Locking the spin states of anionic Fe(L)<sub>2</sub> units in coordination polymers through alkali metal ion incorporation.
Zhou, Jing-Yao; Zhang, Hong-Dong; Yin, Fan; Zhu, Zheng-Zhong; Zhou, Li-Peng; Tian, Chong-Bin; Sun, Qing-Fu; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4319–4326; doi:10.1039/d6dt00162a

data_7720016
_publ_section_title
;
 Locking the spin states of anionic Fe(L)<sub>2</sub> units in
 coordination polymers through alkali metal ion incorporation.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4319
_journal_page_last               4326
_journal_paper_doi               10.1039/d6dt00162a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C16 H14 Fe K2 N18 O2'
_chemical_formula_sum            'C16 H14 Fe K2 N18 O2'
_chemical_formula_weight         624.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2026-01-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2026-01-20 deposited with the CCDC.	2026-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5376(6)
_cell_length_b                   8.0985(4)
_cell_length_c                   21.7556(10)
_cell_measurement_reflns_used    4173
_cell_measurement_temperature    240.00(10)
_cell_measurement_theta_max      66.0920
_cell_measurement_theta_min      4.5560
_cell_volume                     2385.16(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      240.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.947
_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     21.00  82.00   0.50    2.00    --   86.29 -71.00 170.00  122
  2  \w     13.00  38.00   0.50    2.00    --   86.29 -38.00  60.00   50
  3  \w     17.00  43.00   0.50    2.00    --   86.29 -38.00   0.00   52
  4  \w     13.00  42.00   0.50    2.00    --   86.29 -38.00 -90.00   58
  5  \w     15.00  41.00   0.50    2.00    --   86.29 -38.00-150.00   52
  6  \w     15.00  42.00   0.50    2.00    --   86.29 -38.00-180.00   54
  7  \w    114.00 152.00   0.50    2.00    --   86.29  71.00 -58.00   76
  8  \w     84.00 151.00   0.50    2.00    --   86.29 125.00-120.00  134
  9  \w     63.00 144.00   0.50    2.00    --   86.29  77.00  30.00  162
 10  \w     24.00  70.00   0.50    1.00    --   -1.56  71.00 -58.00   92
 11  \w    -62.00 -16.00   0.50    2.00    --  -89.42  57.00 -60.00   92
 12  \w    -88.00 -48.00   0.50    2.00    --  -89.42  71.00 -58.00   80
 13  \w    -43.00 -18.00   0.50    2.00    --  -89.42  38.00 -60.00   50
 14  \w    -43.00 -18.00   0.50    2.00    --  -89.42  38.00  60.00   50
 15  \w    -43.00 -18.00   0.50    2.00    --  -89.42  38.00  90.00   50
 16  \w    -41.00 -16.00   0.50    2.00    --  -89.42  38.00 150.00   50
 17  \w    -43.00 -18.00   0.50    2.00    --  -89.42  38.00 120.00   50
 18  \w     58.50  71.00   0.50    1.00    --   -1.56  38.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15217
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         67.635
_diffrn_reflns_theta_min         4.534
_exptl_absorpt_coefficient_mu    5.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3107
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.2751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2483
_reflns_number_total             3107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00162a2.cif
_cod_data_source_block           K
_cod_depositor_comments
'Adding full bibliography for 7720015--7720017.cif.'
_cod_database_code               7720016
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.469
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 K1-H1_$5
 2.98 with sigma of 0.04
 H1_$5-K1
 3.2 with sigma of 0.02
 H8B_$5-K1
 3.2 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              28500
_shelx_hkl_checksum              19256
_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
;