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_7058176
_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 Dy N10 O24 Zn4, C2 H2 Cl6, C2 H6 N O4'
_chemical_formula_sum            'C76 H72 Cl6 Dy N11 O28 Zn4'
_chemical_formula_weight         2224.12
_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                 111.278(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9466(9)
_cell_length_b                   23.0127(12)
_cell_length_c                   24.9394(15)
_cell_measurement_reflns_used    1546
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     9063.0(9)
_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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40263
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.656
_diffrn_reflns_theta_min         2.491
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.693
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             4468
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10506
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0591P)^2^+46.8786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7981
_reflns_number_total             10506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00014c2.cif
_cod_data_source_block           dy
_cod_depositor_comments
'Adding full bibliography for 7058171--7058176.cif.'
_cod_database_code               7058176
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.609
_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
 Cl8-C42 = C42-Cl9
 1.7 with sigma of 0.02
 O9-H9
 0.85 with sigma of 0.01
 H24-H31A
 2.2 with sigma of 0.02
 C33-H9
 1.906924 with sigma of 0.02
 Zn1-H9
 2.576156 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C37, Cl1, Cl2, Cl4, Cl5, Cl3, C38, Cl6, Cl9, Cl7, C42, Cl8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C31, C32, C34, C35, C26A, C27A, C31A, C32A, C34A, C35A, C25, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, O20, O19, O18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H33C)=Sof(H33D)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Fixed Sof: C26(0.5) C27(0.5) H28(0.5) H28A(0.5) C31(0.5) H31(0.5) C32(0.5)
 H32(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5) Cl1(0.5) Cl2(0.5) Cl3(0.25)
 Cl4(0.5) Cl5(0.25) Cl6(0.25) H18(0.5) O19(0.5) O20(0.5) N6(0.5) C37(0.5)
 H37(0.5) C38(0.25) H38(0.25) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5)
 H41B(0.5) H41C(0.5) Cl7(0.25) Cl8(0.25) Cl9(0.25) C42(0.25) H42(0.25)
 C26A(0.5) C27A(0.5) C31A(0.5) H31A(0.5) C32A(0.5) H32A(0.5) C34A(0.5)
 H34A(0.5) C35A(0.5) H35A(0.5)
6.a Riding coordinates:
 O18(H18)
6.b Ternary CH refined with riding coordinates:
 C37(H37), C38(H38), C42(H42)
6.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B), C33(H33A,
 H33B), C33(H33C,H33D), C40(H40A,H40B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C14(H14), C16(H16),
 C17(H17), C21(H21), C24(H24), C28(H28), C28(H28A), C29(H29), C31(H31),
 C32(H32), C34(H34), C35(H35), C31A(H31A), C32A(H32A), C34A(H34A), C35A(H35A)
6.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              94424
_olex2_submission_special_instructions 'No special instructions were received'