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_7251433
_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         'C29 H20 Cl2 Cu2 N2 O7'
_chemical_formula_sum            'C29 H20 Cl2 Cu2 N2 O7'
_chemical_formula_weight         706.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8851(4)
_cell_length_b                   13.6763(4)
_cell_length_c                   14.8823(5)
_cell_measurement_reflns_used    7450
_cell_measurement_temperature    102(4)
_cell_measurement_theta_max      71.9040
_cell_measurement_theta_min      4.5350
_cell_volume                     2622.57(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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9684
_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      1.00  28.00   1.00    2.00    --   37.70 -59.00   8.00   27
  2  \w    -30.00   1.00   1.00    2.00    --   37.70 -77.00-115.00   31
  3  \w     25.00  62.00   1.00    2.00    --   37.70  59.00 148.00   37
  4  \w    136.00 164.00   1.00    3.00    --  107.00  59.00 148.00   28
  5  \w     87.00 132.00   1.00    3.00    --  107.00  77.00   9.00   45
  6  \w     82.00 167.00   1.00    3.00    --  107.00  88.00-103.00   85
  7  \w    -28.00  55.00   1.00    2.00    --   37.70 -38.00-120.00   83
  8  \w     40.00 108.00   1.00    2.00    --   37.70 178.00 150.00   68
  9  \w     49.00  76.00   1.00    3.00    --  107.00-111.00-150.00   27
 10  \w     41.00 130.00   1.00    3.00    --  107.00 178.00 -30.00   89
 11  \w     80.00 175.00   1.00    3.00    --  107.00  77.00 -60.00   95
 12  \w     54.00  82.00   1.00    3.00    --  107.00-111.00 -90.00   28
 13  \w     47.00 130.00   1.00    3.00    --  107.00 178.00 150.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1022537000
_diffrn_orient_matrix_UB_12      -0.0560210000
_diffrn_orient_matrix_UB_13      -0.0146543000
_diffrn_orient_matrix_UB_21      0.0334430000
_diffrn_orient_matrix_UB_22      0.0761096000
_diffrn_orient_matrix_UB_23      -0.0708573000
_diffrn_orient_matrix_UB_31      0.0520847000
_diffrn_orient_matrix_UB_32      0.0612953000
_diffrn_orient_matrix_UB_33      0.0741027000
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9354
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.983
_diffrn_reflns_theta_min         4.391
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36200
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.906
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 2075 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4999
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      21.861
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0521
_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^)+(0.1158P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                4924
_reflns_number_total             4999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01110h2.cif
_cod_data_source_block           kp1165a2_auto
_cod_database_code               7251433
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe Cu C H N O Cl'
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.508
_diffrn_oxdiff_digest_frames
;
01c601b65e6d55b02a2fcf42f42d22aacd0002807a7
;
_diffrn_oxdiff_digest_hkl
;
011ba055eee1ac863dc5923659830e5f1c4857
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O41-H41
 0.87 with sigma of 0.01
 Cu2-H41_$1
 2.965808 with sigma of 0.02
 C42-H41
 1.897236 with sigma of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C23(H23), C34(H34), C32(H32), C7(H7), C8(H8), C15(H15), C16(H16),
 C33(H33), C26(H26), C13(H13), C24(H24), C14(H14), C5(H5), C29(H29), C10(H10)
2.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              16687
_shelx_hkl_checksum              63885
_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 2.826
_oxdiff_exptl_absorpt_empirical_full_min 0.435