The bis-salphen Zn(II) unit: a versatile building block for self-assembled heteroleptic coordination cages.
Donaggio, Leonardo; Schweimer, Kristian; Heinemann, Frank W.; Hennig, Janosch; Kurz, Hannah; Nanoscale 18 (2026) 7002–7009; doi:10.1039/d5nr04564a

data_1577025
_publ_section_title
;
 The bis-salphen Zn(II) unit: a versatile building block for
 self-assembled heteroleptic coordination cages.
;
_journal_issue                   13
_journal_name_full               Nanoscale
_journal_page_first              7002
_journal_page_last               7009
_journal_paper_doi               10.1039/d5nr04564a
_journal_volume                  18
_journal_year                    2026
_chemical_formula_moiety
'C234 H282 N24 O12 Zn6, 8(C2 H3 N), 4(C H2 Cl2)'
_chemical_formula_sum            'C254 H314 Cl8 N32 O12 Zn6'
_chemical_formula_weight         4683.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-24 deposited with the CCDC.	2026-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                86.198(4)
_cell_angle_beta                 72.187(4)
_cell_angle_gamma                60.289(3)
_cell_formula_units_Z            2
_cell_length_a                   23.8937(19)
_cell_length_b                   23.9314(18)
_cell_length_c                   36.662(3)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      22.34
_cell_measurement_theta_min      2.25
_cell_volume                     17242(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa ImuS Duo Photon II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1466
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            456941
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.703
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1149 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.7833.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.902
_exptl_crystal_description       prism
_exptl_crystal_F_000             4948
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.732
_refine_diff_density_min         -2.123
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.729
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2837
_refine_ls_number_reflns         65347
_refine_ls_number_restraints     3185
_refine_ls_restrained_S_all      1.707
_refine_ls_R_factor_all          0.2107
_refine_ls_R_factor_gt           0.1644
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4436
_refine_ls_wR_factor_ref         0.4655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41260
_reflns_number_total             65347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr04564a2.cif
_cod_data_source_block           hku2503a
_cod_original_cell_volume        17243(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1577025
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9550(6)
 0.0450(6)
2. 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
3. Uiso/Uaniso restraints and constraints
C129 \\sim C130 \\sim C131 \\sim C132: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C150 \\sim C151 \\sim C152 \\sim C153: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C402 \\sim Cl43 \\sim Cl44: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C404 \\sim Cl47 \\sim Cl48: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N302 \\sim C303 \\sim C304: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C150) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq,
Uanis(C153) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C64) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C113) \\sim Ueq, Uanis(C117) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C128) \\sim Ueq, Uanis(C132) \\sim Ueq, Uanis(C149) \\sim Ueq,
Uanis(C177) \\sim Ueq, Uanis(C216) \\sim Ueq, Uanis(C226) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C205) \\sim Ueq, Uanis(Cl43) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N301) \\sim Ueq, Uanis(C301) \\sim Ueq, Uanis(C302) \\sim Ueq,
Uanis(N302) \\sim Ueq, Uanis(C303) \\sim Ueq, Uanis(C304) \\sim Ueq,
Uanis(N303) \\sim Ueq, Uanis(C305) \\sim Ueq, Uanis(C306) \\sim Ueq,
Uanis(N304) \\sim Ueq, Uanis(C307) \\sim Ueq, Uanis(C308) \\sim Ueq,
Uanis(N305) \\sim Ueq, Uanis(C309) \\sim Ueq, Uanis(C310) \\sim Ueq,
Uanis(N306) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C312) \\sim Ueq,
Uanis(N307) \\sim Ueq, Uanis(C313) \\sim Ueq, Uanis(C314) \\sim Ueq,
Uanis(N308) \\sim Ueq, Uanis(C315) \\sim Ueq, Uanis(C316) \\sim Ueq,
Uanis(C401) \\sim Ueq, Uanis(Cl41) \\sim Ueq, Uanis(Cl42) \\sim Ueq,
Uanis(C402) \\sim Ueq, Uanis(Cl43) \\sim Ueq, Uanis(Cl44) \\sim Ueq,
Uanis(C403) \\sim Ueq, Uanis(Cl45) \\sim Ueq, Uanis(Cl46) \\sim Ueq,
Uanis(C404) \\sim Ueq, Uanis(Cl47) \\sim Ueq, Uanis(Cl48) \\sim Ueq,
Uanis(C405) \\sim Ueq, Uanis(Cl50) \\sim Ueq, Uanis(Cl49) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C129, C130, C131, C132} sigma for 1-2: 0.02, 1-3: 0.04
{C150, C151, C152, C153} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C84, C85, C86, C87}
{C401, Cl41, Cl42} sigma for 1-2: 0.02, 1-3: 0.04
{C403, Cl45, Cl46} sigma for 1-2: 0.02, 1-3: 0.04
{C404, Cl47, Cl48} sigma for 1-2: 0.02, 1-3: 0.04
{C405, Cl50, Cl49} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C402, Cl43, Cl44}
{N302, C303, C304} sigma for 1-2: 0.02, 1-3: 0.04
{N303, C305, C306} sigma for 1-2: 0.02, 1-3: 0.04
{N306, C311, C312} sigma for 1-2: 0.02, 1-3: 0.04
{N307, C313, C314} sigma for 1-2: 0.02, 1-3: 0.04
{N308, C315, C316} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N301, C301, C302}
{N304, C307, C308} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N305, C309, C310}
6. Others
 Fixed Sof: C403(0.5) H40E(0.5) H40F(0.5) Cl45(0.5) Cl46(0.5) C404(0.5)
 H40G(0.5) H40H(0.5) Cl47(0.5) Cl48(0.5)
7.a Riding coordinates:
 C302(H30D,H30E,H30F), C304(H30G,H30H,H30I), C306(H30J,H30K,H30L), C308(H30M,
 H30N,H30O), C310(H31D,H31E,H31F), C312(H31G,H31H,H31I), C314(H31J,H31K,H31L),
 C316(H31M,H31N,H31O)
7.b Secondary CH2 refined with riding coordinates:
 C401(H40A,H40B), C402(H40C,H40D), C403(H40E,H40F), C404(H40G,H40H), C405(H40I,
 H40J)
7.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C),
 C100(H10A,H10B,H10C), C101(H10D,H10E,H10F), C102(H10G,H10H,H10I), C111(H11A,
 H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C115(H11J,H11K,H11L),
 C116(H11M,H11N,H11O), C117(H11P,H11Q,H11R), C126(H12A,H12B,H12C), C127(H12D,
 H12E,H12F), C128(H12G,H12H,H12I), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F),
 C132(H13G,H13H,H13I), C147(H14A,H14B,H14C), C148(H14D,H14E,H14F), C149(H14G,
 H14H,H14I), C151(H15D,H15E,H15F), C152(H15G,H15H,H15I), C153(H15J,H15K,H15L),
 C162(H16D,H16E,H16F), C163(H16G,H16H,H16I), C164(H16J,H16K,H16L), C166(H16M,
 H16N,H16O), C167(H16P,H16Q,H16R), C168(H16S,H16T,H16U), C177(H17D,H17E,H17F),
 C178(H17G,H17H,H17I), C179(H17J,H17K,H17L), C181(H18A,H18B,H18C), C182(H18D,
 H18E,H18F), C183(H18G,H18H,H18I), C192(H19D,H19E,H19F), C193(H19G,H19H,H19I),
 C194(H19J,H19K,H19L), C196(H19M,H19N,H19O), C197(H19P,H19Q,H19R), C198(H19S,
 H19T,H19U)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C11(H11), C13(H13), C22(H22), C26(H26), C28(H28),
 C37(H37), C41(H41), C43(H43), C52(H52), C56(H56), C58(H58), C69(H69), C72(H72),
  C73(H73), C77(H77), C79(H79), C88(H88), C92(H92), C94(H94), C103(H103),
 C107(H107), C109(H109), C118(H118), C122(H122), C124(H124), C135(H135),
 C138(H138), C139(H139), C143(H143), C145(H145), C154(H154), C158(H158),
 C160(H160), C169(H169), C173(H173), C175(H175), C184(H184), C188(H188),
 C190(H190), C203(H203), C204(H204), C205(H205), C206(H206), C208(H208),
 C209(H209), C210(H210), C211(H211), C213(H213), C214(H214), C215(H215),
 C216(H216), C221(H221), C222(H222), C223(H223), C224(H224), C226(H226),
 C227(H227), C228(H228), C229(H229), C231(H231), C232(H232), C233(H233),
 C234(H234)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40485
_shelx_fab_checksum              72734
_olex2_submission_special_instructions 'No special instructions were received'