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_7719955
_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         'C12 H8 Cu N2 O4, 2(H2 O)'
_chemical_formula_sum            'C12 H12 Cu N2 O6'
_chemical_formula_weight         343.78
_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     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2pprbh
_audit_creation_date             2025-09-18
_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                75.938(3)
_cell_angle_beta                 85.132(3)
_cell_angle_gamma                72.141(3)
_cell_formula_units_Z            1
_cell_length_a                   5.0897(2)
_cell_length_b                   7.5229(3)
_cell_length_c                   9.0809(3)
_cell_measurement_reflns_used    5423
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.2820
_cell_measurement_theta_min      6.3290
_cell_volume                     321.01(2)
_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      100.00(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 0.992
_diffrn_measured_fraction_theta_max 0.991
_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      8.00  37.00   0.50    0.05    --   22.00  72.00 178.11   58
  2  \w     23.00  54.00   0.50    0.05    --   34.00  65.00  73.50   62
  3  \w     18.00  44.00   0.50    0.05    --   30.00  68.00  57.23   52
  4  \w     30.00  59.00   0.50    0.05    --   38.00  59.00 110.60   58
  5  \w     23.00  51.00   0.50    0.05    --   34.00  66.00 -88.71   56
  6  \w     20.00  54.00   0.50    0.05    --   30.00  64.00-151.85   68
  7  \w    -73.00 -26.00   0.50    0.05    --  -92.65  77.00-150.00   94
  8  \w    -51.00 -21.00   0.50    0.05    --  -92.65  61.00 -30.00   60
  9  \w    -51.00 -21.00   0.50    0.05    --  -92.65  61.00  30.00   60
 10  \w    -51.00 -21.00   0.50    0.05    --  -92.65  61.00 120.00   60
 11  \w    -51.00 -21.00   0.50    0.05    --  -92.65  61.00 150.00   60
 12  \w    -22.00  20.00   0.50    0.05    --  -54.87  38.00 150.00   84
 13  \w    -92.00 -30.00   0.50    0.05    --  -99.00  93.00 166.19  124
 14  \w    -83.00   9.00   0.50    0.05    --  -54.87  97.00  29.00  184
 15  \w    -83.00   9.00   0.50    0.05    --  -54.87  97.00  29.00  184
 16  \w    -92.00 -23.00   0.50    0.05    --  -92.65  97.00  29.00  138
 17  \w   -101.00 -21.00   0.50    0.05    --  -92.65 125.00-150.00  160
 18  \w   -101.00 -21.00   0.50    0.05    --  -92.65 125.00-150.00  160
 19  \w   -161.00 -97.00   0.50    0.05    --  -92.65 -97.00 -78.00  128
 20  \w   -157.00 -79.00   0.50    0.05    --  -86.00 -61.00-114.48  156
 21  \w   -143.00 -65.00   0.50    0.05    --  -70.00 -53.00 -55.02  156
 22  \w   -143.00 -65.00   0.50    0.05    --  -70.00 -53.00 -55.02  156
 23  \w   -150.00 -92.00   0.50    0.05    --  -92.65 -15.00-180.00  116
 24  \w   -135.00 -57.00   0.50    0.05    --  -62.00 -53.00  10.68  156
 25  \w   -170.00 -89.00   0.50    0.05    --  -99.00 -63.00   2.87  162
 26  \w   -143.00 -65.00   0.50    0.05    --  -70.00 -53.00 121.93  156
 27  \w     37.00  73.00   0.50    0.05    --  103.98 -77.00 150.00   72
 28  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00 -30.00  114
 29  \w     -9.00  80.00   0.50    0.05    --   51.62 -97.00 -78.00  178
 30  \w     35.00  92.00   0.50    0.05    --  103.98 -97.00 -78.00  114
 31  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00 -60.00  114
 32  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00 -30.00  114
 33  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00   0.00  114
 34  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00  60.00  114
 35  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00  90.00  114
 36  \w     35.00  92.00   0.50    0.05    --  103.98 -95.00-150.00  114
 37  \w     97.00 173.00   0.50    0.05    --  103.98  97.00  29.00  152
 38  \w     79.00 124.00   0.50    0.05    --   51.62  57.00-180.00   90
 39  \w     79.00 124.00   0.50    0.05    --   51.62  57.00-120.00   90
 40  \w    103.00 150.00   0.50    0.05    --  103.98  15.00-150.00   94
 41  \w    103.00 150.00   0.50    0.05    --  103.98  15.00-180.00   94
 42  \w    104.00 171.00   0.50    0.05    --  103.98  30.00 -60.00  134
 43  \w    104.00 171.00   0.50    0.05    --  103.98  30.00 -60.00  134
 44  \w    103.00 150.00   0.50    0.05    --  103.98  15.00  60.00   94
 45  \w    103.00 150.00   0.50    0.05    --  103.98  15.00 120.00   94
;
_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      0.1172078000
_diffrn_orient_matrix_UB_12      -0.1404355000
_diffrn_orient_matrix_UB_13      0.1497077000
_diffrn_orient_matrix_UB_21      0.0097904000
_diffrn_orient_matrix_UB_22      -0.1704177000
_diffrn_orient_matrix_UB_23      -0.0683348000
_diffrn_orient_matrix_UB_31      0.2954788000
_diffrn_orient_matrix_UB_32      -0.0090498000
_diffrn_orient_matrix_UB_33      -0.0592293000
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5883
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         6.350
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.119a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.778
_exptl_crystal_description       block
_exptl_crystal_F_000             175
_exptl_crystal_size_max          0.97
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0313P)^2^+0.3095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1154
_reflns_number_total             1156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02405f2.cif
_cod_data_source_block           250918b
_cod_database_code               7719955
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C12 h12 N2 O4 Cu1 '
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.178
_diffrn_oxdiff_digest_hkl
;
43bcc208b32a2a75337e12a6a81da2ce36ad24
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name 250918b.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C1(H1)
;
_shelx_res_checksum              54194
_shelx_hkl_checksum              73645
_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 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.716