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_7249805
_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, C6 H Cl2 O4, C3 Cl0.989 O2, H2 O, C3 H Cl O2'
_chemical_formula_sum            'C42 H26 Cl4 Fe N6 O9'
_chemical_formula_weight         956.16
_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.cc2kq33j
_audit_creation_date             2024-07-31
_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                85.702(2)
_cell_angle_beta                 80.124(2)
_cell_angle_gamma                85.417(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9753(2)
_cell_length_b                   10.8907(2)
_cell_length_c                   20.9485(4)
_cell_measurement_reflns_used    12707
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.4440
_cell_measurement_theta_min      2.0740
_cell_volume                     2006.95(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      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.942
_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     85.00 110.00   0.50   28.00    --   20.00  54.00 -90.00   50
  2  \w    -74.00 107.00   0.50   28.00    --   20.00  54.00 150.00  362
  3  \w    -73.00  29.00   0.50   28.00    --   20.00  54.00  30.00  204
  4  \w    -69.00  95.00   0.50   28.00    --   20.00  54.00-150.00  328
  5  \w    -72.00  11.00   0.50   28.00    --   20.00  54.00 -30.00  166
  6  \w     44.00  71.00   0.50   28.00    --   20.00  54.00 -30.00   54
  7  \w    -64.00 -35.00   0.50   28.00    --   20.00  54.00  60.00   58
  8  \w     20.00  67.00   0.50   28.00    --   20.00  54.00  60.00   94
  9  \w    -74.00 -42.00   0.50   28.00    --   20.00  54.00 -60.00   64
 10  \w     -1.00  36.00   0.50   28.00    --   20.00  54.00 -60.00   74
 11  \w    -63.00 -38.00   0.50   28.00    --   20.00  54.00   0.00   50
 12  \w     70.00  97.00   0.50   28.00    --   20.00  54.00   0.00   54
 13  \w    -71.00 -44.00   0.50   28.00    --   20.00  54.00 120.00   54
 14  \w    -17.00  11.00   0.50   28.00    --   20.00  54.00 120.00   56
 15  \w    -43.00 -18.00   0.50   28.00    --   20.00  54.00-180.00   50
 16  \w     31.00  56.00   0.50   28.00    --   20.00  54.00-180.00   50
 17  \w    -74.00  33.00   0.50   28.00    --   20.00  54.00 -90.00  214
;
_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      -0.0328982000
_diffrn_orient_matrix_UB_12      0.0602356000
_diffrn_orient_matrix_UB_13      -0.0060659000
_diffrn_orient_matrix_UB_21      -0.0201388000
_diffrn_orient_matrix_UB_22      0.0064043000
_diffrn_orient_matrix_UB_23      0.0338955000
_diffrn_orient_matrix_UB_31      0.0705473000
_diffrn_orient_matrix_UB_32      0.0248258000
_diffrn_orient_matrix_UB_33      0.0003118000
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.942
_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            35122
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         2.178
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54444
_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    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11624
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0638P)^2^+1.2101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9355
_reflns_number_total             11624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01214c2.cif
_cod_data_source_block           exp_729
_cod_depositor_comments
'Adding full bibliography for 7249805--7249810.cif.'
_cod_database_code               7249805
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C30H30N10O20Cl2Fe1
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.676
_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. Restrained distances
 O1A-C31 \\sim O1B-C31
 with sigma of 0.02
 C32-Cl1A \\sim C32-Cl1B
 with sigma of 0.02
3. Others
 Fixed Sof: O1A(0.5) H1A(0.5) Cl1A(0.5) O2B(0.5) O2A(0.5) O1B(0.5) H1B(0.5)
 Cl1B(0.5)
4.a Free rotating group:
 O9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C1(H1), C22(H22), C19(H19), C15(H15), C7(H7), C18(H18), C30(H30),
 C8(H8), C17(H17), C23(H23), C24(H24), C9(H9), C12(H12), C27(H27), C29(H29),
 C3(H3), C28(H28), C2(H2), C14(H14), C13(H13)
4.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1B)
4.d Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_shelx_res_checksum              53743
_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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.679