A Preformed 1‐D {CuII2}n Helical Chain as Precursor to a Decanuclear 0-D {CuII8MnII2} Cluster: Synthesis, Structure and Magnetism
Pantelis, Konstantinos; Alexandropoulos, Dimitris I.; Escuer, Albert; Kostakis, George E.; Stamatatos, Theocharis C.; CrystEngComm  (2026) –; doi:10.1039/D5CE01110H

data_7251434
_publ_section_title
;
 A Preformed 1&#x2010;D {CuII2}n Helical Chain as Precursor to a
 Decanuclear 0-D {CuII8MnII2} Cluster: Synthesis, Structure and Magnetism
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE01110H
_journal_year                    2026
_chemical_formula_moiety         '3(C112 H72 Cl8 Cu8 Mn2 N8 O30), 10(C2 H3 N)'
_chemical_formula_sum            'C369 H266 Cl24 Cu24 Mn6 N40.5 O90.25'
_chemical_formula_weight         9416.61
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-01-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-11-22 deposited with the CCDC.	2025-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.799(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   77.1822(12)
_cell_length_b                   16.6415(4)
_cell_length_c                   29.2589(7)
_cell_measurement_reflns_used    12984
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      67.6150
_cell_measurement_theta_min      2.0820
_cell_volume                     36915.4(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -85.00 -14.00   1.00   30.00    --    0.00  40.00 -30.00   71
  2  \w     17.00  76.00   1.00   30.00    --    0.00  40.00 -30.00   59
  3  \w    -62.00 -13.00   1.00   60.00    --  -89.00  50.00  30.00   49
  4  \w   -173.00 -71.00   1.00   60.00    --  -89.00  50.00  30.00  102
  5  \w    -89.00  -6.00   1.00   60.00    --  -89.00  10.00 -30.00   83
  6  \w   -171.00-100.00   1.00   60.00    --  -89.00  10.00 -30.00   71
  7  \w    -84.00 -19.00   1.00   60.00    --  -89.00  50.00 120.00   65
  8  \w   -178.00-102.00   1.00   60.00    --  -89.00  50.00 120.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0076493000
_diffrn_orient_matrix_UB_12      0.0163804000
_diffrn_orient_matrix_UB_13      -0.0516557000
_diffrn_orient_matrix_UB_21      -0.0188282000
_diffrn_orient_matrix_UB_22      -0.0057617000
_diffrn_orient_matrix_UB_23      0.0102699000
_diffrn_orient_matrix_UB_31      0.0001439000
_diffrn_orient_matrix_UB_32      0.0909131000
_diffrn_orient_matrix_UB_33      0.0099118000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       92
_diffrn_reflns_limit_h_min       -87
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            76551
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.315
_diffrn_reflns_theta_min         2.331
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.111a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       plate
_exptl_crystal_F_000             18958
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2463
_refine_ls_number_reflns         32630
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+207.0321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25788
_reflns_number_total             32630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01110h2.cif
_cod_data_source_block           kp1227
_cod_original_formula_sum        'C369 H266 Cl24 Cu24 Mn6 N40.50 O90.25'
_cod_database_code               7251434
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O N Cu Cl'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.565
_olex2_refinement_description
;
1. Rigid bond restraints
 Cl02, C162, C167, C166, C165, C164, C163, Cl12, C0, C07D, C07J, C169, C170,
 C171
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(Cl02) \\sim Ueq, Uanis(C162) \\sim Ueq, Uanis(C167) \\sim Ueq,
Uanis(C166) \\sim Ueq, Uanis(C165) \\sim Ueq, Uanis(C164) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(Cl12) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C07D)
\\sim Ueq, Uanis(C07J) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq,
Uanis(C171) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl02) \\sim Ueq, Uanis(C162) \\sim Ueq, Uanis(C167) \\sim Ueq,
Uanis(C166) \\sim Ueq, Uanis(C165) \\sim Ueq, Uanis(C164) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C07J) \\sim Ueq, Uanis(C169)
\\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq, Uanis(Cl12) \\sim Ueq,
Uanis(C07D) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 C162, C167, C165, C164, C163, C0, C07J, C169, C170, C171, C07D, Cl02, Cl12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Cl02(0.5) C162(0.5) C167(0.5) C166(0.5) H166(0.5) C165(0.5)
 C164(0.5) H164(0.5) C163(0.5) H163(0.5) Cl12(0.5) C0(0.5) C07D(0.5) C07J(0.5)
 C169(0.5) H169(0.5) C170(0.5) H170(0.5) C171(0.5) H171(0.5)
5.a Rotating group:
 O29(H29A,H29B), O30(H30A,H30B), O45(H45A,H45B)
5.b Ternary CH refined with riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4), O31(H31A), O32(H32A)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C4(H4A), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C37(H37), C38(H38),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C51(H51), C52(H52),
  C54(H54), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C65(H65),
 C66(H66), C68(H68), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77), C79(H79),
  C80(H80), C82(H82), C86(H86), C87(H87), C88(H88), C89(H89), C91(H91),
 C93(H93), C94(H94), C96(H96), C100(H100), C101(H101), C102(H102), C103(H103),
 C105(H105), C107(H107), C108(H108), C110(H110), C114(H114), C115(H115),
 C116(H116), C117(H117), C119(H119), C121(H121), C122(H122), C124(H124),
 C128(H128), C129(H129), C130(H130), C131(H131), C133(H133), C135(H135),
 C136(H136), C138(H138), C142(H142), C143(H143), C144(H144), C145(H145),
 C147(H147), C149(H149), C150(H150), C152(H152), C156(H156), C157(H157),
 C158(H158), C159(H159), C161(H161), C166(H166), C164(H164), C163(H163),
 C169(H169), C170(H170), C171(H171)
5.d Fitted hexagon refined as free rotating group:
 C162(C167,C166,C165,C164,C163)
5.e Idealised Me refined as rotating group:
 C06X(H06A,H06B,H06C), C06Y(H06D,H06E,H06F), C05P(H05A,H05B,H05C), C065(H06G,
 H06H,H06I), C07E(H07A,H07B,H07C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1361
_shelx_hkl_checksum              717
_shelx_fab_checksum              92450
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.354
_oxdiff_exptl_absorpt_empirical_full_min 0.454