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_7058172
_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 Sm Zn4, C2 H2 Cl6, H2 N O4'
_chemical_formula_sum            'C74 H68 Cl6 N11 O28 Sm Zn4'
_chemical_formula_weight         2183.92
_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             2019-02-07
_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                 108.673(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8229(9)
_cell_length_b                   23.2495(12)
_cell_length_c                   24.2036(14)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.50
_cell_volume                     8968.3(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      153.15
_diffrn_measured_fraction_theta_full 0.996
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38065
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.582
_diffrn_reflns_theta_min         2.604
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  0.5671
_exptl_absorpt_correction_T_min  0.4398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             4388
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0678P)^2^+45.6030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8065
_reflns_number_total             10314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00014c2.cif
_cod_data_source_block           20180131w128_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7058171--7058176.cif.'
_cod_database_code               7058172
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.672
_shelx_estimated_absorpt_t_min   0.630
_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,H) groups
2. Restrained distances
 O12-H12
 0.87 with sigma of 0.01
 O12-H12A
 0.87 with sigma of 0.01
 O20-N6
 1.2 with sigma of 0.02
 C36A-C35A = C35-C36
 1.5 with sigma of 0.01
 H29-H36D_$1
 2.2 with sigma of 0.02
 C35-H12
 1.978389 with sigma of 0.02
 Zn2-H12
 2.614584 with sigma of 0.02
 C35A-H12A
 1.883287 with sigma of 0.02
 Zn2-H12A
 2.588463 with sigma of 0.02
 Cl6-C39 \\sim C39-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl8) \\sim Ueq, Uanis(Cl7) \\sim Ueq, Uanis(Cl6) \\sim Ueq, Uanis(Cl5)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O13)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C35A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl6, Cl8, Cl7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O20, N6, O21, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl6, C39, Cl5, Cl4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, Cl8, Cl7, Cl9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36A, C35A, C35, C36, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H12(0.5) H12A(0.5) C35(0.5) H35A(0.5) H35B(0.5) C35A(0.5)
 H35C(0.5) H35D(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C36A(0.5) H36D(0.5)
 H36E(0.5) H36F(0.5) Cl1(0.55) Cl2(0.55) Cl3(0.55) C38(0.55) H38(0.55)
 H13C(0.5) H13D(0.5) Cl6(0.2) Cl8(0.25) Cl7(0.25) Cl5(0.2) N6(0.5) O20(0.5)
 O21(0.5) Cl4(0.2) C39(0.2) H39(0.2) C40(0.25) H40(0.25) Cl9(0.25)
6.a Riding coordinates:
 O13(H13C,H13D)
6.b Ternary CH refined with riding coordinates:
 C38(H38), C39(H39), C40(H40)
6.c Secondary CH2 refined with riding coordinates:
 C12(H12B,H12C), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B), C35(H35A,
 H35B), C35A(H35C,H35D)
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), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33)
6.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              60902
_olex2_submission_special_instructions 'No special instructions were received'