Structural analysis and water adsorption properties of chloranilate anion–terpyridine metal complexes forming hydrogen-bonded frameworks
Mishima, Akio; Mori, Runa; Kanazashi, Ken; Hamaguchi, Tomohiko; Ishikawa, Ryuta; Kawata, Satoshi; CrystEngComm 27 (2025) 931–938; doi:10.1039/D4CE01214C

data_7249806
_publ_section_title
;
 Structural analysis and water adsorption properties of chloranilate
 anion--terpyridine metal complexes forming hydrogen-bonded frameworks
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              931
_journal_page_last               938
_journal_paper_doi               10.1039/D4CE01214C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'C30 H22 Co N6, C6 H Cl2 O4, C3 H Cl O2, C3 Cl O2, H2 O'
_chemical_formula_sum            'C42 H26 Cl4 Co N6 O9'
_chemical_formula_weight         959.42
_chemical_name_systematic
'[Co(C15N3H11)2](C6O4H2Cl2)0.5(C6O4HCl2)(C6O4Cl2)0.5(H2O)'
_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.cc2kq47p
_audit_creation_date             2024-06-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                85.6270(10)
_cell_angle_beta                 80.052(2)
_cell_angle_gamma                85.213(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9669(2)
_cell_length_b                   10.9875(2)
_cell_length_c                   20.9096(4)
_cell_measurement_reflns_used    12454
_cell_measurement_temperature    292.6(3)
_cell_measurement_theta_max      30.5710
_cell_measurement_theta_min      2.0080
_cell_volume                     2018.03(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.6(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.945
_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      9.00  51.00   0.50   25.00    --   20.00  54.00-161.22   84
  2  \w     59.00 110.00   0.50   25.00    --   20.00  54.00-161.22  102
  3  \w    -74.00 -14.00   0.50   25.00    --   20.00  54.00-132.08  120
  4  \w     30.00  56.00   0.50   25.00    --   20.00  54.00-132.08   52
  5  \w    -73.00  64.00   0.50   25.00    --   20.00  54.00 150.00  274
  6  \w     75.00 107.00   0.50   25.00    --   20.00  54.00 150.00   64
  7  \w    -70.00 -27.00   0.50   25.00    --   20.00  54.00 -60.00   86
  8  \w    -16.00  13.00   0.50   25.00    --   20.00  54.00 -60.00   58
  9  \w     19.00  44.00   0.50   25.00    --   20.00  54.00 -60.00   50
 10  \w    -63.00  99.00   0.50   25.00    --   20.00  54.00 -30.00  324
 11  \w    -64.00 -38.00   0.50   25.00    --   20.00  54.00 120.00   52
 12  \w     75.00 107.00   0.50   25.00    --   20.00  54.00 120.00   64
 13  \w    -72.00  85.00   0.50   25.00    --   20.00  54.00  30.00  314
 14  \w    -61.00 -34.00   0.50   25.00    --   20.00  54.00-180.00   54
 15  \w     20.00  45.00   0.50   25.00    --   20.00  54.00-180.00   50
 16  \w    -72.00 -47.00   0.50   25.00    --   20.00  54.00 -90.00   50
 17  \w      1.00  49.00   0.50   25.00    --   20.00  54.00 -90.00   96
 18  \w    -70.00  49.00   0.50   25.00    --   20.00  54.00  90.00  238
 19  \w    -33.00  -8.00   0.50   25.00    --   20.00  54.00-161.22   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081807000
_diffrn_orient_matrix_UB_12      0.0639001000
_diffrn_orient_matrix_UB_13      -0.0020312000
_diffrn_orient_matrix_UB_21      0.0285836000
_diffrn_orient_matrix_UB_22      -0.0019603000
_diffrn_orient_matrix_UB_23      -0.0337513000
_diffrn_orient_matrix_UB_31      -0.0748261000
_diffrn_orient_matrix_UB_32      0.0112349000
_diffrn_orient_matrix_UB_33      -0.0068967000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38624
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       plate
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+1.5965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9014
_reflns_number_total             11660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01214c2.cif
_cod_data_source_block           exp_698
_cod_depositor_comments
'Adding full bibliography for 7249805--7249810.cif.'
_cod_database_code               7249806
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C30H30N10O10Co1Cl2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C16(H16), C12(H12), C24(H24), C7(H7), C15(H15), C23(H23),
 C18(H18), C17(H17), C30(H30), C8(H8), C27(H27), C4(H4), C1(H1), C13(H13),
 C28(H28), C29(H29), C14(H14), C2(H2), C3(H3)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O3(H3A)
;
_shelx_res_checksum              62186
_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 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.873