Solvent-and metal-gated coordination diversity in a dynamic aminal ligand
Juan, Jen-Wen; Ciou, Ji-Ming; Hsiang, Yi-Rong; Lin, Ya-Fan; Dalton Transactions  (2025) –; doi:10.1039/D5DT02405F

data_7719954
_publ_section_title
;
 Solvent-and metal-gated coordination diversity in a dynamic aminal ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02405F
_journal_year                    2025
_chemical_formula_moiety         '2(C12 H13 Cu0.5 N3 O), 2(Cl O4)'
_chemical_formula_sum            'C24 H26 Cl2 Cu N6 O10'
_chemical_formula_weight         692.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2ppr5b
_audit_creation_date             2025-09-17
_audit_creation_method
;
Olex2 1.5-ac7-016
(compiled 2025.05.29 svn.r8cd99b3d for Rigaku Oxford Diffraction, GUI svn.r7254)
;
_audit_update_record
;
2025-10-06 deposited with the CCDC.	2025-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.737(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0096(2)
_cell_length_b                   18.7829(3)
_cell_length_c                   12.7611(2)
_cell_measurement_reflns_used    16138
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      77.2810
_cell_measurement_theta_min      3.5880
_cell_volume                     2783.89(8)
_computing_cell_refinement       'CrysAlisPro 1.171.44.119a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.120a 64-bit (release 22-08-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.119a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac7-016 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-016 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_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     16.00 104.00   0.50    0.08    --   51.87-135.00-128.00  176
  2  \w     45.00  70.00   0.50    0.08    --  103.95-135.00-128.00   50
  3  \w     64.00  91.00   0.50    0.08    --  103.95 -95.00   0.00   54
  4  \w     35.00  90.00   0.50    0.08    --  103.95 -95.00  30.00  110
  5  \w     45.00  70.00   0.50    0.08    --  103.95-135.00  50.00   50
  6  \w     37.00  92.00   0.50    0.08    --  103.95 -95.00 120.00  110
  7  \w     16.00 104.00   0.50    0.08    --   51.87-135.00  50.00  176
  8  \w     37.00  67.00   0.50    0.08    --  103.95 -77.00 -60.00   60
  9  \w     37.00  62.00   0.50    0.08    --  103.95 -77.00 -90.00   50
 10  \w     37.00  62.00   0.50    0.08    --  103.95 -77.00-150.00   50
 11  \w    103.00 147.00   0.50    0.08    --  103.95  15.00-150.00   88
 12  \w    104.00 137.00   0.50    0.08    --  103.95  15.00 -60.00   66
 13  \w     -2.00  23.00   0.50    0.08    --   14.00  77.00 109.61   50
 14  \w    109.00 143.00   0.50    0.08    --  103.95  15.00  60.00   68
 15  \w     98.00 123.00   0.50    0.08    --  103.95 135.00 116.00   50
 16  \w    122.00 147.00   0.50    0.08    --  103.95 135.00 -63.00   50
 17  \w     -4.00  21.00   0.50    0.08    --   14.00  81.00-144.88   50
 18  \w    -93.00 -32.00   0.50    0.08    --  -99.00  98.00-177.67  122
 19  \w    -64.00 -25.00   0.50    0.08    --  -92.68 135.00 -63.00   78
 20  \w    -57.00 -30.00   0.50    0.08    --  -99.00  98.00 -72.27   54
 21  \w    -93.00 -67.00   0.50    0.08    --  -99.00  98.00 -80.11   52
 22  \w    -93.00 -61.00   0.50    0.08    --  -99.00  98.00 -72.27   64
 23  \w    -92.00 -31.00   0.50    0.08    --  -99.00  94.00 -94.75  122
 24  \w   -105.00 -16.00   0.50    0.08    --  -54.87 135.00 116.00  178
 25  \w    -63.00 -27.00   0.50    0.08    --  -92.68 135.00 116.00   72
 26  \w    -47.00 -21.00   0.50    0.08    --  -92.68  61.00 150.00   52
 27  \w    -47.00 -22.00   0.50    0.08    --  -92.68  61.00 120.00   50
 28  \w    -22.00  15.00   0.50    0.08    --  -54.87  38.00-150.00   74
 29  \w    -49.00 -23.00   0.50    0.08    --  -92.68  61.00 -90.00   52
 30  \w   -150.00-104.00   0.50    0.08    --  -92.68 -15.00-150.00   92
 31  \w   -122.00 -82.00   0.50    0.08    --  -92.68-135.00-128.00   80
 32  \w   -139.00 -64.00   0.50    0.08    --  -66.00 -46.00  58.31  150
 33  \w    -51.00 -26.00   0.50    0.08    --  -34.00 -66.00  27.79   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0724934000
_diffrn_orient_matrix_UB_12      0.0089555000
_diffrn_orient_matrix_UB_13      -0.0828873000
_diffrn_orient_matrix_UB_21      -0.0073052000
_diffrn_orient_matrix_UB_22      0.0815293000
_diffrn_orient_matrix_UB_23      0.0096068000
_diffrn_orient_matrix_UB_31      0.1108271000
_diffrn_orient_matrix_UB_32      -0.0004507000
_diffrn_orient_matrix_UB_33      0.0928485000
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27754
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.629
_diffrn_reflns_theta_min         3.806
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.119a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.799
_exptl_crystal_size_mid          0.416
_exptl_crystal_size_min          0.355
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5677
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+25.4783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5575
_reflns_number_total             5677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02405f2.cif
_cod_data_source_block           250912c_yfl
_cod_database_code               7719954
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C22 H24 Cl2 Cu N6 O12'
_diffrn_oxdiff_digest_hkl
;
430a1733ad7bd8f0f06348f44ab78994d7c127
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name 250912c_YFL.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C12, C12B}
{C24, C24B}
3. Uiso/Uaniso restraints and constraints
Uanis(O10) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N6B) = Uanis(N6)
Uanis(C24) = Uanis(C24B)
Uanis(C18B) = Uanis(C18)
Uanis(C12) = Uanis(C12B)
Uanis(O1B) = Uanis(O1)
Uanis(N3) = Uanis(N3B)
Uanis(C6B) = Uanis(C6)
Uanis(O2) = Uanis(O2B)
4. Others
 Sof(N6)=Sof(H6A)=1-FVAR(1)
 Sof(N6B)=Sof(H6BA)=FVAR(1)
 Fixed Sof: O1(0.5) O1B(0.5) O2(0.5) O2B(0.5) N3(0.5) H3(0.5) N3B(0.5)
 H3B(0.5) C6(0.5) H6(0.5) C6B(0.5) H6B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5) C12B(0.5) H12D(0.5) H12E(0.5) H12F(0.5) C18(0.5) H18(0.5) C18B(0.5)
 H18B(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C24B(0.5) H24D(0.5) H24E(0.5)
 H24F(0.5)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C6B(H6B), C18(H18), C18B(H18B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N3B(H3B), N6(H6A), N6B(H6BA), C1(H1), C2(H2), C3(H3A), C4(H4), C8(H8),
  C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C20(H20),
 C21(H21), C22(H22), C23(H23)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C12B(H12D,H12E,H12F), C24(H24A,H24B,H24C), C24B(H24D,
 H24E,H24F)
;
_shelx_res_checksum              64015
_shelx_hkl_checksum              26821
_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 1.860
_oxdiff_exptl_absorpt_empirical_full_min 0.695