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_7058174
_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 N10 O24 Tb Zn4, N O3, C2 H6 O'
_chemical_formula_sum            'C74 H70 N11 O28 Tb Zn4'
_chemical_formula_weight         1981.81
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.675(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.542(3)
_cell_length_b                   28.886(7)
_cell_length_c                   19.183(4)
_cell_measurement_reflns_used    4188
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.25
_cell_volume                     7453(3)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33737
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.280
_exptl_absorpt_coefficient_mu    2.300
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.635
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         12830
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+159.0645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2247
_refine_ls_wR_factor_ref         0.2660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9450
_reflns_number_total             12830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00014c2.cif
_cod_data_source_block           tb
_cod_depositor_comments
'Adding full bibliography for 7058171--7058176.cif.'
_cod_database_code               7058174
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.597
_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
 O26-H26
 0.87 with sigma of 0.01
 C74-C69 = C74A-C69A
 1.5 with sigma of 0.02
 O27-H27A
 0.87 with sigma of 0.01
 C69-O27 = O27-C69A
 1.4 with sigma of 0.02
 H62_$1-H69D
 2.2 with sigma of 0.02
 O27-C74A
 2.4 with sigma of 0.02
 C71-H26
 1.955149 with sigma of 0.02
 Zn4-H26
 2.649447 with sigma of 0.02
 C69-H27A
 2.060785 with sigma of 0.02
 Zn3-H27A
 2.661609 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(C74A) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C69A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C69, O27, C74, C69A, C74A, Zn3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(1)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
6.a Riding coordinates:
 O27(H27A)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B), C46(H46A,
 H46B), C47(H47A,H47B), C56(H56A,H56B), C57(H57A,H57B), C69(H69A,H69B),
 C71(H71A,H71B), C72(H72A,H72B), C69A(H69C,H69D)
6.c 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), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
 C45(H45), C48(H48), C50(H50), C51(H51), C55(H55), C58(H58), C61(H61), C62(H62),
  C63(H63), C64(H64), C66(H66), C67(H67)
6.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C74A(H74D,H74E,
 H74F)
6.e Idealised tetrahedral OH refined as rotating group:
 O28(H28A)
;
_shelx_res_checksum              94591
_olex2_submission_special_instructions 'No special instructions were received'