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_7249810
_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, 2(C3 Cl O2), 6(H2 O)'
_chemical_formula_sum            'C36 H34 Cl2 Co N6 O10'
_chemical_formula_weight         840.52
_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     iterative
_audit_creation_date             2024-06-27
_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                92.0770(12)
_cell_angle_beta                 95.9851(11)
_cell_angle_gamma                90.5673(11)
_cell_formula_units_Z            2
_cell_length_a                   9.03554(12)
_cell_length_b                   9.04710(13)
_cell_length_c                   22.3304(3)
_cell_measurement_reflns_used    14361
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.6200
_cell_measurement_theta_min      2.2540
_cell_volume                     1814.09(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.950
_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    -74.00 107.00   0.50   25.00    --   20.00  54.00-116.41  362
  2  \w    -74.00   5.00   0.50   25.00    --   20.00  54.00 -60.00  158
  3  \w     15.00  84.00   0.50   25.00    --   20.00  54.00 -60.00  138
  4  \w    -73.00  75.00   0.50   25.00    --   20.00  54.00-180.00  296
  5  \w    -69.00   2.00   0.50   25.00    --   20.00  54.00 -30.00  142
  6  \w     22.00  47.00   0.50   25.00    --   20.00  54.00 -30.00   50
  7  \w     77.00 102.00   0.50   25.00    --   20.00  54.00 -30.00   50
  8  \w    -73.00 -17.00   0.50   25.00    --   20.00  54.00  60.00  112
  9  \w     56.00 109.00   0.50   25.00    --   20.00  54.00  60.00  106
 10  \w      6.00  93.00   0.50   25.00    --   20.00  54.00-150.00  174
 11  \w    -63.00 -37.00   0.50   25.00    --   20.00  54.00 120.00   52
 12  \w      8.00  78.00   0.50   25.00    --   20.00  54.00 120.00  140
 13  \w    -60.00 -34.00   0.50   25.00    --   20.00  54.00   0.00   52
 14  \w      0.00  25.00   0.50   25.00    --   20.00  54.00   0.00   50
 15  \w    -40.00 -15.00   0.50   25.00    --   20.00  54.00-120.00   50
 16  \w     25.00  50.00   0.50   25.00    --   20.00  54.00-120.00   50
 17  \w    -68.00  24.00   0.50   25.00    --   20.00  54.00 107.90  184
;
_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      0.0526315000
_diffrn_orient_matrix_UB_12      0.0408135000
_diffrn_orient_matrix_UB_13      -0.0144114000
_diffrn_orient_matrix_UB_21      -0.0587780000
_diffrn_orient_matrix_UB_22      0.0325705000
_diffrn_orient_matrix_UB_23      -0.0183405000
_diffrn_orient_matrix_UB_31      -0.0025341000
_diffrn_orient_matrix_UB_32      0.0585607000
_diffrn_orient_matrix_UB_33      0.0218496000
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35106
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.532
_diffrn_reflns_theta_min         2.253
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91913
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0006(4)
_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   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10517
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0369P)^2^+0.6483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8338
_reflns_number_total             10517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01214c2.cif
_cod_data_source_block           exp_693
_cod_depositor_comments
'Adding full bibliography for 7249805--7249810.cif.'
_cod_database_code               7249810
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C30H30N10O20Co1Cl2
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.683
_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. Restrained distances
 O10-H10A = O10-H10B
 0.85 with sigma of 0.02
 O9-H9A = O9-H9B
 0.85 with sigma of 0.02
 O7-H7A = O7-H7B
 0.85 with sigma of 0.02
 O8-H8A = O8-H8B
 0.85 with sigma of 0.02
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
 O6-H6A = O6-H6B
 0.85 with sigma of 0.02
 H10A-H10B
 1.34 with sigma of 0.04
 H9A-H9B
 1.34 with sigma of 0.04
 H7A-H7B
 1.34 with sigma of 0.04
 H8A-H8B
 1.34 with sigma of 0.04
 H5A-H5B
 1.34 with sigma of 0.04
 H6A-H6B
 1.34 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C16(H16), C9(H9), C22(H22), C1(H1), C30(H30), C7(H7),
 C19(H19), C17(H17), C14(H14), C27(H27), C8(H8), C15(H15), C18(H18), C2(H2),
 C13(H13), C29(H29), C3(H3), C12(H12), C4(H4), C28(H28)
;
_shelx_res_checksum              9841
_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 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.932