#------------------------------------------------------------------------------
#$Date: 2026-09-22 22:15:14 +0100 (Tue, 22 Sep 2026) $
#$Revision: 306895 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023569.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023569
loop_
_publ_author_name
'Thiam, Mariama'
'Diouf, Ngon\'e'
'Orton, James'
'Ndoye, Cheikh'
'Gueye, Amadou'
'Diouf, Ousmane'
'Thiam, Ibrahima Elhadji'
'Gaye, Mohamed'
'Coles, Simon'
_publ_section_title
;
Structures of bimetallic FeIII--FeIII and trimetallic FeIII--K--FeIII
complexes incorporating the deprotonated ligand
N,N′-bis(2-hydroxy-3-methoxybenzylidene)-1,2-phenylenediamine
;
_journal_coeditor_code HB8251
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989026009734
_journal_volume 82
_journal_year 2026
_chemical_formula_iupac '[K Fe2 (C22 H18 N2 O4)2 Cl2] N O3'
_chemical_formula_moiety 'C44 H36 Cl2 Fe2 K N4 O8 +, N O3 -'
_chemical_formula_sum 'C44 H36 Cl2 Fe2 K N5 O11'
_chemical_formula_weight 1032.48
_chemical_name_systematic
'Dichloridobis(\m-2-{[2-(3-methoxy-2-oxidobenzylideneamino)phenylimino]methyl}-6-methoxyphenolato)diiron(III)potassium(I) nitrate'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 103.438(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.5443(8)
_cell_length_b 10.0392(5)
_cell_length_c 24.4944(13)
_cell_measurement_reflns_used 6255
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 37.9710
_cell_measurement_theta_min 2.3650
_cell_volume 4196.1(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)
;
_computing_data_collection
'CrysAlisPro system (CCD 43.124a 64-bit (release 23-05-2024))'
_computing_data_reduction
;
CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku FRE+ '
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0276
_diffrn_reflns_av_unetI/netI 0.0192
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 59339
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 36.318
_diffrn_reflns_theta_min 1.710
_exptl_absorpt_coefficient_mu 0.989
_exptl_absorpt_correction_T_max 0.952
_exptl_absorpt_correction_T_min 0.888
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour dark-red
_exptl_crystal_density_diffrn 1.634
_exptl_crystal_description '(cut) irregular block'
_exptl_crystal_F_000 2112
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.570
_refine_diff_density_min -0.318
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 314
_refine_ls_number_reflns 10162
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.041
_refine_ls_R_factor_all 0.0378
_refine_ls_R_factor_gt 0.0309
_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^)+(0.0500P)^2^+1.8043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0842
_refine_ls_wR_factor_ref 0.0873
_reflns_number_gt 8768
_reflns_number_total 10162
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8251.cif
_cod_data_source_block 3
_cod_database_code 2023569
_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_min 0.812
_shelx_estimated_absorpt_t_max 0.943
_shelx_hkl_file
;
0 0 -2 192.39 4.76
0 0 -2 192.22 4.83
0 0 -3 0.07 0.11
0 0 3 -0.09 0.08
0 0 3 -0.26 0.28
0 0 -3 -0.04 0.36
0 0 4 276.03 6.68
0 0 4 260.95 6.50
0 0 -4 259.96 6.50
0 0 4 259.65 6.62
0 0 -4 259.10 6.65
0 0 5 0.04 0.16
0 0 5 0.01 0.17
0 0 -5 -0.02 0.17
0 0 5 -0.20 0.49
0 0 5 -0.04 0.65
0 0 -5 -0.13 0.61
0 0 6 545.54 13.51
0 0 -6 530.25 13.50
0 0 -6 563.52 13.45
0 0 -6 524.45 13.72
0 0 6 529.14 13.50
0 0 6 546.21 13.77
0 0 -7 -0.13 0.23
0 0 7 0.08 0.20
0 0 -7 0.10 0.74
0 0 7 -0.01 0.21
0 0 -8 2401.54 61.60
0 0 8 2397.14 61.30
0 0 -9 0.74 0.85
0 0 9 0.25 0.42
0 0 9 0.01 0.26
0 0 10 0.63 0.26
0 0 -10 1.16 0.92
0 0 10 0.48 0.30
0 0 -11 0.22 0.96
0 0 11 0.33 0.33
0 0 -12 7.89 1.14
0 0 12 8.09 0.52
0 0 13 -0.22 0.18
0 0 -13 -0.22 1.07
0 0 13 0.10 0.39
0 0 14 559.15 13.74
0 0 -14 540.49 14.53
0 0 14 544.79 13.95
0 0 -15 -0.20 1.15
0 0 15 0.09 0.19
0 0 15 0.36 1.09
0 0 15 -0.10 0.45
0 0 -16 21.83 1.65
0 0 16 21.47 0.66
0 0 16 21.64 1.51
0 0 16 20.19 0.95
0 0 -17 0.96 1.31
0 0 17 -0.47 0.57
0 0 17 0.30 0.22
0 0 17 0.33 1.13
0 0 18 277.80 7.40
0 0 -18 256.76 8.03
0 0 18 271.01 7.25
0 0 18 280.29 6.92
0 0 18 266.40 7.62
0 0 19 -0.48 0.63
0 0 -19 -0.19 1.49
0 0 19 0.17 0.23
0 0 19 -0.13 0.61
0 0 20 79.65 2.67
0 0 20 77.83 2.32
0 0 -20 76.39 3.45
0 0 20 79.78 2.56
0 0 20 83.32 2.15
0 0 20 81.44 2.72
0 0 21 0.08 0.49
0 0 21 -0.50 0.75
0 0 -21 -0.11 1.66
0 0 21 0.29 0.27
0 0 21 -0.26 0.76
0 0 22 541.96 14.06
0 0 -22 560.23 15.23
0 0 22 546.46 14.24
0 0 22 547.07 14.26
0 0 23 0.54 0.73
0 0 -23 -0.50 1.89
0 0 23 -0.46 0.78
0 0 23 0.47 0.79
0 0 24 4.00 0.84
0 0 -24 3.35 2.03
0 0 24 1.69 0.79
0 0 24 2.11 0.83
0 0 25 -0.90 0.78
0 0 -25 -1.57 2.19
0 0 25 0.53 0.78
0 0 25 0.18 0.30
0 0 25 -0.46 0.79
0 0 26 23.68 1.48
0 0 -26 26.48 2.78
0 0 26 23.36 1.34
0 0 26 21.58 0.80
0 0 26 25.06 1.50
0 0 27 0.87 0.94
0 0 -27 -0.63 2.30
0 0 27 -0.93 0.91
0 0 27 -0.06 0.35
0 0 -27 -0.47 0.67
0 0 28 378.84 10.67
0 0 28 399.51 9.82
0 0 -28 387.77 12.05
0 0 28 383.27 9.77
0 0 28 373.49 10.64
0 0 -28 387.19 10.16
0 0 29 -1.34 1.01
0 0 29 -0.73 0.42
0 0 29 -0.48 1.09
0 0 -29 -1.02 0.68
0 0 -30 67.70 4.29
0 0 30 62.77 2.65
0 0 30 60.97 1.79
0 0 30 56.19 2.60
0 0 31 0.55 1.55
0 0 -31 -2.14 2.71
0 0 31 -0.26 1.02
0 0 31 -0.52 1.07
0 0 32 17.95 2.08
0 0 -32 20.87 3.27
0 0 32 16.17 1.58
0 0 32 16.17 1.53
0 0 33 1.12 1.64
0 0 33 -0.47 1.11
0 0 33 -0.18 1.09
0 0 34 3.96 1.67
0 0 34 1.72 1.14
0 0 34 0.84 1.12
0 0 35 -0.86 1.59
0 0 35 0.20 1.16
0 0 35 -0.86 1.24
0 0 36 67.18 3.54
0 0 36 64.29 2.96
0 0 36 60.15 2.90
0 0 37 1.30 1.63
0 0 37 1.30 1.24
0 0 38 0.29 1.56
0 0 38 0.30 1.22
0 0 39 4.21 1.76
0 2 0 11.18 0.40
0 -2 0 12.45 0.40
0 -2 0 11.35 0.39
0 -2 0 11.15 0.74
0 2 0 11.21 0.37
0 2 0 11.68 0.37
0 -2 0 12.26 1.20
0 2 1 0.51 0.18
0 2 -1 0.47 0.20
0 -2 1 0.61 0.19
0 2 -1 0.60 0.10
0 -2 1 0.57 0.10
0 -2 -1 0.50 0.16
0 -2 1 0.36 0.16
0 2 -1 0.54 0.16
0 -2 1 0.56 0.16
0 -2 -1 0.02 0.58
0 2 1 0.60 0.15
0 -2 1 0.42 0.55
0 2 -1 0.49 0.15
0 -2 1 0.70 0.16
0 -2 -1 0.43 1.10
0 2 1 0.88 0.15
0 -2 2 806.95 19.88
0 2 -2 776.29 19.89
0 2 2 780.01 19.87
0 -2 -2 815.56 19.82
0 2 -2 802.57 19.85
0 -2 2 813.52 19.85
0 -2 2 792.16 19.87
0 -2 -2 802.19 20.05
0 -2 2 821.83 19.88
0 -2 -2 788.66 20.08
0 -2 2 781.15 20.01
0 2 -2 807.99 19.87
0 2 2 797.40 19.85
0 2 -2 811.52 19.87
0 -2 -2 801.34 20.45
0 -2 2 826.08 19.88
0 2 2 822.27 20.41
0 -2 -3 856.37 20.24
0 -2 3 774.33 20.27
0 -2 3 818.40 20.28
0 2 3 833.07 20.27
0 2 3 810.36 20.23
0 -2 3 825.68 20.26
0 2 -3 830.35 20.26
0 -2 -3 821.13 20.49
0 2 3 806.85 20.25
0 2 -3 828.76 20.24
0 -2 3 818.54 20.28
0 -2 3 782.71 20.39
0 -2 -3 807.71 20.89
0 -2 3 832.25 20.28
0 2 3 840.14 20.85
0 -2 -4 7.24 0.26
0 -2 4 6.88 0.28
0 -2 4 6.97 0.32
0 -2 -4 7.76 0.58
0 2 4 7.03 0.26
0 -2 4 7.36 0.30
0 2 -4 6.75 0.30
0 2 4 6.15 0.69
0 -2 -4 7.29 0.75
0 -2 4 7.34 0.31
0 2 -4 7.51 0.27
0 -2 4 7.06 0.52
0 -2 4 7.10 0.26
0 -2 4 7.54 0.31
0 -2 4 7.05 0.28
0 -2 -5 173.37 4.37
0 -2 5 177.30 4.38
0 -2 -5 176.44 4.38
0 -2 5 167.97 4.39
0 -2 -5 176.31 4.62
0 -2 5 165.42 4.40
0 2 -5 182.34 4.41
0 2 5 172.61 4.37
0 2 5 177.21 4.73
0 -2 5 173.69 4.36
0 -2 5 173.79 4.45
0 -2 5 175.26 4.40
0 2 -5 177.67 4.36
0 2 -5 176.31 4.37
0 2 5 174.44 5.12
0 -2 5 177.80 4.40
0 -2 5 176.45 4.38
0 -2 6 10.92 0.37
0 -2 -6 11.23 0.37
0 -2 -6 10.21 0.38
0 2 -6 10.97 0.44
0 -2 6 9.47 0.40
0 2 6 10.22 0.59
0 -2 -6 10.16 0.77
0 -2 -6 9.50 0.64
0 2 6 10.09 0.38
0 2 -6 11.33 0.43
0 2 6 10.12 0.88
0 -2 6 10.73 0.46
0 -2 6 11.24 0.35
0 2 6 9.06 1.49
0 -2 6 10.66 0.38
0 -2 -6 10.88 0.68
0 2 -7 1200.86 31.16
0 -2 -7 1215.64 31.13
0 -2 7 1277.96 31.12
0 -2 -7 1275.59 31.11
0 -2 7 1228.53 31.13
0 2 -7 1244.12 31.15
0 2 -7 1267.43 31.20
0 -2 -7 1252.76 31.29
0 2 7 1229.25 31.13
0 2 7 1351.39 31.59
0 -2 -7 1229.38 31.35
0 -2 7 1296.41 31.10
0 -2 -7 1287.15 31.33
0 -2 7 1303.31 31.10
0 2 7 1283.82 31.86
0 -2 -7 1249.33 31.31
0 -2 -7 1337.82 31.39
0 -2 7 1263.25 31.12
0 -2 -8 249.64 6.43
0 -2 8 259.48 6.40
0 2 -8 263.18 6.48
0 -2 -8 261.61 6.40
0 2 -8 254.52 6.45
0 -2 8 241.90 6.42
0 -2 -8 260.21 6.59
0 2 -8 255.71 6.50
0 2 8 256.94 6.62
0 -2 -8 258.52 6.71
0 2 8 257.75 6.44
0 -2 8 227.64 6.76
0 -2 -8 251.39 6.63
0 2 8 278.56 6.97
0 -2 -8 256.04 6.63
0 -2 8 264.12 6.40
0 -2 8 258.90 6.41
0 2 8 258.38 7.26
0 -2 -8 257.74 6.61
0 -2 -9 262.83 6.87
0 -2 -9 274.10 6.81
0 -2 9 276.93 6.82
0 2 -9 275.27 6.92
0 -2 9 264.82 6.85
0 2 -9 281.09 6.88
0 -2 -9 277.29 7.01
0 2 9 277.68 7.08
0 2 -9 271.23 6.92
0 -2 9 246.95 7.23
0 -2 -9 276.06 7.18
0 2 9 280.93 6.87
0 2 9 297.49 7.47
0 -2 -9 269.48 7.03
0 -2 -9 282.48 7.04
0 -2 9 273.25 6.84
0 2 9 268.56 7.15
0 -2 -9 277.62 7.04
0 2 9 276.65 7.72
0 -2 -10 260.59 6.74
0 -2 -10 267.30 6.66
0 2 -10 266.91 6.78
0 -2 10 271.08 6.67
0 -2 10 263.03 6.70
0 2 10 262.17 6.95
0 -2 -10 269.67 6.87
0 -2 -10 270.91 7.08
0 2 10 272.12 6.73
0 -2 -10 262.16 6.85
0 -2 -10 279.21 6.87
0 2 10 260.62 7.57
0 2 10 266.61 7.03
0 -2 -11 1194.30 29.97
0 -2 11 1227.79 29.88
0 2 -11 1206.03 30.01
0 -2 -11 1231.37 29.87
0 -2 11 1165.78 29.91
0 2 11 1208.34 30.18
0 2 11 1191.72 29.96
0 -2 -11 1264.58 30.36
0 -2 -11 1203.47 30.04
0 -2 -11 1253.19 30.06
0 2 11 1224.65 30.80
0 2 11 1215.09 30.27
0 -2 12 49.23 1.31
0 2 -12 52.06 1.47
0 -2 -12 50.32 1.30
0 -2 -12 48.25 1.41
0 -2 12 45.50 1.34
0 2 12 50.24 1.73
0 2 12 48.80 1.69
0 -2 -12 47.99 1.88
0 -2 -12 49.15 2.61
0 -2 -12 48.21 1.46
0 -2 -12 49.44 1.48
0 2 12 44.34 2.38
0 2 12 48.81 1.74
0 -2 -13 107.97 2.77
0 2 -13 110.07 2.95
0 -2 -13 106.08 2.90
0 -2 13 106.91 2.78
0 -2 13 108.97 2.74
0 -2 13 104.67 2.82
0 2 13 120.04 3.26
0 2 13 110.00 3.17
0 -2 -13 116.16 4.07
0 -2 -13 109.57 3.39
0 -2 -13 110.69 2.91
0 -2 -13 114.93 2.95
0 2 13 111.88 3.25
0 2 13 113.14 3.88
0 -2 -14 314.61 8.10
0 -2 -14 327.95 7.95
0 -2 14 318.09 7.96
0 2 -14 326.79 8.15
0 -2 14 321.44 7.91
0 -2 14 308.62 8.00
0 2 14 308.98 8.32
0 2 14 320.57 8.42
0 -2 -14 309.45 8.61
0 -2 -14 321.70 8.07
0 -2 -14 315.60 8.10
0 2 14 320.26 8.45
0 2 -15 166.52 4.16
0 -2 -15 150.77 4.10
0 -2 -15 153.42 3.91
0 -2 15 154.06 3.94
0 -2 15 153.18 3.99
0 2 15 161.08 4.46
0 2 15 149.12 4.33
0 -2 -15 153.73 3.89
0 -2 15 158.59 3.88
0 -2 -15 154.92 4.69
0 -2 -15 161.92 4.08
0 2 15 155.81 4.47
0 -2 16 45.74 1.16
0 -2 -16 44.37 1.18
0 2 16 49.10 1.79
0 2 16 45.43 1.68
0 -2 16 48.89 1.32
0 -2 -16 45.31 2.09
0 2 16 49.10 1.84
0 -2 -16 46.36 1.43
0 2 -16 45.18 1.46
0 -2 16 47.63 1.25
0 2 17 73.10 2.49
0 -2 -17 76.12 2.82
0 2 17 74.39 2.45
0 2 17 71.45 2.31
0 -2 -17 73.03 1.80
0 -2 -17 68.47 1.79
0 2 -17 74.83 2.12
0 -2 17 73.51 1.85
0 -2 -17 73.00 2.08
0 2 18 83.97 2.74
0 2 18 81.77 2.58
0 -2 18 88.55 2.88
0 -2 -18 79.00 3.11
0 2 18 81.44 2.78
0 -2 -18 80.76 2.35
0 2 -18 80.68 2.39
0 2 19 0.31 0.73
0 -2 -19 -0.24 1.29
0 -2 19 0.45 0.49
0 2 19 1.44 0.73
0 2 19 0.87 0.76
0 2 -19 0.48 0.41
0 -2 -19 0.62 0.41
0 -2 20 13.34 0.87
0 2 20 11.40 1.11
0 2 20 12.50 1.04
0 2 20 12.85 0.96
0 -2 -20 11.27 1.58
0 -2 20 11.81 0.78
0 -2 20 12.30 0.57
0 2 -20 13.52 0.74
0 -2 -20 13.01 0.71
0 2 21 109.63 3.74
0 2 21 113.93 3.74
0 2 21 114.03 3.46
0 -2 -21 111.04 4.24
0 -2 21 116.29 3.39
0 -2 21 123.76 3.18
0 -2 -21 116.74 3.31
0 2 -21 121.91 3.36
0 2 22 30.42 1.67
0 2 22 30.89 1.64
0 2 22 29.75 1.37
0 -2 -22 31.76 2.25
0 2 22 32.13 2.18
0 -2 22 29.34 1.30
0 -2 22 33.05 1.08
0 2 -22 33.39 1.28
0 -2 -22 33.07 1.25
0 2 23 13.76 1.22
0 -2 23 15.73 0.70
0 2 23 15.57 1.25
0 2 23 13.64 0.95
0 -2 -23 15.78 1.99
0 2 23 15.64 1.78
0 -2 23 14.35 0.91
0 -2 23 12.74 0.63
0 -2 -23 14.28 0.81
0 2 -23 13.72 0.84
0 -2 24 19.08 0.79
0 2 24 16.52 1.33
0 2 24 16.21 0.99
0 2 24 16.65 1.34
0 -2 -24 15.26 2.08
0 2 24 15.26 1.84
0 -2 24 16.90 1.00
0 -2 24 18.16 0.74
0 -2 -24 18.86 0.94
0 2 -24 16.79 0.94
0 -2 25 108.67 2.80
0 2 25 92.33 3.46
0 2 25 95.23 2.91
0 2 25 98.39 3.45
0 -2 25 91.30 3.01
0 2 25 98.39 4.08
0 -2 -25 99.85 4.26
0 -2 25 100.60 2.75
0 2 -25 97.03 2.97
0 -2 -25 98.44 2.95
0 -2 26 1.30 0.38
0 2 26 0.63 0.99
0 2 26 -0.24 1.57
0 -2 26 1.48 0.67
0 -2 -26 1.73 1.87
0 -2 26 1.74 0.36
0 2 -26 1.15 0.57
0 -2 -26 1.40 0.56
0 -2 27 6.53 0.53
0 2 27 4.52 1.12
0 -2 -27 4.69 2.11
0 -2 27 4.87 0.77
0 2 27 6.15 1.69
0 -2 27 5.12 0.47
0 2 -27 4.61 0.66
0 2 28 79.83 3.27
0 -2 28 89.99 2.47
0 -2 28 81.12 3.09
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28 2 -10 5.08 1.06
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28 -4 -14 17.19 1.36
28 4 -14 17.48 1.43
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28 4 -10 3.43 1.05
28 -4 -10 5.27 1.06
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28 4 -9 1.86 1.01
28 -4 -9 4.58 1.02
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28 4 -8 0.72 0.97
28 -4 -8 0.39 0.88
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28 -4 -7 2.04 0.95
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28 -4 -6 0.60 0.92
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28 -4 -5 9.27 1.13
28 4 -5 8.18 1.22
28 4 -4 11.81 1.28
28 -4 -4 11.59 1.20
28 4 -3 5.01 1.09
28 -4 -3 3.72 1.03
-29 1 13 6.31 2.85
-29 -1 13 5.11 2.78
-29 1 12 32.63 3.38
-29 -1 12 24.76 3.47
29 -1 -11 20.09 1.48
-29 1 11 18.57 3.02
-29 -1 11 20.58 3.14
29 1 -10 0.06 1.01
29 -1 -10 1.49 1.00
-29 1 10 -2.19 2.64
-29 -1 10 -0.78 2.69
-29 1 9 6.50 0.93
29 1 -9 8.54 1.16
29 -1 -9 9.00 1.16
-29 1 9 3.49 2.43
-29 -1 9 5.29 2.59
-29 1 8 6.83 0.94
29 1 -8 6.54 1.12
29 -1 -8 7.32 1.12
-29 1 8 9.16 2.45
-29 -1 8 9.46 2.63
-29 1 7 8.03 0.96
29 1 -7 8.05 1.12
29 -1 -7 7.13 1.14
-29 1 7 6.65 2.40
-29 -1 7 7.33 2.67
-29 1 6 4.49 2.24
-29 1 6 6.16 0.92
29 1 -6 4.96 1.09
29 -1 -6 6.87 1.13
-29 -1 6 4.78 2.31
-29 1 5 12.10 1.07
-29 -1 5 12.31 1.05
29 1 -5 11.61 1.25
29 -1 -5 10.21 1.21
0 0 0 0.00 0.00
TITL 2024ncs0409_1b in C2/c
REM C2/c (#15 in standard setting)
CELL 0.71075 17.544258 10.039176 24.494368 90.0000 103.4384 90.0000
ZERR 8.00 0.000819 0.000460 0.001256 0.0000 0.0050 0.0000
LATT 7
SYMM -x, y,-z+1/2
SFAC C H N O Cl K Fe
UNIT 176.00 144.00 20.00 44.00 8.00 4.00 8.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.06 0.12 0.22
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 79539
_shelx_res_file
;
TITL 2024ncs0409_1b_a.res in C2/c
a6k_no3.res
created by SHELXL-2018/3 at 09:02:56 on 17-Aug-2026
REM Old TITL 2024ncs0409_1b in C2/c
REM SHELXT solution in C2/c: R1 0.081, Rweak 0.003, Alpha 0.025
REM 0.410 for 254 systematic absences, Orientation as input
REM Formula found by SHELXT: C49 N6 O8 Cl2 K Fe2
CELL 0.71075 17.5443 10.0392 24.4944 90 103.438 90
ZERR 4 0.0008 0.0005 0.0013 0 0.005 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cl Fe K N O
UNIT 176 144 8 8 4 20 44
EQIV $1 1-X,+Y,0.5-Z
EQIV $2 -0.5+X,-0.5+Y,+Z
EQIV $3 1-X,1-Y,1-Z
EQIV $4 1-X,-Y,1-Z
EQIV $5 0.5-X,-0.5+Y,0.5-Z
L.S. 6 0 0
PLAN 5
SIZE 0.06 0.12 0.22
TEMP -173(2)
CONF
HTAB C3 O5_$2
HTAB C6 Cl1_$3
HTAB C7 Cl1_$3
HTAB C15 O6_$4
HTAB C19 Cl1_$5
HTAB C22 O7_$1
CONN 8 K1
HTAB
MORE -1
BOND $H
fmap 2 53
acta
OMIT -8 0 2
OMIT 3 5 1
OMIT 5 7 1
OMIT 17 7 18
REM
REM
REM
WGHT 0.050000 1.804300
FVAR 0.14950
C1 1 0.501930 0.247854 0.513062 11.00000 0.01571 0.01541 =
0.02062 0.00205 0.00508 0.00173
C2 1 0.446509 0.146405 0.495786 11.00000 0.01576 0.01535 =
0.02652 0.00228 0.00648 0.00127
C3 1 0.419831 0.071838 0.536092 11.00000 0.02237 0.02137 =
0.03598 0.00580 0.01247 -0.00092
AFIX 43
H3 2 0.382175 0.003222 0.524806 11.00000 -1.20000
AFIX 0
C4 1 0.448901 0.099251 0.592371 11.00000 0.02833 0.02837 =
0.03348 0.00831 0.01655 0.00268
AFIX 43
H4 2 0.431973 0.047444 0.619790 11.00000 -1.20000
AFIX 0
C5 1 0.502418 0.201270 0.609408 11.00000 0.02901 0.02635 =
0.02436 0.00413 0.01208 0.00597
AFIX 43
H5 2 0.520826 0.220049 0.648257 11.00000 -1.20000
AFIX 0
C6 1 0.529190 0.275918 0.570173 11.00000 0.02321 0.01997 =
0.02031 0.00068 0.00629 0.00167
AFIX 43
H6 2 0.565848 0.345765 0.581977 11.00000 -1.20000
AFIX 0
C7 1 0.585409 0.396906 0.480300 11.00000 0.01567 0.01705 =
0.01851 -0.00174 0.00344 -0.00116
AFIX 43
H7 2 0.613315 0.403463 0.518398 11.00000 -1.20000
AFIX 0
C8 1 0.613478 0.475165 0.439934 11.00000 0.01410 0.01547 =
0.02080 -0.00182 0.00437 -0.00182
C9 1 0.583261 0.462785 0.381730 11.00000 0.01365 0.01571 =
0.02097 -0.00053 0.00447 -0.00098
C10 1 0.614952 0.544460 0.345171 11.00000 0.01644 0.01862 =
0.02291 0.00138 0.00669 -0.00054
C11 1 0.672618 0.636598 0.366487 11.00000 0.01924 0.01939 =
0.03040 0.00089 0.00997 -0.00275
AFIX 43
H11 2 0.692316 0.692528 0.341650 11.00000 -1.20000
AFIX 0
C12 1 0.702313 0.648064 0.424712 11.00000 0.02128 0.02101 =
0.03254 -0.00368 0.00860 -0.00756
AFIX 43
H12 2 0.742020 0.711618 0.439103 11.00000 -1.20000
AFIX 0
C13 1 0.674115 0.567701 0.460857 11.00000 0.01953 0.02064 =
0.02489 -0.00484 0.00491 -0.00654
AFIX 43
H13 2 0.695403 0.574201 0.500138 11.00000 -1.20000
AFIX 0
C14 1 0.606178 0.610862 0.250213 11.00000 0.03314 0.02901 =
0.02785 0.00816 0.01232 -0.00117
AFIX 137
H14A 2 0.662778 0.603632 0.253535 11.00000 -1.50000
H14B 2 0.593072 0.702596 0.258218 11.00000 -1.50000
H14C 2 0.578244 0.586882 0.212015 11.00000 -1.50000
AFIX 0
C15 1 0.376621 0.030538 0.415357 11.00000 0.01593 0.01384 =
0.03527 0.00106 0.00215 -0.00079
AFIX 43
H15 2 0.360109 -0.028962 0.440487 11.00000 -1.20000
AFIX 0
C16 1 0.349710 0.005336 0.356316 11.00000 0.01589 0.01341 =
0.03649 -0.00231 -0.00118 -0.00044
C17 1 0.376159 0.077416 0.314713 11.00000 0.01454 0.01515 =
0.03204 -0.00628 -0.00022 0.00071
C18 1 0.345325 0.043982 0.257562 11.00000 0.01746 0.01804 =
0.03332 -0.00726 -0.00072 0.00283
C19 1 0.290852 -0.057245 0.243309 11.00000 0.02218 0.01937 =
0.03818 -0.00831 -0.00614 0.00056
AFIX 43
H19 2 0.270229 -0.078458 0.204915 11.00000 -1.20000
AFIX 0
C20 1 0.265827 -0.128843 0.285161 11.00000 0.02367 0.01791 =
0.04627 -0.00433 -0.00638 -0.00366
AFIX 43
H20 2 0.228562 -0.198452 0.274915 11.00000 -1.20000
AFIX 0
C21 1 0.294772 -0.099032 0.340673 11.00000 0.02012 0.01592 =
0.04449 -0.00167 -0.00270 -0.00303
AFIX 43
H21 2 0.277917 -0.148565 0.368758 11.00000 -1.20000
AFIX 0
C22 1 0.329251 0.110733 0.162004 11.00000 0.02766 0.04178 =
0.02845 -0.01726 0.00544 -0.00154
AFIX 137
H22A 2 0.350967 0.173913 0.139136 11.00000 -1.50000
H22B 2 0.274081 0.132198 0.159616 11.00000 -1.50000
H22C 2 0.333272 0.020085 0.148094 11.00000 -1.50000
AFIX 0
CL1 3 0.349507 0.417493 0.387302 11.00000 0.02003 0.02151 =
0.02147 -0.00103 -0.00090 0.00524
FE1 4 0.452674 0.285702 0.390541 11.00000 0.01339 0.01431 =
0.01887 -0.00074 0.00173 -0.00220
K1 5 0.500000 0.291938 0.250000 10.50000 0.02232 0.02485 =
0.01974 0.00000 0.00370 0.00000
N1 6 0.525057 0.317850 0.469139 11.00000 0.01405 0.01477 =
0.01850 0.00080 0.00273 -0.00040
N2 6 0.421956 0.128881 0.436954 11.00000 0.01428 0.01412 =
0.02748 0.00010 0.00288 -0.00060
PART -1
N3 6 0.745748 0.240740 0.500071 10.50000 0.01860 0.01484 =
0.02189 0.00260 0.00154 0.00012
O5 7 0.801899 0.321553 0.512336 10.50000 0.02571 0.02445 =
0.06332 0.00917 0.00408 -0.00676
O6 7 0.705833 0.219949 0.536026 10.50000 0.03185 0.03570 =
0.04279 0.01709 0.02027 0.00801
O7 7 0.730058 0.184680 0.454955 10.50000 0.05920 0.04494 =
0.02399 -0.00686 -0.00481 0.01270
PART 0
O1 7 0.527411 0.377413 0.359401 11.00000 0.01944 0.02421 =
0.01929 -0.00041 0.00270 -0.00853
O2 7 0.583500 0.522648 0.289376 11.00000 0.02627 0.02908 =
0.02041 0.00415 0.00605 -0.00649
O3 7 0.428675 0.173777 0.326377 11.00000 0.01930 0.02140 =
0.02708 -0.00733 0.00489 -0.00564
O4 7 0.372511 0.119558 0.219571 11.00000 0.02099 0.02788 =
0.02917 -0.00877 0.00123 -0.00055
HKLF 4
REM 2024ncs0409_1b_a.res in C2/c
REM wR2 = 0.0873, GooF = S = 1.041, Restrained GooF = 1.041 for all data
REM R1 = 0.0309 for 8768 Fo > 4sig(Fo) and 0.0378 for all 10162 data
REM 314 parameters refined using 0 restraints
END
WGHT 0.0500 1.8043
REM Instructions for potential hydrogen bonds
HTAB C3 O5_$2
HTAB C6 Cl1_$3
HTAB C7 Cl1_$3
HTAB C15 O6_$4
HTAB C19 Cl1_$5
HTAB C22 O7_$1
REM Highest difference peak 0.570, deepest hole -0.318, 1-sigma level 0.073
Q1 1 0.4844 0.2838 0.3803 11.00000 0.05 0.57
Q2 1 0.4740 0.1944 0.5015 11.00000 0.05 0.54
Q3 1 0.4425 0.3386 0.3811 11.00000 0.05 0.54
Q4 1 0.6398 0.5933 0.3570 11.00000 0.05 0.53
Q5 1 0.5160 0.3465 0.2578 11.00000 0.05 0.52
;
_shelx_res_checksum 91548
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.50193(5) 0.24785(9) 0.51306(4) 0.01710(13) Uani d 1 . .
C C2 0.44651(5) 0.14641(9) 0.49579(4) 0.01895(14) Uani d 1 . .
C C3 0.41983(6) 0.07184(10) 0.53609(5) 0.02564(18) Uani d 1 . .
H H3 0.382175 0.003222 0.524806 0.031 Uiso calc 1 . .
C C4 0.44890(7) 0.09925(11) 0.59237(5) 0.0285(2) Uani d 1 . .
H H4 0.431973 0.047444 0.619790 0.034 Uiso calc 1 . .
C C5 0.50242(7) 0.20127(10) 0.60941(4) 0.02561(18) Uani d 1 . .
H H5 0.520826 0.220049 0.648257 0.031 Uiso calc 1 . .
C C6 0.52919(6) 0.27592(9) 0.57017(4) 0.02096(15) Uani d 1 . .
H H6 0.565848 0.345765 0.581977 0.025 Uiso calc 1 . .
C C7 0.58541(5) 0.39691(9) 0.48030(4) 0.01716(13) Uani d 1 . .
H H7 0.613315 0.403463 0.518398 0.021 Uiso calc 1 . .
C C8 0.61348(5) 0.47516(8) 0.43993(4) 0.01674(13) Uani d 1 . .
C C9 0.58326(5) 0.46279(8) 0.38173(4) 0.01670(13) Uani d 1 . .
C C10 0.61495(5) 0.54446(9) 0.34517(4) 0.01898(14) Uani d 1 . .
C C11 0.67262(6) 0.63660(9) 0.36649(4) 0.02232(16) Uani d 1 . .
H H11 0.692316 0.692528 0.341650 0.027 Uiso calc 1 . .
C C12 0.70231(6) 0.64806(10) 0.42471(5) 0.02456(17) Uani d 1 . .
H H12 0.742020 0.711618 0.439103 0.029 Uiso calc 1 . .
C C13 0.67411(5) 0.56770(9) 0.46086(4) 0.02173(16) Uani d 1 . .
H H13 0.695403 0.574201 0.500138 0.026 Uiso calc 1 . .
C C14 0.60618(7) 0.61086(12) 0.25021(5) 0.0291(2) Uani d 1 . .
H H14A 0.662778 0.603632 0.253535 0.044 Uiso calc 1 . .
H H14B 0.593072 0.702596 0.258218 0.044 Uiso calc 1 . .
H H14C 0.578244 0.586882 0.212015 0.044 Uiso calc 1 . .
C C15 0.37662(5) 0.03054(9) 0.41536(5) 0.02230(16) Uani d 1 . .
H H15 0.360109 -0.028962 0.440487 0.027 Uiso calc 1 . .
C C16 0.34971(5) 0.00534(9) 0.35632(5) 0.02312(17) Uani d 1 . .
C C17 0.37616(5) 0.07742(9) 0.31471(4) 0.02150(16) Uani d 1 . .
C C18 0.34533(5) 0.04398(9) 0.25756(5) 0.02402(17) Uani d 1 . .
C C19 0.29085(6) -0.05724(10) 0.24331(5) 0.0287(2) Uani d 1 . .
H H19 0.270229 -0.078458 0.204915 0.034 Uiso calc 1 . .
C C20 0.26583(6) -0.12884(10) 0.28516(5) 0.0317(2) Uani d 1 . .
H H20 0.228562 -0.198452 0.274915 0.038 Uiso calc 1 . .
C C21 0.29477(6) -0.09903(10) 0.34067(5) 0.0285(2) Uani d 1 . .
H H21 0.277917 -0.148565 0.368758 0.034 Uiso calc 1 . .
C C22 0.32925(7) 0.11073(13) 0.16200(5) 0.0328(2) Uani d 1 . .
H H22A 0.350967 0.173913 0.139136 0.049 Uiso calc 1 . .
H H22B 0.274081 0.132198 0.159616 0.049 Uiso calc 1 . .
H H22C 0.333272 0.020085 0.148094 0.049 Uiso calc 1 . .
Cl Cl1 0.34951(2) 0.41749(2) 0.38730(2) 0.02194(5) Uani d 1 . .
Fe Fe1 0.45267(2) 0.28570(2) 0.39054(2) 0.01585(3) Uani d 1 . .
K K1 0.500000 0.29194(3) 0.250000 0.02250(5) Uani d 1 . .
N N1 0.52506(4) 0.31785(7) 0.46914(3) 0.01594(11) Uani d 1 . .
N N2 0.42196(4) 0.12888(7) 0.43695(3) 0.01895(13) Uani d 1 . .
N N3 0.7457(13) 0.2407(17) 0.5001(11) 0.0190(12) Uani d 0.5 A -1
O O5 0.80190(10) 0.32155(18) 0.51234(10) 0.0389(4) Uani d 0.5 A -1
O O6 0.70583(11) 0.21995(18) 0.53603(8) 0.0349(4) Uani d 0.5 A -1
O O7 0.73006(15) 0.1847(2) 0.45496(8) 0.0451(5) Uani d 0.5 A -1
O O1 0.52741(4) 0.37741(7) 0.35940(3) 0.02128(12) Uani d 1 . .
O O2 0.58350(4) 0.52265(8) 0.28938(3) 0.02515(14) Uani d 1 . .
O O3 0.42868(4) 0.17378(7) 0.32638(3) 0.02267(13) Uani d 1 . .
O O4 0.37251(4) 0.11956(8) 0.21957(3) 0.02677(14) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0157(3) 0.0154(3) 0.0206(3) 0.0017(2) 0.0051(3) 0.0021(3)
C2 0.0158(3) 0.0153(3) 0.0265(4) 0.0013(3) 0.0065(3) 0.0023(3)
C3 0.0224(4) 0.0214(4) 0.0360(5) -0.0009(3) 0.0125(4) 0.0058(3)
C4 0.0283(5) 0.0284(5) 0.0335(5) 0.0027(4) 0.0165(4) 0.0083(4)
C5 0.0290(4) 0.0264(4) 0.0244(4) 0.0060(3) 0.0121(4) 0.0041(3)
C6 0.0232(4) 0.0200(4) 0.0203(4) 0.0017(3) 0.0063(3) 0.0007(3)
C7 0.0157(3) 0.0171(3) 0.0185(3) -0.0012(2) 0.0034(3) -0.0017(3)
C8 0.0141(3) 0.0155(3) 0.0208(3) -0.0018(2) 0.0044(3) -0.0018(3)
C9 0.0136(3) 0.0157(3) 0.0210(3) -0.0010(2) 0.0045(3) -0.0005(3)
C10 0.0164(3) 0.0186(3) 0.0229(4) -0.0005(3) 0.0067(3) 0.0014(3)
C11 0.0192(3) 0.0194(4) 0.0304(4) -0.0028(3) 0.0100(3) 0.0009(3)
C12 0.0213(4) 0.0210(4) 0.0325(5) -0.0076(3) 0.0086(3) -0.0037(3)
C13 0.0195(3) 0.0206(4) 0.0249(4) -0.0065(3) 0.0049(3) -0.0048(3)
C14 0.0331(5) 0.0290(5) 0.0279(5) -0.0012(4) 0.0123(4) 0.0082(4)
C15 0.0159(3) 0.0138(3) 0.0353(5) -0.0008(3) 0.0021(3) 0.0011(3)
C16 0.0159(3) 0.0134(3) 0.0365(5) -0.0004(3) -0.0012(3) -0.0023(3)
C17 0.0145(3) 0.0152(3) 0.0320(4) 0.0007(3) -0.0002(3) -0.0063(3)
C18 0.0175(3) 0.0180(4) 0.0333(5) 0.0028(3) -0.0007(3) -0.0073(3)
C19 0.0222(4) 0.0194(4) 0.0382(5) 0.0006(3) -0.0061(4) -0.0083(4)
C20 0.0237(4) 0.0179(4) 0.0463(6) -0.0037(3) -0.0064(4) -0.0043(4)
C21 0.0201(4) 0.0159(4) 0.0445(6) -0.0030(3) -0.0027(4) -0.0017(4)
C22 0.0277(5) 0.0418(6) 0.0285(5) -0.0015(4) 0.0054(4) -0.0173(4)
Cl1 0.02003(9) 0.02151(9) 0.02147(9) 0.00524(7) -0.00090(7) -0.00103(7)
Fe1 0.01339(5) 0.01431(5) 0.01887(6) -0.00220(4) 0.00173(4) -0.00074(4)
K1 0.02232(12) 0.02485(13) 0.01974(11) 0.000 0.00370(9) 0.000
N1 0.0141(3) 0.0148(3) 0.0185(3) -0.0004(2) 0.0027(2) 0.0008(2)
N2 0.0143(3) 0.0141(3) 0.0275(4) -0.0006(2) 0.0029(2) 0.0001(2)
N3 0.019(4) 0.015(4) 0.0219(5) 0.000(2) 0.002(2) 0.003(3)
O5 0.0257(8) 0.0244(7) 0.0633(13) -0.0068(7) 0.0041(8) 0.0092(8)
O6 0.0318(8) 0.0357(9) 0.0428(10) 0.0080(6) 0.0203(7) 0.0171(7)
O7 0.0592(13) 0.0449(10) 0.0240(8) 0.0127(10) -0.0048(8) -0.0069(7)
O1 0.0194(3) 0.0242(3) 0.0193(3) -0.0085(2) 0.0027(2) -0.0004(2)
O2 0.0263(3) 0.0291(3) 0.0204(3) -0.0065(3) 0.0060(2) 0.0042(3)
O3 0.0193(3) 0.0214(3) 0.0271(3) -0.0056(2) 0.0049(2) -0.0073(2)
O4 0.0210(3) 0.0279(3) 0.0292(4) -0.0006(3) 0.0012(3) -0.0088(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0162
1 -1 0 0.0692
1 0 -1 0.0745
-1 0 1 0.0523
1 2 1 0.0153
-1 -2 -1 0.0422
0 0 1 0.1070
-2 0 -1 0.0297
1 0 1 0.0769
0 -1 2 0.0864
-1 0 0 0.0205
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 N1 . . 115.48(8) ?
C6 C1 C2 . . 119.99(8) ?
C6 C1 N1 . . 124.51(8) ?
C1 C2 N2 . . 115.00(8) ?
C3 C2 C1 . . 119.73(9) ?
C3 C2 N2 . . 125.27(9) ?
C2 C3 H3 . . 120.3 ?
C4 C3 C2 . . 119.31(9) ?
C4 C3 H3 . . 120.3 ?
C3 C4 H4 . . 119.5 ?
C3 C4 C5 . . 120.96(9) ?
C5 C4 H4 . . 119.5 ?
C4 C5 H5 . . 119.8 ?
C6 C5 C4 . . 120.42(10) ?
C6 C5 H5 . . 119.8 ?
C1 C6 H6 . . 120.2 ?
C5 C6 C1 . . 119.56(9) ?
C5 C6 H6 . . 120.2 ?
C8 C7 H7 . . 117.2 ?
N1 C7 H7 . . 117.2 ?
N1 C7 C8 . . 125.57(8) ?
C9 C8 C7 . . 122.73(7) ?
C9 C8 C13 . . 119.97(8) ?
C13 C8 C7 . . 117.30(8) ?
C8 C9 C10 . . 118.55(8) ?
O1 C9 C8 . . 123.07(8) ?
O1 C9 C10 . . 118.37(8) ?
C11 C10 C9 . . 120.56(8) ?
O2 C10 C9 . . 114.32(8) ?
O2 C10 C11 . . 125.12(8) ?
C10 C11 H11 . . 119.8 ?
C10 C11 C12 . . 120.34(9) ?
C12 C11 H11 . . 119.8 ?
C11 C12 H12 . . 119.9 ?
C13 C12 C11 . . 120.17(9) ?
C13 C12 H12 . . 119.9 ?
C8 C13 H13 . . 119.8 ?
C12 C13 C8 . . 120.37(9) ?
C12 C13 H13 . . 119.8 ?
H14A C14 H14B . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
O2 C14 H14A . . 109.5 ?
O2 C14 H14B . . 109.5 ?
O2 C14 H14C . . 109.5 ?
C16 C15 H15 . . 117.6 ?
N2 C15 H15 . . 117.6 ?
N2 C15 C16 . . 124.78(9) ?
C17 C16 C15 . . 123.36(8) ?
C17 C16 C21 . . 120.07(10) ?
C21 C16 C15 . . 116.56(10) ?
C16 C17 C18 . . 118.46(8) ?
O3 C17 C16 . . 123.27(9) ?
O3 C17 C18 . . 118.27(9) ?
C19 C18 C17 . . 120.37(10) ?
O4 C18 C17 . . 115.23(8) ?
O4 C18 C19 . . 124.40(10) ?
C18 C19 H19 . . 119.8 ?
C18 C19 C20 . . 120.47(10) ?
C20 C19 H19 . . 119.8 ?
C19 C20 H20 . . 119.8 ?
C21 C20 C19 . . 120.44(9) ?
C21 C20 H20 . . 119.8 ?
C16 C21 H21 . . 119.9 ?
C20 C21 C16 . . 120.19(11) ?
C20 C21 H21 . . 119.9 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
O4 C22 H22A . . 109.5 ?
O4 C22 H22B . . 109.5 ?
O4 C22 H22C . . 109.5 ?
Cl1 Fe1 K1 . . 108.107(8) ?
N1 Fe1 Cl1 . . 104.96(2) ?
N1 Fe1 K1 . . 129.53(2) ?
N1 Fe1 N2 . . 77.94(3) ?
N2 Fe1 Cl1 . . 99.03(2) ?
N2 Fe1 K1 . . 131.16(2) ?
O1 Fe1 Cl1 . . 109.17(2) ?
O1 Fe1 K1 . . 45.44(2) ?
O1 Fe1 N1 . . 88.07(3) ?
O1 Fe1 N2 . . 150.97(3) ?
O3 Fe1 Cl1 . . 107.46(2) ?
O3 Fe1 K1 . . 45.48(2) ?
O3 Fe1 N1 . . 146.34(3) ?
O3 Fe1 N2 . . 88.21(3) ?
O3 Fe1 O1 . . 89.74(3) ?
O1 K1 O1 2_655 . 143.60(3) ?
O1 K1 O2 2_655 . 92.10(2) ?
O1 K1 O2 . 2_655 92.11(2) ?
O1 K1 O2 2_655 2_655 56.27(2) ?
O1 K1 O2 . . 56.27(2) ?
O1 K1 O3 2_655 2_655 58.36(2) ?
O1 K1 O3 2_655 . 142.57(2) ?
O1 K1 O3 . 2_655 142.57(2) ?
O1 K1 O3 . . 58.36(2) ?
O1 K1 O4 2_655 . 89.16(2) ?
O1 K1 O4 . 2_655 89.17(2) ?
O1 K1 O4 . . 113.71(2) ?
O1 K1 O4 2_655 2_655 113.71(2) ?
O2 K1 O2 . 2_655 67.77(3) ?
O3 K1 O2 . 2_655 107.94(2) ?
O3 K1 O2 2_655 2_655 114.10(2) ?
O3 K1 O2 2_655 . 107.93(2) ?
O3 K1 O2 . . 114.10(2) ?
O3 K1 O3 2_655 . 128.89(3) ?
O3 K1 O4 . . 56.68(2) ?
O3 K1 O4 2_655 . 90.80(2) ?
O3 K1 O4 2_655 2_655 56.67(2) ?
O3 K1 O4 . 2_655 90.80(2) ?
O4 K1 O2 . . 158.68(2) ?
O4 K1 O2 2_655 . 95.66(2) ?
O4 K1 O2 2_655 2_655 158.68(2) ?
O4 K1 O2 . 2_655 95.66(2) ?
O4 K1 O4 2_655 . 103.29(3) ?
C1 N1 Fe1 . . 113.93(5) ?
C7 N1 C1 . . 120.30(8) ?
C7 N1 Fe1 . . 125.74(6) ?
C2 N2 Fe1 . . 113.90(6) ?
C15 N2 C2 . . 121.40(8) ?
C15 N2 Fe1 . . 124.24(7) ?
O5 N3 O6 . . 118.1(19) ?
O7 N3 O5 . . 121.1(18) ?
O7 N3 O6 . . 120.9(12) ?
C9 O1 Fe1 . . 131.50(6) ?
C9 O1 K1 . . 123.46(5) ?
Fe1 O1 K1 . . 105.03(3) ?
C10 O2 C14 . . 117.47(8) ?
C10 O2 K1 . . 122.41(5) ?
C14 O2 K1 . . 119.23(6) ?
C17 O3 Fe1 . . 128.48(7) ?
C17 O3 K1 . . 125.01(6) ?
Fe1 O3 K1 . . 105.04(3) ?
C18 O4 C22 . . 116.34(9) ?
C18 O4 K1 . . 123.13(6) ?
C22 O4 K1 . . 120.48(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.4038(12) ?
C1 C6 . 1.3979(13) ?
C1 N1 . 1.4208(11) ?
C2 C3 . 1.4032(13) ?
C2 N2 . 1.4159(13) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.3818(17) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.3866(16) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.3840(14) ?
C6 H6 . 0.9500 ?
C7 H7 . 0.9500 ?
C7 C8 . 1.4365(12) ?
C7 N1 . 1.3005(11) ?
C8 C9 . 1.4063(12) ?
C8 C13 . 1.4156(12) ?
C9 C10 . 1.4194(12) ?
C9 O1 . 1.3209(10) ?
C10 C11 . 1.3807(13) ?
C10 O2 . 1.3674(12) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.4048(15) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.3722(14) ?
C13 H13 . 0.9500 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C14 O2 . 1.4284(12) ?
C15 H15 . 0.9500 ?
C15 C16 . 1.4356(15) ?
C15 N2 . 1.3006(12) ?
C16 C17 . 1.4132(15) ?
C16 C21 . 1.4149(13) ?
C17 C18 . 1.4188(14) ?
C17 O3 . 1.3206(11) ?
C18 C19 . 1.3831(14) ?
C18 O4 . 1.3694(14) ?
C19 H19 . 0.9500 ?
C19 C20 . 1.4034(18) ?
C20 H20 . 0.9500 ?
C20 C21 . 1.3694(17) ?
C21 H21 . 0.9500 ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C22 O4 . 1.4404(14) ?
Fe1 Cl1 . 2.2285(3) y
Fe1 K1 . 3.7246(2) ?
Fe1 N1 . 2.0705(8) y
Fe1 N2 . 2.0848(8) y
Fe1 O1 . 1.9010(7) y
Fe1 O3 . 1.8980(7) y
K1 O1 2_655 2.7476(7) ?
K1 O1 . 2.7476(7) y
K1 O2 2_655 2.7900(8) ?
K1 O2 . 2.7900(8) y
K1 O3 . 2.7497(8) y
K1 O3 2_655 2.7497(8) ?
K1 O4 . 2.7890(8) y
K1 O4 2_655 2.7889(8) ?
N3 O5 . 1.258(15) ?
N3 O6 . 1.26(2) ?
N3 O7 . 1.21(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C3 H3 O5 3_445 0.95 2.28 3.221(2) 170.0 yes
C6 H6 Cl1 5_666 0.95 2.81 3.7493(10) 169.7 yes
C7 H7 Cl1 5_666 0.95 2.88 3.6840(9) 143.1 yes
C15 H15 O6 5_656 0.95 2.38 3.2611(19) 154.5 yes
C19 H19 Cl1 4_545 0.95 2.70 3.5639(11) 150.9 yes
C22 H22A O7 2_655 0.98 2.41 2.908(2) 110.7 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 C2 C3 C4 . . . . -0.26(14) ?
C1 C2 N2 C15 . . . . 173.39(8) ?
C1 C2 N2 Fe1 . . . . -14.17(9) ?
C2 C1 C6 C5 . . . . 1.35(13) ?
C2 C1 N1 C7 . . . . -167.93(8) ?
C2 C1 N1 Fe1 . . . . 14.15(9) ?
C2 C3 C4 C5 . . . . 1.61(16) ?
C3 C2 N2 C15 . . . . -6.72(14) ?
C3 C2 N2 Fe1 . . . . 165.73(7) ?
C3 C4 C5 C6 . . . . -1.49(16) ?
C4 C5 C6 C1 . . . . -0.01(15) ?
C6 C1 C2 C3 . . . . -1.22(13) ?
C6 C1 C2 N2 . . . . 178.68(8) ?
C6 C1 N1 C7 . . . . 13.54(13) ?
C6 C1 N1 Fe1 . . . . -164.39(7) ?
C7 C8 C9 C10 . . . . -179.90(8) ?
C7 C8 C9 O1 . . . . -0.81(13) ?
C7 C8 C13 C12 . . . . -178.34(9) ?
C8 C7 N1 C1 . . . . -178.51(8) ?
C8 C7 N1 Fe1 . . . . -0.85(13) ?
C8 C9 C10 C11 . . . . -1.82(13) ?
C8 C9 C10 O2 . . . . 178.20(8) ?
C8 C9 O1 Fe1 . . . . 19.15(13) ?
C8 C9 O1 K1 . . . . -159.48(6) ?
C9 C8 C13 C12 . . . . 1.69(14) ?
C9 C10 C11 C12 . . . . 1.83(14) ?
C9 C10 O2 C14 . . . . 173.29(8) ?
C9 C10 O2 K1 . . . . -17.59(10) ?
C10 C9 O1 Fe1 . . . . -161.76(7) ?
C10 C9 O1 K1 . . . . 19.61(11) ?
C10 C11 C12 C13 . . . . -0.05(15) ?
C11 C10 O2 C14 . . . . -6.70(14) ?
C11 C10 O2 K1 . . . . 162.42(7) ?
C11 C12 C13 C8 . . . . -1.71(15) ?
C13 C8 C9 C10 . . . . 0.07(12) ?
C13 C8 C9 O1 . . . . 179.16(8) ?
C15 C16 C17 C18 . . . . -179.87(8) ?
C15 C16 C17 O3 . . . . 0.69(14) ?
C15 C16 C21 C20 . . . . 179.58(9) ?
C16 C15 N2 C2 . . . . -179.48(8) ?
C16 C15 N2 Fe1 . . . . 8.87(13) ?
C16 C17 C18 C19 . . . . -0.20(13) ?
C16 C17 C18 O4 . . . . 178.84(8) ?
C16 C17 O3 Fe1 . . . . -25.98(13) ?
C16 C17 O3 K1 . . . . 169.98(6) ?
C17 C16 C21 C20 . . . . -1.32(15) ?
C17 C18 C19 C20 . . . . -0.49(15) ?
C17 C18 O4 C22 . . . . -165.44(8) ?
C17 C18 O4 K1 . . . . 11.77(11) ?
C18 C17 O3 Fe1 . . . . 154.58(7) ?
C18 C17 O3 K1 . . . . -9.47(11) ?
C18 C19 C20 C21 . . . . 0.28(16) ?
C19 C18 O4 C22 . . . . 13.56(14) ?
C19 C18 O4 K1 . . . . -169.23(7) ?
C19 C20 C21 C16 . . . . 0.62(16) ?
C21 C16 C17 C18 . . . . 1.10(13) ?
C21 C16 C17 O3 . . . . -178.35(9) ?
Cl1 Fe1 O3 C17 . . . . -68.02(8) ?
Cl1 Fe1 O3 K1 . . . . 98.49(2) ?
K1 Fe1 O3 C17 . . . . -166.52(10) ?
N1 C1 C2 C3 . . . . -179.82(8) ?
N1 C1 C2 N2 . . . . 0.08(11) ?
N1 C1 C6 C5 . . . . 179.82(8) ?
N1 C7 C8 C9 . . . . -7.64(14) ?
N1 C7 C8 C13 . . . . 172.39(9) ?
N1 Fe1 O3 C17 . . . . 95.79(9) ?
N1 Fe1 O3 K1 . . . . -97.69(5) ?
N2 C2 C3 C4 . . . . 179.85(9) ?
N2 C15 C16 C17 . . . . 6.75(15) ?
N2 C15 C16 C21 . . . . -174.19(9) ?
N2 Fe1 O3 C17 . . . . 30.88(8) ?
N2 Fe1 O3 K1 . . . . -162.60(3) ?
O1 C9 C10 C11 . . . . 179.05(8) ?
O1 C9 C10 O2 . . . . -0.94(12) ?
O1 Fe1 O3 C17 . . . . -178.07(8) ?
O1 Fe1 O3 K1 . . . . -11.56(3) ?
O2 C10 C11 C12 . . . . -178.18(9) ?
O3 C17 C18 C19 . . . . 179.27(9) ?
O3 C17 C18 O4 . . . . -1.69(12) ?
O4 C18 C19 C20 . . . . -179.44(9) ?