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_7058175
_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 Gd N10 O24 Zn4, C2 H2 Cl6, C2 H6 N O4'
_chemical_formula_sum            'C76 H72 Cl6 Gd N11 O28 Zn4'
_chemical_formula_weight         2218.87
_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                 111.300(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9752(18)
_cell_length_b                   23.090(2)
_cell_length_c                   24.837(3)
_cell_measurement_reflns_used    7919
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      26.88
_cell_measurement_theta_min      2.49
_cell_volume                     9070.1(17)
_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 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34092
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         2.492
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  0.6751
_exptl_absorpt_correction_T_min  0.5039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SABABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             4460
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.425
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10510
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0846
_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^)+(0.0438P)^2^+226.8073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7400
_reflns_number_total             10510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00014c2.cif
_cod_data_source_block           w132_sq
_cod_depositor_comments
'Adding full bibliography for 7058171--7058176.cif.'
_cod_original_cell_volume        9069.8(16)
_cod_database_code               7058175
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.665
_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
 C40-C41
 1.5 with sigma of 0.01
 O9-H9
 0.87 with sigma of 0.01
 H31A-H24
 2.2 with sigma of 0.02
 C33-H9
 1.920898 with sigma of 0.02
 Zn1-H9
 2.610052 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C27A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C35A) \\sim Ueq,
Uanis(C34A) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl7, C42, Cl8, Cl9, Cl5, Cl3, C38, Cl6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36A, C33, C36, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C31, C32, C34, C35, C31A, C26A, C27A, C32A, C35A, C34A, C25, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O18, N6, C40, O19, O20, C41
 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)
 C31A(0.5) H31A(0.5) C26A(0.5) C27A(0.5) C32A(0.5) H32A(0.5) C35A(0.5)
 H35A(0.5) C34A(0.5) H34A(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), C35A(H35A), C34A(H34A)
6.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              58122
_olex2_submission_special_instructions 'No special instructions were received'