#------------------------------------------------------------------------------
#$Date: 2026-04-05 14:04:06 +0200 (Sun 05 de Apr de 2026) $
#$Revision: 305366 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/00/7720015.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7720015
loop_
_publ_author_name
'Zhou, Jing-Yao'
'Zhang, Hong-Dong'
'Yin, Fan'
'Zhu, Zheng-Zhong'
'Zhou, Li-Peng'
'Tian, Chong-Bin'
'Sun, Qing-Fu'
_publ_section_title
;
 Locking the spin states of anionic Fe(L)₂ 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         'C14 H14 Fe Li2 N18 O4, 4(H2 O)'
_chemical_formula_sum            'C14 H22 Fe Li2 N18 O8'
_chemical_formula_weight         640.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                   13.9830(5)
_cell_length_b                   21.1145(11)
_cell_length_c                   8.9586(4)
_cell_measurement_reflns_used    2673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.3900
_cell_measurement_theta_min      4.1800
_cell_volume                     2645.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.118a (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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     60.00  98.00   0.50    0.20    --  108.03-107.00 111.00   76
  2  ω     50.00 109.00   0.50    0.20    --  108.03-125.00-180.00  118
  3  ω   -149.00 -83.00   0.50    0.20    -- -105.00 -74.00-163.00  132
  4  ω   -171.00-127.00   0.50    0.20    -- -105.00 -51.00 -20.00   88
  5  ω    -58.00 -33.00   0.50    0.20    -- -105.00  51.00 124.00   50
  6  ω    -69.00 -42.00   0.50    0.20    -- -105.00  61.00 150.00   54
  7  ω     -2.00  23.00   0.50    0.05    --  -46.40  19.00 -60.00   50
  8  ω     82.00 108.00   0.50    0.05    --   46.40  51.00 124.00   52
  9  ω     38.00  64.00   0.50    0.05    --   46.40  51.00 124.00   52
 10  ω     -9.00  20.00   0.50    0.05    --   46.40 -19.00 -30.00   58
 11  ω    -29.00  27.00   0.50    0.05    --   46.40 -19.00 -90.00  112
 12  ω    -13.00  23.00   0.50    0.05    --   46.40 -19.00-180.00   72
 13  ω     38.00  79.00   0.50    0.20    --  108.03 -74.00-163.00   82
 14  ω     45.00  71.00   0.50    0.20    --  108.03 -61.00-120.00   52
 15  ω     45.00  70.00   0.50    0.20    --  108.03 -61.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4416
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.617
_diffrn_reflns_theta_min         6.230
_exptl_absorpt_coefficient_mu    5.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.118a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1341
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0364
_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/[σ²(Fo²)+(0.0688P)²+0.6368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1226
_reflns_number_total             1341
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00162a2.cif
_cod_data_source_block           Li
_cod_depositor_comments
'Adding full bibliography for 7720015--7720017.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               7720015
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.505
_shelx_estimated_absorpt_t_min   0.419
_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
 Li1-H1A \\sim Li1-H1B
 with sigma of 0.02
3.a Free rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
;
_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
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x, y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.250000 0.250000 0.01889(19) Uani 1 4 d S T P . .
N2 N 0.52500(10) 0.31600(7) 0.40115(17) 0.0236(3) Uani 1 1 d . . . . .
N5 N 0.62997(11) 0.37331(8) 0.52584(17) 0.0302(4) Uani 1 1 d . . . . .
N3 N 0.47755(11) 0.35414(8) 0.49333(18) 0.0288(4) Uani 1 1 d . . . . .
N1 N 0.63785(15) 0.250000 0.250000 0.0213(5) Uani 1 2 d S T P . .
N4 N 0.54030(11) 0.38820(8) 0.56827(18) 0.0315(4) Uani 1 1 d . . . . .
O2 O 0.68796(12) 0.56569(9) 0.5987(3) 0.0614(5) Uani 1 1 d G . . . .
H2A H 0.740807 0.585501 0.593999 0.092 Uiso 1 1 d G U . . .
H2B H 0.645858 0.593737 0.580781 0.092 Uiso 1 1 d G U . . .
C3 C 0.68609(12) 0.29120(8) 0.33670(17) 0.0236(4) Uani 1 1 d . . . . .
O1 O 0.61182(15) 0.48798(10) 0.8146(2) 0.0676(6) Uani 1 1 d G . . . .
H1A H 0.644968 0.515006 0.766920 0.101 Uiso 1 1 d DG U . . .
H1B H 0.642712 0.481924 0.895078 0.101 Uiso 1 1 d DG U . . .
C4 C 0.61813(11) 0.32874(8) 0.42315(19) 0.0238(4) Uani 1 1 d . . . . .
C2 C 0.78471(13) 0.29312(10) 0.3380(2) 0.0320(4) Uani 1 1 d . . . . .
H2 H 0.817200 0.322534 0.396291 0.038 Uiso 1 1 calc R U . . .
C1 C 0.83429(19) 0.250000 0.250000 0.0340(7) Uani 1 2 d S T P . .
H1 H 0.900796 0.250001 0.250000 0.041 Uiso 1 2 calc R U P . .
Li1 Li 0.500000 0.4452(3) 0.750000 0.0347(11) Uani 1 2 d DS T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 159.60(8) . 8_455 ?
N2 Fe1 N2 90.21(9) 8_455 6 ?
N2 Fe1 N2 93.39(9) . 6 ?
N2 Fe1 N2 90.21(9) . 3_655 ?
N2 Fe1 N2 159.60(8) 6 3_655 ?
N2 Fe1 N2 93.39(9) 8_455 3_655 ?
N1 Fe1 N2 100.20(4) 6 8_455 ?
N1 Fe1 N2 79.80(4) . . ?
N1 Fe1 N2 79.80(4) 6 3_655 ?
N1 Fe1 N2 79.80(4) . 8_455 ?
N1 Fe1 N2 100.20(4) 6 . ?
N1 Fe1 N2 79.80(4) 6 6 ?
N1 Fe1 N2 100.20(4) . 6 ?
N1 Fe1 N2 100.20(4) . 3_655 ?
N1 Fe1 N1 180.0 6 . ?
N3 N2 Fe1 139.86(12) . . ?
N3 N2 C4 105.71(14) . . ?
C4 N2 Fe1 114.42(12) . . ?
C4 N5 N4 104.19(14) . . ?
N4 N3 N2 108.32(14) . . ?
C3 N1 Fe1 120.05(11) . . ?
C3 N1 Fe1 120.05(11) 8_455 . ?
C3 N1 C3 119.9(2) 8_455 . ?
N5 N4 Li1 127.00(12) . . ?
N3 N4 N5 110.39(15) . . ?
N3 N4 Li1 121.90(13) . . ?
H2A O2 H2B 104.5 . . ?
N1 C3 C4 109.30(15) . . ?
N1 C3 C2 121.62(16) . . ?
C2 C3 C4 129.07(15) . . ?
H1A O1 H1B 104.5 . . ?
Li1 O1 H1A 128.0 . . ?
Li1 O1 H1B 127.3 . . ?
N2 C4 C3 116.37(15) . . ?
N5 C4 N2 111.39(15) . . ?
N5 C4 C3 132.21(15) . . ?
C3 C2 H2 120.8 . . ?
C3 C2 C1 118.33(18) . . ?
C1 C2 H2 120.8 . . ?
C2 C1 C2 120.2(2) . 8_455 ?
C2 C1 H1 119.9 . . ?
C2 C1 H1 119.9 8_455 . ?
N4 Li1 N4 110.1(3) . 3_656 ?
O1 Li1 N4 104.91(8) 3_656 . ?
O1 Li1 N4 106.75(9) 3_656 3_656 ?
O1 Li1 N4 104.91(8) . 3_656 ?
O1 Li1 N4 106.75(9) . . ?
O1 Li1 O1 123.1(3) 3_656 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9742(15) . ?
Fe1 N2 1.9743(15) 6 ?
Fe1 N2 1.9743(15) 8_455 ?
Fe1 N2 1.9743(15) 3_655 ?
Fe1 N1 1.928(2) 6 ?
Fe1 N1 1.928(2) . ?
N2 N3 1.331(2) . ?
N2 C4 1.344(2) . ?
N5 N4 1.347(2) . ?
N5 C4 1.326(2) . ?
N3 N4 1.318(2) . ?
N1 C3 1.3472(19) . ?
N1 C3 1.3472(19) 8_455 ?
N4 Li1 2.102(3) . ?
O2 H2A 0.8501 . ?
O2 H2B 0.8502 . ?
C3 C4 1.460(2) . ?
C3 C2 1.380(2) . ?
O1 H1A 0.8503 . ?
O1 H1B 0.8499 . ?
O1 Li1 1.896(3) . ?
C2 H2 0.9300 . ?
C2 C1 1.389(2) . ?
C1 H1 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 N3 N4 179.76(15) . . . . ?
Fe1 N2 C4 N5 -179.94(12) . . . . ?
Fe1 N2 C4 C3 -1.7(2) . . . . ?
Fe1 N1 C3 C4 2.07(15) . . . . ?
Fe1 N1 C3 C2 -179.10(13) . . . . ?
N2 N3 N4 N5 0.4(2) . . . . ?
N2 N3 N4 Li1 -170.53(18) . . . . ?
N3 N2 C4 N5 0.1(2) . . . . ?
N3 N2 C4 C3 178.32(15) . . . . ?
N1 C3 C4 N2 -0.1(2) . . . . ?
N1 C3 C4 N5 177.61(17) . . . . ?
N1 C3 C2 C1 -1.7(3) . . . . ?
N4 N5 C4 N2 0.1(2) . . . . ?
N4 N5 C4 C3 -177.70(18) . . . . ?
C3 N1 C3 C4 -177.93(15) 8_455 . . . ?
C3 N1 C3 C2 0.90(13) 8_455 . . . ?
C3 C2 C1 C2 0.84(13) . . . 8_455 ?
C4 N2 N3 N4 -0.33(19) . . . . ?
C4 N5 N4 N3 -0.3(2) . . . . ?
C4 N5 N4 Li1 170.05(19) . . . . ?
C4 C3 C2 C1 176.83(15) . . . . ?
C2 C3 C4 N2 -178.83(18) . . . . ?
C2 C3 C4 N5 -1.1(3) . . . . ?
