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_7719956
_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(C11 H12.5 Cu0.5 N4 O), 2(Cl O4)'
_chemical_formula_sum            'C22 H25 Cl2 Cu N8 O10'
_chemical_formula_weight         695.94
_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.cc2ppr7d
_audit_creation_date             2025-09-12
_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                 105.642(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4953(2)
_cell_length_b                   18.2777(3)
_cell_length_c                   12.5438(2)
_cell_measurement_reflns_used    15670
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1060
_cell_measurement_theta_min      3.6080
_cell_volume                     2758.72(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  (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -51.00 -21.00   0.50    0.51    --  -92.65  61.00 150.00   60
  2  \w    -51.00 -23.00   0.50    0.51    --  -92.65  61.00 120.00   56
  3  \w    -47.00 -21.00   0.50    0.51    --  -92.65  61.00  30.00   52
  4  \w    -51.00 -26.00   0.50    0.51    --  -92.65  61.00  90.00   50
  5  \w    -50.00 -22.00   0.50    0.51    --  -92.65  61.00 -60.00   56
  6  \w    -50.00 -21.00   0.50    0.51    --  -92.65  61.00 -90.00   58
  7  \w    -50.00 -23.00   0.50    0.51    --  -92.65  61.00-150.00   54
  8  \w    -47.00 -22.00   0.50    0.51    --  -92.65  61.00-120.00   50
  9  \w    -51.00 -24.00   0.50    0.51    --  -92.65  61.00   0.00   54
 10  \w    -92.00 -24.00   0.50    0.51    --  -92.65  89.00 -47.00  136
 11  \w    -92.00 -24.00   0.50    0.51    --  -92.65  89.00 -47.00  136
 12  \w    -55.00 -30.00   0.50    0.51    --  -51.87  89.00 -47.00   50
 13  \w   -148.00 -95.00   0.50    0.51    --  -92.65 -15.00 -90.00  106
 14  \w   -161.00 -97.00   0.50    0.51    --  -92.65 -89.00-162.00  128
 15  \w   -146.00 -93.00   0.50    0.51    --  -92.65 -15.00 -30.00  106
 16  \w   -123.00 -53.00   0.50    0.51    --  -51.87 -19.00  90.00  140
 17  \w    -14.00  75.00   0.50    0.51    --   51.37 -89.00-162.00  178
 18  \w    -14.00  75.00   0.50    0.51    --   51.37 -89.00-162.00  178
 19  \w     35.00  92.00   0.50    0.51    --  103.98 -89.00-162.00  114
 20  \w     37.00  89.00   0.50    0.51    --  103.98 -95.00-120.00  104
 21  \w     44.00  73.00   0.50    0.51    --  103.98 -77.00 120.00   58
 22  \w     41.00  66.00   0.50    0.51    --  103.98 -77.00  90.00   50
 23  \w     38.00  70.00   0.50    0.51    --  103.98 -77.00  60.00   64
 24  \w    -23.00  22.00   0.50    0.51    --   51.37 -38.00 120.00   90
 25  \w     41.00  66.00   0.50    0.51    --  103.98 -77.00 -60.00   50
 26  \w     43.00  68.00   0.50    0.51    --  103.98 -77.00 -90.00   50
 27  \w     37.00  63.00   0.50    0.51    --  103.98 -77.00-120.00   52
 28  \w    114.00 147.00   0.50    0.51    --  103.98  15.00 -60.00   66
 29  \w    108.00 135.00   0.50    0.51    --  103.98  15.00 -90.00   54
 30  \w    134.00 160.00   0.50    0.51    --  103.98  89.00 -47.00   52
 31  \w     80.00 124.00   0.50    0.51    --   51.37  57.00 -90.00   88
 32  \w     79.00 123.00   0.50    0.51    --   51.37  57.00   0.00   88
;
_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      -0.0638728000
_diffrn_orient_matrix_UB_12      0.0193209000
_diffrn_orient_matrix_UB_13      -0.1197440000
_diffrn_orient_matrix_UB_21      -0.0336658000
_diffrn_orient_matrix_UB_22      0.0740835000
_diffrn_orient_matrix_UB_23      0.0397943000
_diffrn_orient_matrix_UB_31      0.1057322000
_diffrn_orient_matrix_UB_32      0.0353871000
_diffrn_orient_matrix_UB_33      -0.0180044000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26789
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.976
_diffrn_reflns_theta_min         3.673
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.533
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.211
_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    1.676
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0624P)^2^+6.1354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4767
_reflns_number_total             5224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02405f2.cif
_cod_data_source_block           250911c_yfl
_cod_database_code               7719956
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Cu C N O H Cl'
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.530
_diffrn_oxdiff_digest_hkl
;
4397ad1cb6e4d08eba56a8fbf307e7c067f0d1
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name 250911c_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
{C1X, C1XA}
{C2X, C2XA}
3. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O1A)
Uanis(O2) = Uanis(O2A)
Uanis(C1X) = Uanis(C1XA)
Uanis(C2X) = Uanis(C2XA)
Uanis(C5) = Uanis(C5A)
Uanis(C15) = Uanis(C15A)
Uanis(N4) = Uanis(N4A)
Uanis(N8) = Uanis(N8A)
4. Others
 Fixed Sof: O1(0.5) O1A(0.5) O2(0.5) O2A(0.5) N4(0.5) H4(0.5) N4A(0.5) N8(0.5)
 H8(0.5) N8A(0.5) C1X(0.5) H1XA(0.5) H1XB(0.5) H1XC(0.5) C5(0.5) H5(0.5)
 C5A(0.5) H5A(0.5) C2X(0.5) H2XA(0.5) H2XB(0.5) H2XC(0.5) C15(0.5) H15(0.5)
 C15A(0.5) H15A(0.5) C1XA(0.5) H1XD(0.5) H1XE(0.5) H1XF(0.5) C2XA(0.5)
 H2XD(0.5) H2XE(0.5) H2XF(0.5)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C15(H15)
5.b Me refined with riding coordinates:
 C1X(H1XA,H1XB,H1XC), C2X(H2XA,H2XB,H2XC), C1XA(H1XD,H1XE,H1XF), C2XA(H2XD,
 H2XE,H2XF)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N7(H7), N8(H8), C1(H1), C2(H2), C3(H3A), C5A(H5A), C7(H7A),
 C8(H8A), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15A(H15A), C17(H17),
 C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              87747
_shelx_hkl_checksum              30579
_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 1.638
_oxdiff_exptl_absorpt_empirical_full_min 0.500