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_7249809
_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 Fe N6, 2(C3 Cl O2), 6(H2 O)'
_chemical_formula_sum            'C36 H34 Cl2 Fe N6 O10'
_chemical_formula_weight         837.44
_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_creation_date             2024-06-26
_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                91.6850(10)
_cell_angle_beta                 95.6840(10)
_cell_angle_gamma                90.432(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0180(2)
_cell_length_b                   9.02320(10)
_cell_length_c                   22.2494(3)
_cell_measurement_reflns_used    12428
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6700
_cell_measurement_theta_min      2.2550
_cell_volume                     1800.68(5)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.944
_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    -20.00  20.00   0.50   30.00    --   20.00  54.00  90.00   80
  2  \w    -74.00 -33.00   0.50   30.00    --   20.00  54.00-150.00   82
  3  \w    -23.00   3.00   0.50   30.00    --   20.00  54.00-150.00   52
  4  \w      8.00  34.00   0.50   30.00    --   20.00  54.00-150.00   52
  5  \w     85.00 110.00   0.50   30.00    --   20.00  54.00-150.00   50
  6  \w    -71.00  76.00   0.50   30.00    --   20.00  54.00 -30.00  294
  7  \w    -71.00 -13.00   0.50   30.00    --   20.00  54.00 -90.00  116
  8  \w      3.00  69.00   0.50   30.00    --   20.00  54.00 -90.00  132
  9  \w     85.00 110.00   0.50   30.00    --   20.00  54.00 -90.00   50
 10  \w    -71.00 -38.00   0.50   30.00    --   20.00  54.00  30.00   66
 11  \w    -25.00  79.00   0.50   30.00    --   20.00  54.00  30.00  208
 12  \w    -72.00  26.00   0.50   30.00    --   20.00  54.00 120.00  196
 13  \w     80.00 105.00   0.50   30.00    --   20.00  54.00 120.00   50
 14  \w    -65.00 -39.00   0.50   30.00    --   20.00  54.00-120.00   52
 15  \w     27.00  52.00   0.50   30.00    --   20.00  54.00-120.00   50
 16  \w    -63.00  98.00   0.50   30.00    --   20.00  54.00 150.00  322
 17  \w    -43.00 -18.00   0.50   30.00    --   20.00  54.00 -60.00   50
 18  \w     68.00  93.00   0.50   30.00    --   20.00  54.00 -60.00   50
 19  \w    -66.00  -2.00   0.50   30.00    --   20.00  54.00  60.00  128
 20  \w    -63.00 -38.00   0.50   30.00    --   20.00  54.00  90.00   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      -0.0375796000
_diffrn_orient_matrix_UB_12      -0.0343121000
_diffrn_orient_matrix_UB_13      -0.0263625000
_diffrn_orient_matrix_UB_21      0.0371822000
_diffrn_orient_matrix_UB_22      -0.0673339000
_diffrn_orient_matrix_UB_23      0.0068346000
_diffrn_orient_matrix_UB_31      -0.0587681000
_diffrn_orient_matrix_UB_32      -0.0217730000
_diffrn_orient_matrix_UB_33      0.0169006000
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.944
_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            34721
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.606
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94080
_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 violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0388P)^2^+0.7410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7616
_reflns_number_total             10443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01214c2.cif
_cod_data_source_block           exp_783
_cod_depositor_comments
'Adding full bibliography for 7249805--7249810.cif.'
_cod_database_code               7249809
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C30H30N20O20Cl2Fe1
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.702
_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:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O5(H5A,H5B), O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C30(H30), C9(H9), C1(H1), C22(H22), C24(H24), C8(H8),
 C7(H7), C12(H12), C27(H27), C23(H23), C29(H29), C17(H17), C28(H28), C4(H4),
 C2(H2), C19(H19), C18(H18), C14(H14), C13(H13), C3(H3)
;
_shelx_res_checksum              46010
_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 1.112
_oxdiff_exptl_absorpt_empirical_full_min 0.931