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_7719949
_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         '3(C20 H18 Co N8 O2), 6(H2 O), N O3'
_chemical_formula_sum            'C60 H66 Co3 N25 O15'
_chemical_formula_weight         1554.16
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2ppr8f
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.4927(7)
_cell_length_b                   24.4927(7)
_cell_length_c                   20.8894(7)
_cell_measurement_reflns_used    8706
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.0230
_cell_measurement_theta_min      3.6010
_cell_volume                     10852.5(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -126.00 -52.00   0.50    4.70    --  -51.87 -42.00 155.00  148
  2  \w    -78.00 -26.00   0.50    4.70    --  -92.65  80.00 127.00  104
  3  \w   -160.00 -98.00   0.50    4.70    --  -92.65 -79.00 -18.00  124
  4  \w     98.00 171.00   0.50    4.70    --  103.98  80.00 127.00  146
  5  \w    -23.00  22.00   0.50    4.70    --   51.37 -38.00   0.00   90
  6  \w    -73.00 -26.00   0.50    4.70    --  -92.65  77.00  60.00   94
  7  \w   -150.00 -92.00   0.50    4.70    --  -92.65 -15.00  60.00  116
  8  \w    -51.00 -21.00   0.50    4.70    --  -92.65  61.00-120.00   60
  9  \w   -124.00 -79.00   0.50    4.70    --  -51.87 -57.00   0.00   90
 10  \w   -124.00 -79.00   0.50    4.70    --  -51.87 -57.00 120.00   90
 11  \w   -150.00-125.00   0.50    4.70    --  -92.65 -15.00-120.00   50
 12  \w   -150.00 -92.00   0.50    4.70    --  -92.65 -15.00   0.00  116
 13  \w    -51.00 -21.00   0.50    4.70    --  -92.65  61.00 -30.00   60
 14  \w    103.00 150.00   0.50    4.70    --  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      -0.0445975000
_diffrn_orient_matrix_UB_12      0.0228922000
_diffrn_orient_matrix_UB_13      0.0243956000
_diffrn_orient_matrix_UB_21      -0.0425604000
_diffrn_orient_matrix_UB_22      -0.0647964000
_diffrn_orient_matrix_UB_23      0.0308341000
_diffrn_orient_matrix_UB_31      0.0384404000
_diffrn_orient_matrix_UB_32      0.0231995000
_diffrn_orient_matrix_UB_33      0.0624203000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17937
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.969
_diffrn_reflns_theta_min         5.912
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.000
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.691
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4812
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.000027(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2183
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0624P)^2^+83.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2025
_reflns_number_total             2183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02405f2.cif
_cod_data_source_block           250910c_yfl
_cod_original_cell_volume        10852.5(7)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7719949
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C22 H22 N8 O6 Co1 '
_shelx_estimated_absorpt_t_max   0.533
_shelx_estimated_absorpt_t_min   0.411
_diffrn_oxdiff_digest_hkl
;
4307e76b9f303c05be3d5697adefc9e6c7e39b
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name 250910c_YFL.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. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: O8(0.5)
4.a Free rotating group:
 O2(H2B,H2C)
4.b Ternary CH refined with riding coordinates:
 C6(H6)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C2(H2A), C8(H8), C4(H4), C9(H9), C3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78424
_shelx_hkl_checksum              83396
_shelx_fab_checksum              67553
_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 1.599
_oxdiff_exptl_absorpt_empirical_full_min 0.806