 Zn4, C2 H2 Cl6, C2 H6 N O4'
_chemical_formula_sum            'C76 H72 Cl6 Eu N11 O28 Zn4'
_chemical_formula_weight         2213.58
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.679(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8834(9)
_cell_length_b                   23.1409(12)
_cell_length_c                   24.3047(12)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.50
_cell_volume                     8995.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40357
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.691
_diffrn_reflns_theta_min         2.020
_exptl_absorpt_coefficient_mu    1.999
_exptl_absorpt_correction_T_max  0.6759
_exptl_absorpt_correction_T_min  0.4811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             4456
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10453
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+43.6746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7685
_reflns_number_total             10453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00014c2.cif
_cod_data_source_block           w131_sq
_cod_depositor_comments
'Adding full bibliography for 7058171--7058176.cif.'
_cod_database_code               7058173
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.625
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C45-C47
 1.5 with sigma of 0.01
 H30B-H36_$1
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, Cl8, Cl7, Cl9, C42, Cl4, Cl6, Cl5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, Cl8, Cl9, Cl7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, O14, N6, C45, O18, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Sof: Cl1(0.5) Cl2(0.5) Cl3(0.5) Cl4(0.25) C38(0.5) H38(0.5) H14(0.5)
 Cl6(0.25) Cl5(0.25) C42(0.25) H42(0.25) N6(0.5) O19(0.5) O18(0.5) C45(0.5)
 H45A(0.5) H45B(0.5) Cl8(0.25) Cl7(0.25) Cl9(0.25) C46(0.25) H46(0.25) C47(0.5)
 H47A(0.5) H47B(0.5) H47C(0.5)
6.a Riding coordinates:
 O12(H12), O14(H14), C47(H47A,H47B,H47C)
6.b Ternary CH refined with riding coordinates:
 C38(H38), C42(H42), C46(H46)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C16(H16A,H16B), C17(H17A,H17B), C29(H29A,H29B),
 C29(H29C,H29D), C45(H45A,H45B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C15(H15), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C33(H33), C34(H34),
  C35(H35), C36(H36)
6.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C30A(H30D,H30E,H30F)
;
_shelx_res_checksum              2798
_olex2_submission_special_instructions 'No special instructions were received'