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_7249808
_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 N6 Ni, C6 H Cl2 O4, C3 H Cl O2, C3 Cl O2, H2 O'
_chemical_formula_sum            'C42 H26 Cl4 N6 Ni O9'
_chemical_formula_weight         959.20
_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             2024-06-24
_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                85.086(2)
_cell_angle_beta                 80.136(2)
_cell_angle_gamma                85.180(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9581(3)
_cell_length_b                   11.0350(3)
_cell_length_c                   20.9833(5)
_cell_measurement_reflns_used    12079
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.2750
_cell_measurement_theta_min      2.0310
_cell_volume                     2030.99(10)
_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      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.935
_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     72.00 109.00   0.50   26.00    --   20.00  54.00 156.45   74
  2  \w    -72.00 -26.00   0.50   26.00    --   20.00  54.00  49.05   92
  3  \w      7.00 109.00   0.50   26.00    --   20.00  54.00  49.05  204
  4  \w    -70.00 -32.00   0.50   26.00    --   20.00  54.00 -90.00   76
  5  \w     28.00  75.00   0.50   26.00    --   20.00  54.00 -90.00   94
  6  \w    -72.00   5.00   0.50   26.00    --   20.00  54.00  -9.64  154
  7  \w     27.00  53.00   0.50   26.00    --   20.00  54.00  -9.64   52
  8  \w    -74.00 -17.00   0.50   26.00    --   20.00  54.00 120.00  114
  9  \w    -12.00  60.00   0.50   26.00    --   20.00  54.00 120.00  144
 10  \w    -73.00  74.00   0.50   26.00    --   20.00  54.00-150.00  294
 11  \w    -70.00 -45.00   0.50   26.00    --   20.00  54.00 -60.00   50
 12  \w    -18.00   7.00   0.50   26.00    --   20.00  54.00 -60.00   50
 13  \w     26.00  51.00   0.50   26.00    --   20.00  54.00 -60.00   50
 14  \w     69.00  94.00   0.50   26.00    --   20.00  54.00 -60.00   50
 15  \w    -63.00 -16.00   0.50   26.00    --   20.00  54.00  60.00   94
 16  \w     21.00  51.00   0.50   26.00    --   20.00  54.00  60.00   60
 17  \w    -65.00 -38.00   0.50   26.00    --   20.00  54.00 -30.00   54
 18  \w     82.00 107.00   0.50   26.00    --   20.00  54.00 -30.00   50
 19  \w    -71.00  49.00   0.50   26.00    --   20.00  54.00-180.00  240
 20  \w     21.00  52.00   0.50   26.00    --   20.00  54.00 156.45   62
;
_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      -0.0079681000
_diffrn_orient_matrix_UB_12      0.0051182000
_diffrn_orient_matrix_UB_13      0.0339005000
_diffrn_orient_matrix_UB_21      0.0033677000
_diffrn_orient_matrix_UB_22      0.0641157000
_diffrn_orient_matrix_UB_23      -0.0054492000
_diffrn_orient_matrix_UB_31      -0.0801028000
_diffrn_orient_matrix_UB_32      0.0067823000
_diffrn_orient_matrix_UB_33      0.0021181000
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.935
_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            36938
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79625
_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    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         11630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0458P)^2^+1.4601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9556
_reflns_number_total             11630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01214c2.cif
_cod_data_source_block           exp_709
_cod_depositor_comments
'Adding full bibliography for 7249805--7249810.cif.'
_cod_database_code               7249808
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C30H30N10O10Ni1Cl2
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.643
_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:
 C22(H22), C16(H16), C19(H19), C24(H24), C23(H23), C4(H4), C7(H7), C18(H18),
 C1(H1), C15(H15), C17(H17), C9(H9), C27(H27), C30(H30), C8(H8), C12(H12),
 C3(H3), C2(H2), C28(H28), C29(H29), C14(H14), C13(H13)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_shelx_res_checksum              4738
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.865