#------------------------------------------------------------------------------
#$Date: 2023-11-01 05:16:00 +0200 (Wed, 01 Nov 2023) $
#$Revision: 287191 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/29/2022930.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_2022930
loop_
_publ_author_name
'N\"ather, Christian'
'M\"uller-Meinhard, Asmus'
'Jess, Inke'
_publ_section_title
;
Synthesis, crystal structure and properties of
tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of
diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II)
pyridine-3-carbonitrile monosolvate
;
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1093
_journal_page_last 1099
_journal_paper_doi 10.1107/S205698902300909X
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Fe (N C S)2 (C6 H4 N2)2 (H2 O)2], 2C6 H4 N2'
_chemical_formula_moiety 'C14 H12 Fe N6 O2 S2, 2(C6 H4 N2)'
_chemical_formula_sum 'C26 H20 Fe N10 O2 S2'
_chemical_formula_weight 624.49
_chemical_name_systematic
;
Diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile
monosolvate
;
_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_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha 84.7650(10)
_cell_angle_beta 77.7870(10)
_cell_angle_gamma 70.8260(10)
_cell_formula_units_Z 1
_cell_length_a 8.10650(10)
_cell_length_b 8.28800(10)
_cell_length_c 11.4347(2)
_cell_measurement_reflns_used 25131
_cell_measurement_temperature 99.99(10)
_cell_measurement_theta_max 79.6570
_cell_measurement_theta_min 3.9450
_cell_volume 709.021(18)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015a)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015b)
;
_diffrn_ambient_temperature 99.99(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0219
_diffrn_reflns_av_unetI/netI 0.0089
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 29397
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 80.346
_diffrn_reflns_theta_min 3.957
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 6.012
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.72660
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.463
_exptl_crystal_description block
_exptl_crystal_F_000 320
_exptl_crystal_size_max 0.11
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.287
_refine_diff_density_min -0.245
_refine_ls_extinction_coef 0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/6 (Sheldrick 2016)
;
_refine_ls_goodness_of_fit_ref 1.146
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 196
_refine_ls_number_reflns 2999
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.146
_refine_ls_R_factor_all 0.0215
_refine_ls_R_factor_gt 0.0215
_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^)+(0.0302P)^2^+0.2457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0600
_refine_ls_wR_factor_ref 0.0600
_reflns_number_gt 2999
_reflns_number_total 2999
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8079sup1.cif
_cod_data_source_block 2
_cod_database_code 2022930
_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_hkl_file
;
0 0 -1 315.50 5.40
0 0 -1 323.41 5.46
0 0 -1 315.33 5.39
0 0 -1 326.24 5.46
0 0 -1 327.57 5.47
0 0 1 314.17 5.54
0 0 1 325.49 5.49
0 0 1 319.02 5.54
0 0 2 222.98 4.23
0 0 2 220.56 4.12
0 0 2 216.92 4.01
0 0 2 216.52 4.12
0 0 -2 220.94 3.96
0 0 -2 220.15 3.88
0 0 -2 221.51 3.85
0 0 -2 219.99 4.00
0 0 -2 212.17 3.89
0 0 -2 213.00 3.86
0 0 -2 226.54 3.89
0 0 -2 217.40 3.85
0 0 -2 221.70 3.80
0 0 -2 216.66 3.98
0 0 -2 221.91 3.88
0 0 -2 222.29 3.96
0 0 -2 225.79 4.00
0 0 -2 219.83 3.96
0 0 -2 224.91 3.90
0 0 -2 219.25 4.00
0 0 3 3864.34 61.99
0 0 3 3713.30 62.18
0 0 3 3492.97 62.34
0 0 -3 3645.76 61.71
0 0 -3 3778.10 61.73
0 0 -3 3829.65 61.96
0 0 -3 3669.16 61.85
0 0 -3 3816.23 61.79
0 0 -3 3536.19 61.69
0 0 -3 3723.40 61.72
0 0 -3 3782.23 61.79
0 0 -3 3762.18 61.62
0 0 -3 3798.72 61.95
0 0 -3 3693.82 61.71
0 0 -3 3727.54 61.86
0 0 -3 3743.94 61.97
0 0 -3 3685.94 61.73
0 0 -3 3720.66 61.87
0 0 -3 3798.90 61.96
0 0 -4 96.42 2.06
0 0 -4 95.02 2.15
0 0 -4 91.63 1.81
0 0 -4 98.89 2.19
0 0 -4 99.22 2.17
0 0 -4 92.07 1.81
0 0 -4 101.29 2.00
0 0 -4 97.57 2.05
0 0 -4 101.09 1.94
0 0 -4 98.64 2.09
0 0 -4 90.40 1.79
0 0 -4 99.14 2.06
0 0 -4 91.68 1.81
0 0 -4 88.40 1.72
0 0 -4 98.94 1.93
0 0 -4 95.26 2.15
0 0 -4 96.14 2.02
0 0 -4 98.79 2.19
0 0 4 99.02 2.62
0 0 4 107.05 2.86
0 0 -4 100.11 2.19
0 0 -5 200.06 3.98
0 0 -5 199.44 3.97
0 0 -5 191.65 3.93
0 0 -5 187.69 3.92
0 0 -5 201.54 4.01
0 0 -5 202.38 4.29
0 0 -6 357.58 7.46
0 0 -6 381.71 7.65
0 0 -6 369.09 7.31
0 0 6 380.77 8.47
0 0 -7 306.30 6.92
0 0 7 316.70 7.79
0 0 8 226.18 6.72
0 0 -8 223.99 6.02
0 0 9 64.34 2.06
0 0 9 61.37 2.02
0 0 9 65.70 2.02
0 0 9 65.11 1.99
0 0 9 67.84 2.01
0 0 9 64.81 2.01
0 0 9 66.74 2.04
0 0 9 67.29 2.05
0 0 9 63.63 2.02
0 0 9 65.12 2.00
0 0 9 60.42 1.93
0 0 9 63.74 1.95
0 0 9 61.89 2.03
0 0 10 107.82 2.85
0 0 10 108.98 2.72
0 0 10 110.54 2.95
0 0 10 114.34 2.87
0 0 10 109.06 2.87
0 0 10 107.76 2.73
0 0 10 102.90 2.87
0 0 10 108.68 2.87
0 0 10 110.23 2.81
0 0 10 108.94 2.95
0 0 10 112.02 2.91
0 0 10 109.28 2.65
0 0 11 24.50 1.16
0 0 11 24.42 1.15
0 0 11 25.21 1.26
0 0 11 24.81 1.34
0 0 11 24.59 1.28
0 0 11 24.57 1.33
0 0 11 22.97 1.29
0 0 11 22.25 1.20
0 0 11 23.94 1.36
0 0 12 161.30 3.68
0 0 12 163.85 3.61
0 0 12 161.90 3.49
0 0 12 161.55 3.57
0 0 13 197.18 3.88
0 -1 13 301.89 5.66
0 -1 13 324.90 5.80
0 -1 12 186.67 3.85
0 -1 12 192.67 3.96
0 -1 12 181.14 3.88
0 -1 12 186.30 3.99
0 -1 11 29.17 1.17
0 -1 11 30.54 1.35
0 -1 11 30.63 1.23
0 -1 11 31.62 1.39
0 -1 11 32.04 1.35
0 -1 11 31.63 1.30
0 -1 11 29.06 1.42
0 -1 11 29.39 1.36
0 -1 10 27.84 1.20
0 -1 10 25.54 1.37
0 -1 10 23.41 1.28
0 -1 10 27.82 1.29
0 -1 10 25.70 1.42
0 -1 10 25.40 1.30
0 -1 10 26.80 1.22
0 -1 10 25.19 1.22
0 -1 10 25.15 1.32
0 -1 10 27.05 1.33
0 -1 9 37.72 1.55
0 -1 9 35.94 1.45
0 -1 9 37.65 1.39
0 -1 9 34.95 1.52
0 -1 9 39.36 1.46
0 -1 9 39.35 1.44
0 1 -9 36.43 2.47
0 -1 9 35.91 1.51
0 -1 9 40.17 1.41
0 -1 9 36.87 1.51
0 -1 9 35.63 1.54
0 -1 9 38.08 1.50
0 -1 9 35.26 1.45
0 1 -8 502.70 11.09
0 -1 8 481.48 11.41
0 1 -7 122.44 3.92
0 1 -7 118.03 3.67
0 -1 7 119.94 4.10
0 -1 6 2.80 0.68
0 -1 6 2.34 0.75
0 1 -6 2.16 0.79
0 1 -6 2.18 0.57
0 1 -6 3.22 0.73
0 1 -6 2.81 0.56
0 1 -6 1.92 0.59
0 1 -5 15.72 0.81
0 1 -5 13.42 0.89
0 1 -5 15.05 1.03
0 1 -5 13.48 0.89
0 1 -5 14.81 0.80
0 1 -5 14.81 0.81
0 1 -5 13.82 0.97
0 1 -5 14.46 0.79
0 1 -5 16.01 1.04
0 1 -5 13.59 0.90
0 1 -5 14.61 1.09
0 -1 5 12.43 0.88
0 -1 5 13.36 1.06
0 -1 5 13.27 1.04
0 1 -5 13.39 0.78
0 1 -5 15.14 0.88
0 1 -5 15.93 1.02
0 1 -5 15.49 0.72
0 1 -5 14.06 1.01
0 1 -5 14.05 0.90
0 1 -5 13.96 1.03
0 1 -4 1053.31 17.44
0 1 -4 1022.98 17.10
0 1 -4 1022.29 17.73
0 1 -4 1013.98 17.48
0 1 -4 1040.55 17.94
0 -1 4 980.26 16.92
0 1 -4 1059.08 17.55
0 1 -4 1063.61 17.26
0 1 -4 1049.73 17.43
0 1 -4 1046.16 17.91
0 -1 4 991.64 16.93
0 1 -4 995.73 17.49
0 1 -4 1039.06 17.77
0 1 -4 1050.40 17.96
0 1 -4 1017.76 17.72
0 -1 4 985.69 16.93
0 1 -4 996.40 17.47
0 1 -4 996.00 17.28
0 1 -4 990.31 17.55
0 1 -4 1009.78 17.78
0 -1 4 1016.08 18.05
0 -1 4 944.78 16.75
0 -1 4 1031.75 17.70
0 -1 4 928.72 16.81
0 -1 4 1011.69 17.93
0 -1 4 1047.50 17.92
0 1 -3 4808.96 79.74
0 -1 3 4748.31 79.22
0 -1 3 4849.61 79.48
0 1 -3 4593.98 79.85
0 -1 3 4852.95 79.33
0 -1 3 4802.92 79.48
0 -1 3 4687.35 79.22
0 1 -3 4796.88 79.73
0 1 -3 4749.63 79.60
0 -1 3 4860.88 79.32
0 1 -3 4720.20 80.01
0 1 -3 4656.05 79.86
0 1 -3 4823.47 79.38
0 -1 3 4663.99 79.31
0 1 -3 4747.60 79.99
0 1 -3 4735.16 79.60
0 1 -3 4784.80 79.49
0 1 -3 4843.18 79.68
0 -1 3 4837.83 79.33
0 1 -3 4830.20 79.76
0 1 -3 4801.38 80.03
0 1 -3 4677.08 79.90
0 1 -3 4819.90 79.67
0 1 -3 4888.79 79.83
0 1 -3 4695.79 79.54
0 -1 3 4883.33 80.00
0 -1 3 4759.72 79.81
0 -1 3 4832.98 79.78
0 -1 3 4857.04 80.08
0 -1 2 302.07 5.64
0 1 -2 309.02 5.86
0 -1 2 296.22 5.48
0 1 -2 314.23 5.79
0 -1 2 298.33 5.57
0 1 -2 303.11 5.67
0 1 -2 307.42 5.92
0 1 -2 304.47 5.59
0 1 -2 303.83 5.63
0 -1 2 300.84 5.57
0 -1 2 297.68 5.62
0 1 -2 306.03 5.94
0 1 -2 312.35 5.65
0 -1 2 302.20 5.49
0 1 -2 304.79 5.85
0 1 -2 304.73 5.50
0 1 -2 314.66 5.79
0 -1 2 303.55 5.87
0 1 -2 282.72 5.64
0 1 -2 301.78 5.63
0 1 -2 284.73 5.71
0 1 -2 312.89 5.95
0 -1 2 300.89 5.49
0 1 -2 311.50 5.80
0 1 -2 318.60 5.91
0 -1 2 302.94 5.56
0 -1 2 311.59 5.85
0 1 -1 449.41 7.80
0 1 -1 438.39 7.75
0 -1 1 399.47 7.53
0 -1 1 421.56 7.53
0 -1 1 398.24 7.53
0 1 -1 442.11 7.75
0 1 -1 431.77 7.82
0 1 -1 454.39 7.80
0 1 -1 427.40 7.52
0 -1 1 429.59 7.54
0 1 -1 421.55 7.58
0 1 -1 440.11 7.76
0 1 -1 431.69 7.82
0 1 -1 448.50 7.82
0 -1 1 425.52 7.54
0 -1 1 439.00 7.43
0 1 -1 432.98 7.58
0 1 -1 427.95 7.80
0 1 -1 433.77 7.57
0 1 -1 444.82 7.65
0 -1 1 409.86 7.25
0 1 0 929.32 15.55
0 -1 0 920.48 15.71
0 -1 0 922.63 15.69
0 -1 0 917.88 15.71
0 -1 0 950.55 15.76
0 -1 0 909.55 15.72
0 1 0 889.01 15.63
0 -1 0 915.88 15.72
0 -1 0 933.14 15.70
0 -1 0 916.45 15.72
0 -1 0 953.31 15.68
0 1 1 9.64 0.40
0 1 1 9.48 0.43
0 1 1 9.26 0.42
0 1 1 8.67 0.36
0 1 1 10.76 0.42
0 -1 -1 9.49 0.39
0 -1 -1 9.01 0.41
0 -1 -1 9.27 0.43
0 1 1 10.19 0.48
0 1 1 10.63 0.42
0 -1 -1 9.51 0.45
0 1 1 10.15 0.44
0 -1 -1 9.50 0.40
0 -1 -1 9.43 0.46
0 1 1 9.60 0.49
0 -1 -1 9.80 0.46
0 -1 -1 9.42 0.42
0 1 1 10.28 0.48
0 -1 -1 9.44 0.44
0 -1 -1 9.48 0.48
0 -1 -1 10.23 0.40
0 1 1 9.35 0.43
0 -1 -1 9.51 0.45
0 1 1 10.81 0.43
0 1 1 9.63 0.47
0 1 1 8.40 0.47
0 1 2 161.02 2.87
0 1 2 152.74 2.95
0 -1 -2 165.44 3.01
0 -1 -2 175.61 3.11
0 1 2 157.84 2.86
0 -1 -2 168.16 3.15
0 -1 -2 158.32 3.18
0 1 2 163.38 3.47
0 -1 -2 157.52 3.03
0 -1 -2 168.12 3.15
0 -1 -2 174.01 3.11
0 -1 -2 165.76 3.01
0 1 2 160.62 3.46
0 -1 -2 160.06 3.04
0 1 2 162.10 3.27
0 -1 -2 167.98 3.15
0 1 2 157.17 2.86
0 -1 -3 152.28 2.77
0 -1 -3 161.40 3.03
0 -1 -3 160.51 2.91
0 -1 -3 157.31 2.97
0 -1 -3 146.08 2.97
0 1 3 166.42 3.66
0 -1 -3 140.52 2.72
0 -1 -3 160.64 3.15
0 -1 -3 158.51 3.02
0 -1 -3 161.14 2.91
0 -1 -3 150.39 2.77
0 -1 -3 154.26 2.97
0 1 3 153.42 3.55
0 1 3 151.37 3.61
0 -1 -3 158.31 2.98
0 1 3 159.21 3.25
0 -1 -4 236.27 4.02
0 -1 -4 198.37 3.79
0 -1 -4 226.28 3.91
0 -1 -4 229.17 4.01
0 -1 -4 230.68 3.95
0 -1 -4 232.71 4.02
0 -1 -4 194.74 3.82
0 1 4 261.15 5.29
0 -1 -4 240.76 4.39
0 -1 -4 238.22 4.23
0 -1 -4 234.17 4.06
0 1 4 263.59 5.33
0 -1 -4 223.77 3.94
0 -1 -4 220.24 3.89
0 1 4 249.18 5.11
0 -1 -4 233.50 4.03
0 -1 -4 196.45 3.82
0 -1 -4 237.34 4.02
0 -1 -4 228.53 4.01
0 -1 -4 198.03 3.79
0 -1 -4 229.18 3.95
0 -1 -4 219.18 4.11
0 -1 -4 223.33 4.06
0 -1 -4 233.91 3.96
0 -1 -4 238.59 4.04
0 -1 -4 194.94 3.83
0 1 5 248.30 5.73
0 -1 -5 236.84 4.84
0 1 5 246.84 5.93
0 1 6 107.51 3.50
0 1 7 374.45 8.40
0 1 7 362.75 6.57
0 1 7 353.30 6.63
0 1 8 699.54 15.32
0 1 9 590.54 10.70
0 1 9 574.77 10.64
0 1 9 560.39 10.76
0 1 9 578.18 10.77
0 1 9 583.96 10.75
0 1 9 562.28 10.72
0 1 9 572.22 10.66
0 1 9 585.24 10.66
0 1 9 601.48 10.84
0 1 9 597.31 10.69
0 1 9 617.50 10.85
0 1 9 590.97 10.88
0 1 9 615.37 10.86
0 1 9 598.21 10.91
0 1 9 563.74 10.84
0 1 9 609.01 10.69
0 1 9 554.62 10.69
0 1 10 9.27 0.98
0 1 10 15.44 1.07
0 1 10 10.34 0.94
0 1 10 10.16 0.98
0 1 10 11.85 0.90
0 1 10 10.89 0.99
0 1 10 12.07 1.04
0 1 10 15.20 1.13
0 1 10 11.01 0.93
0 1 10 11.23 0.90
0 1 10 11.64 1.06
0 1 10 11.10 1.01
0 1 10 14.69 0.99
0 1 10 12.80 1.08
0 1 10 12.18 1.06
0 1 10 10.90 1.03
0 1 10 12.89 1.11
0 1 10 18.14 1.04
0 1 10 11.66 0.94
0 1 11 33.65 1.54
0 1 11 35.12 1.55
0 1 11 34.09 1.40
0 1 11 34.96 1.33
0 1 11 33.25 1.32
0 1 11 33.95 1.50
0 1 11 35.24 1.55
0 1 11 32.96 1.31
0 1 11 33.18 1.47
0 1 11 34.23 1.46
0 1 12 13.79 0.93
0 1 12 14.45 0.88
0 -2 13 78.14 1.75
0 -2 12 48.41 1.52
0 -2 12 49.28 1.53
0 -2 12 50.45 1.48
0 -2 12 50.09 1.65
0 -2 11 45.65 1.65
0 -2 11 43.99 1.71
0 -2 11 43.32 1.43
0 -2 11 47.90 1.69
0 -2 11 46.18 1.47
0 -2 11 46.81 1.76
0 -2 11 47.10 1.58
0 -2 11 46.71 1.48
0 -2 10 55.85 1.98
0 -2 10 56.45 1.89
0 -2 10 51.89 1.89
0 -2 10 52.92 1.88
0 -2 10 51.76 1.88
0 -2 10 55.60 1.76
0 -2 10 53.78 1.94
0 -2 10 54.27 1.71
0 -2 10 56.77 1.73
0 -2 10 54.76 1.78
0 -2 9 229.97 4.68
0 -2 9 223.45 4.91
0 -2 9 224.27 4.69
0 -2 9 224.35 4.70
0 -2 9 224.29 4.87
0 -2 9 229.85 4.87
0 -2 9 226.23 4.86
0 -2 9 229.04 4.86
0 -2 9 229.24 4.93
0 -2 9 228.50 4.70
0 2 -9 221.03 6.92
0 2 -9 227.43 6.77
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-10 -4 -5 3.92 0.39
10 4 5 3.80 0.34
-10 -4 -6 5.42 0.34
-10 -5 -2 35.80 0.90
10 5 2 42.37 0.95
-10 -5 -3 70.57 1.50
10 5 3 66.46 1.39
-10 -5 -5 76.10 1.59
0 0 0 0.00 0.00
TITL AMM22_auto in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 8.106505 8.288011 11.434654 84.7645 77.7869 70.8263
ZERR 1.00 0.000081 0.000127 0.000198 0.0013 0.0012 0.0012
LATT 1
SFAC C H N O S Fe
UNIT 26.00 20.00 10.00 2.00 2.00 1.00
REM CrysAlisPro recorded range (K): Min=99.9; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 918
_shelx_res_file
;
TITL amm22_a.res in P-1
amm22.res
created by SHELXL-2016/6 at 15:08:05 on 19-Sep-2023
REM Old TITL AMM22_auto in P-1
REM SHELXT solution in P-1
REM R1 0.075, Rweak 0.012, Alpha 0.055, Orientation as input
REM Formula found by SHELXT: C26 N10 O2 S2 Fe
CELL 1.54184 8.1065 8.288 11.4347 84.765 77.787 70.826
ZERR 1 0.0001 0.0001 0.0002 0.001 0.001 0.001
LATT 1
SFAC C H Fe N O S
UNIT 26 20 1 10 2 2
EQIV $1 1-X,1-Y,1-Z
EQIV $2 -X,1-Y,1-Z
EQIV $3 1-X,-Y,1-Z
EQIV $4 1+X,+Y,+Z
L.S. 10
PLAN 5
TEMP -173
CONF
HTAB C11 N1
HTAB C11 S1_$2
HTAB C14 S1_$3
HTAB C15 N1_$1
HTAB C21 S1
HTAB C24 N22_$4
HTAB C25 S1_$4
HTAB O1 N21
HTAB O1 S1_$4
LIST 6
MORE -1
BOND $H
HTAB
fmap 2 53
acta
REM
REM
REM
WGHT 0.030200 0.245700
EXTI 0.003630
FVAR 0.77156
FE1 3 0.500000 0.500000 0.500000 10.50000 0.01011 0.01477 =
0.01245 -0.00395 -0.00059 -0.00513
N1 4 0.237485 0.505169 0.580581 11.00000 0.01336 0.02155 =
0.01884 -0.00654 0.00043 -0.00786
C1 1 0.109304 0.486175 0.640149 11.00000 0.01458 0.01462 =
0.01548 -0.00433 -0.00536 -0.00343
S1 6 -0.066511 0.458904 0.729848 11.00000 0.01226 0.02427 =
0.01741 -0.00184 -0.00037 -0.00805
O1 5 0.587436 0.386597 0.659832 11.00000 0.01457 0.01934 =
0.01656 -0.00450 -0.00246 -0.00459
N11 4 0.550024 0.245666 0.423465 11.00000 0.01318 0.01479 =
0.01313 -0.00201 -0.00128 -0.00484
C11 1 0.412304 0.208382 0.399132 11.00000 0.01343 0.01624 =
0.01372 -0.00185 -0.00226 -0.00480
AFIX 43
H11 2 0.295430 0.284514 0.423936 11.00000 -1.20000
AFIX 0
C12 1 0.434356 0.061623 0.338612 11.00000 0.01593 0.01726 =
0.01414 -0.00182 -0.00247 -0.00768
C13 1 0.604727 -0.052875 0.302939 11.00000 0.01875 0.01603 =
0.01896 -0.00463 -0.00042 -0.00640
AFIX 43
H13 2 0.622799 -0.154127 0.262362 11.00000 -1.20000
AFIX 0
C14 1 0.746563 -0.014018 0.328647 11.00000 0.01407 0.01609 =
0.02229 -0.00384 0.00004 -0.00291
AFIX 43
H14 2 0.864668 -0.088837 0.306060 11.00000 -1.20000
AFIX 0
C15 1 0.714302 0.135528 0.387811 11.00000 0.01323 0.01922 =
0.01722 -0.00135 -0.00189 -0.00661
AFIX 43
H15 2 0.812998 0.161414 0.403931 11.00000 -1.20000
AFIX 0
C16 1 0.278957 0.033580 0.313609 11.00000 0.01881 0.01823 =
0.02174 -0.00745 -0.00191 -0.00583
N12 4 0.154703 0.013572 0.293691 11.00000 0.02092 0.03021 =
0.03975 -0.01514 -0.00586 -0.00885
N21 4 0.403610 0.596532 0.850714 11.00000 0.01802 0.02074 =
0.01394 -0.00189 -0.00237 -0.00569
C21 1 0.228522 0.621445 0.881376 11.00000 0.01911 0.02071 =
0.01531 -0.00187 -0.00415 -0.00844
AFIX 43
H21 2 0.176535 0.564393 0.838477 11.00000 -1.20000
AFIX 0
C22 1 0.119759 0.727838 0.973781 11.00000 0.01522 0.01889 =
0.01524 0.00045 -0.00344 -0.00726
C23 1 0.194229 0.812316 1.037756 11.00000 0.01813 0.01928 =
0.01619 -0.00395 -0.00148 -0.00676
AFIX 43
H23 2 0.122870 0.885180 1.101462 11.00000 -1.20000
AFIX 0
C24 1 0.375324 0.786628 1.005488 11.00000 0.01831 0.02253 =
0.01944 -0.00292 -0.00454 -0.00970
AFIX 43
H24 2 0.430907 0.842236 1.046636 11.00000 -1.20000
AFIX 0
C25 1 0.474333 0.678729 0.912380 11.00000 0.01471 0.02129 =
0.01723 0.00061 -0.00261 -0.00662
AFIX 43
H25 2 0.598501 0.661992 0.891042 11.00000 -1.20000
AFIX 0
C26 1 -0.067974 0.748851 1.002537 11.00000 0.01980 0.02155 =
0.01802 -0.00312 -0.00367 -0.00844
N22 4 -0.217622 0.767966 1.025566 11.00000 0.01881 0.03144 =
0.02904 -0.00546 -0.00407 -0.01025
H1A 2 0.531378 0.449607 0.723681 11.00000 0.04535
H1B 2 0.692820 0.369152 0.655373 11.00000 0.04209
HKLF 4
REM amm22_a.res in P-1
REM R1 = 0.0215 for 2999 Fo > 4sig(Fo) and 0.0215 for all 2999 data
REM 196 parameters refined using 0 restraints
END
WGHT 0.0302 0.2448
REM Instructions for potential hydrogen bonds
HTAB C11 N1
HTAB C11 S1_$2
HTAB C14 S1_$3
HTAB C15 N1_$1
HTAB C21 S1
HTAB C24 N22_$4
HTAB C25 S1_$4
HTAB O1 N21
HTAB O1 S1_$4
REM Highest difference peak 0.287, deepest hole -0.245, 1-sigma level 0.042
Q1 1 0.7194 0.0620 0.3602 11.00000 0.05 0.29
Q2 1 0.5151 0.0115 0.3122 11.00000 0.05 0.27
Q3 1 0.4293 0.1425 0.3636 11.00000 0.05 0.27
Q4 1 0.1586 0.7547 1.0100 11.00000 0.05 0.25
Q5 1 0.6293 0.1824 0.4020 11.00000 0.05 0.25
;
_shelx_res_checksum 22852
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Fe Fe1 0.500000 0.500000 0.500000 0.01216(8) Uani d 1 . .
N N1 0.23749(14) 0.50517(14) 0.58058(10) 0.0175(2) Uani d 1 . .
C C1 0.10930(16) 0.48617(15) 0.64015(11) 0.0145(2) Uani d 1 . .
S S1 -0.06651(4) 0.45890(4) 0.72985(3) 0.01772(9) Uani d 1 . .
O O1 0.58744(12) 0.38660(11) 0.65983(8) 0.01684(18) Uani d 1 . .
N N11 0.55002(13) 0.24567(12) 0.42347(9) 0.0137(2) Uani d 1 . .
C C11 0.41230(15) 0.20838(15) 0.39913(10) 0.0144(2) Uani d 1 . .
H H11 0.295430 0.284514 0.423936 0.017 Uiso calc 1 . .
C C12 0.43436(16) 0.06162(15) 0.33861(11) 0.0151(2) Uani d 1 . .
C C13 0.60473(17) -0.05288(15) 0.30294(11) 0.0179(2) Uani d 1 . .
H H13 0.622799 -0.154127 0.262362 0.022 Uiso calc 1 . .
C C14 0.74656(16) -0.01402(16) 0.32865(12) 0.0183(2) Uani d 1 . .
H H14 0.864668 -0.088837 0.306060 0.022 Uiso calc 1 . .
C C15 0.71430(16) 0.13553(15) 0.38781(11) 0.0163(2) Uani d 1 . .
H H15 0.812998 0.161414 0.403931 0.020 Uiso calc 1 . .
C C16 0.27896(17) 0.03358(16) 0.31361(12) 0.0195(3) Uani d 1 . .
N N12 0.15470(16) 0.01357(16) 0.29369(12) 0.0292(3) Uani d 1 . .
N N21 0.40361(14) 0.59653(13) 0.85071(9) 0.0177(2) Uani d 1 . .
C C21 0.22852(17) 0.62145(16) 0.88138(11) 0.0176(2) Uani d 1 . .
H H21 0.176535 0.564393 0.838477 0.021 Uiso calc 1 . .
C C22 0.11976(16) 0.72784(15) 0.97378(11) 0.0160(2) Uani d 1 . .
C C23 0.19423(17) 0.81232(16) 1.03776(11) 0.0177(2) Uani d 1 . .
H H23 0.122870 0.885180 1.101462 0.021 Uiso calc 1 . .
C C24 0.37532(17) 0.78663(16) 1.00549(12) 0.0190(3) Uani d 1 . .
H H24 0.430907 0.842236 1.046636 0.023 Uiso calc 1 . .
C C25 0.47433(16) 0.67873(16) 0.91238(11) 0.0177(2) Uani d 1 . .
H H25 0.598501 0.661992 0.891042 0.021 Uiso calc 1 . .
C C26 -0.06797(17) 0.74885(16) 1.00254(11) 0.0191(3) Uani d 1 . .
N N22 -0.21762(15) 0.76797(16) 1.02557(11) 0.0256(3) Uani d 1 . .
H H1A 0.531(3) 0.450(3) 0.724(2) 0.045(6) Uiso d 1 . .
H H1B 0.693(3) 0.369(3) 0.6554(18) 0.042(6) Uiso 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
Fe1 0.01011(13) 0.01477(14) 0.01245(14) -0.00513(10) -0.00059(9) -0.00395(9)
N1 0.0134(5) 0.0216(5) 0.0188(5) -0.0079(4) 0.0004(4) -0.0065(4)
C1 0.0146(5) 0.0146(5) 0.0155(6) -0.0034(4) -0.0054(4) -0.0043(4)
S1 0.01226(14) 0.02427(16) 0.01741(16) -0.00805(11) -0.00037(10) -0.00184(11)
O1 0.0146(4) 0.0193(4) 0.0166(4) -0.0046(3) -0.0025(3) -0.0045(3)
N11 0.0132(5) 0.0148(5) 0.0131(5) -0.0048(4) -0.0013(4) -0.0020(4)
C11 0.0134(5) 0.0162(5) 0.0137(6) -0.0048(4) -0.0023(4) -0.0018(4)
C12 0.0159(6) 0.0173(5) 0.0141(6) -0.0077(5) -0.0025(4) -0.0018(4)
C13 0.0188(6) 0.0160(6) 0.0190(6) -0.0064(5) -0.0004(5) -0.0046(5)
C14 0.0141(5) 0.0161(6) 0.0223(6) -0.0029(4) 0.0000(5) -0.0038(5)
C15 0.0132(5) 0.0192(6) 0.0172(6) -0.0066(5) -0.0019(4) -0.0013(5)
C16 0.0188(6) 0.0182(6) 0.0217(6) -0.0058(5) -0.0019(5) -0.0074(5)
N12 0.0209(6) 0.0302(6) 0.0397(7) -0.0088(5) -0.0059(5) -0.0151(5)
N21 0.0180(5) 0.0207(5) 0.0139(5) -0.0057(4) -0.0024(4) -0.0019(4)
C21 0.0191(6) 0.0207(6) 0.0153(6) -0.0084(5) -0.0041(5) -0.0019(5)
C22 0.0152(6) 0.0189(6) 0.0152(6) -0.0073(5) -0.0034(4) 0.0005(4)
C23 0.0181(6) 0.0193(6) 0.0162(6) -0.0068(5) -0.0015(5) -0.0040(5)
C24 0.0183(6) 0.0225(6) 0.0194(6) -0.0097(5) -0.0045(5) -0.0029(5)
C25 0.0147(5) 0.0213(6) 0.0172(6) -0.0066(5) -0.0026(4) 0.0006(5)
C26 0.0198(6) 0.0216(6) 0.0180(6) -0.0084(5) -0.0037(5) -0.0031(5)
N22 0.0188(6) 0.0314(6) 0.0290(6) -0.0103(5) -0.0041(5) -0.0055(5)
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'
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'
S S 0.3331 0.5567 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 N1 2_666 . 180.0 n
N1 Fe1 O1 . . 89.42(4) y
N1 Fe1 O1 2_666 . 90.58(4) y
N1 Fe1 O1 . 2_666 90.58(4) ?
N1 Fe1 O1 2_666 2_666 89.42(4) ?
N1 Fe1 N11 . . 89.86(4) y
N1 Fe1 N11 2_666 . 90.14(4) y
N1 Fe1 N11 2_666 2_666 89.86(4) ?
N1 Fe1 N11 . 2_666 90.14(4) ?
O1 Fe1 O1 2_666 . 180.0 n
O1 Fe1 N11 2_666 . 87.62(3) y
O1 Fe1 N11 2_666 2_666 92.38(3) ?
O1 Fe1 N11 . . 92.38(3) y
O1 Fe1 N11 . 2_666 87.62(3) ?
N11 Fe1 N11 . 2_666 180.0 n
Fe1 N1 C1 . . 167.09(10) y
N1 C1 S1 . . 177.12(11) ?
Fe1 O1 H1A . . 113.2(14) ?
Fe1 O1 H1B . . 112.3(14) ?
H1A O1 H1B . . 106.9(19) ?
C11 N11 Fe1 . . 118.64(8) ?
C11 N11 C15 . . 117.74(10) ?
C15 N11 Fe1 . . 123.18(8) ?
N11 C11 H11 . . 118.8 ?
N11 C11 C12 . . 122.34(11) ?
C12 C11 H11 . . 118.8 ?
C11 C12 C16 . . 118.64(11) ?
C13 C12 C11 . . 119.66(11) ?
C13 C12 C16 . . 121.70(11) ?
C12 C13 H13 . . 121.1 ?
C14 C13 C12 . . 117.77(11) ?
C14 C13 H13 . . 121.1 ?
C13 C14 H14 . . 120.4 ?
C13 C14 C15 . . 119.26(11) ?
C15 C14 H14 . . 120.4 ?
N11 C15 C14 . . 123.23(11) ?
N11 C15 H15 . . 118.4 ?
C14 C15 H15 . . 118.4 ?
N12 C16 C12 . . 179.12(14) ?
C21 N21 C25 . . 117.81(11) ?
N21 C21 H21 . . 118.8 ?
N21 C21 C22 . . 122.43(11) ?
C22 C21 H21 . . 118.8 ?
C21 C22 C23 . . 119.45(11) ?
C21 C22 C26 . . 119.67(11) ?
C23 C22 C26 . . 120.87(11) ?
C22 C23 H23 . . 121.0 ?
C24 C23 C22 . . 117.93(12) ?
C24 C23 H23 . . 121.0 ?
C23 C24 H24 . . 120.5 ?
C23 C24 C25 . . 119.07(11) ?
C25 C24 H24 . . 120.5 ?
N21 C25 C24 . . 123.30(11) ?
N21 C25 H25 . . 118.3 ?
C24 C25 H25 . . 118.3 ?
N22 C26 C22 . . 179.03(14) ?
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
Fe1 N1 2_666 2.1207(10) ?
Fe1 N1 . 2.1207(10) y
Fe1 O1 2_666 2.1267(9) ?
Fe1 O1 . 2.1267(9) y
Fe1 N11 . 2.2358(10) y
Fe1 N11 2_666 2.2358(10) ?
N1 C1 . 1.1649(17) ?
C1 S1 . 1.6387(12) ?
O1 H1A . 0.89(2) ?
O1 H1B . 0.81(2) ?
N11 C11 . 1.3390(15) ?
N11 C15 . 1.3463(15) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3960(16) ?
C12 C13 . 1.3949(17) ?
C12 C16 . 1.4421(17) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.3841(17) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.3883(17) ?
C15 H15 . 0.9500 ?
C16 N12 . 1.1435(18) ?
N21 C21 . 1.3380(16) ?
N21 C25 . 1.3436(16) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.3916(18) ?
C22 C23 . 1.3956(17) ?
C22 C26 . 1.4419(17) ?
C23 H23 . 0.9500 ?
C23 C24 . 1.3844(17) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.3850(18) ?
C25 H25 . 0.9500 ?
C26 N22 . 1.1456(17) ?
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
O1 H1A N21 . 0.89(2) 1.88(2) 2.7615(14) 175(2)
O1 H1B S1 1_655 0.81(2) 2.62(2) 3.3184(9) 145.7(18)
C11 H11 N1 . 0.95 2.54 3.1243(16) 120
C11 H11 S1 2_566 0.95 3.03 3.6833(12) 128
C14 H14 S1 2_656 0.95 2.98 3.7688(13) 141
C15 H15 N1 2_666 0.95 2.67 3.1894(16) 115
C21 H21 S1 . 0.95 2.92 3.8513(13) 165
C24 H24 N22 1_655 0.95 2.67 3.3082(17) 125
C25 H25 S1 1_655 0.95 3.01 3.8056(13) 142
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
Fe1 N11 C11 C12 . . . . 172.36(9) ?
Fe1 N11 C15 C14 . . . . -172.87(9) ?
N11 C11 C12 C13 . . . . 0.88(18) ?
N11 C11 C12 C16 . . . . -178.52(11) ?
C11 N11 C15 C14 . . . . -0.63(18) ?
C11 C12 C13 C14 . . . . -0.64(18) ?
C12 C13 C14 C15 . . . . -0.17(18) ?
C13 C14 C15 N11 . . . . 0.84(19) ?
C15 N11 C11 C12 . . . . -0.24(17) ?
C16 C12 C13 C14 . . . . 178.74(12) ?
N21 C21 C22 C23 . . . . -0.10(19) ?
N21 C21 C22 C26 . . . . -179.84(11) ?
C21 N21 C25 C24 . . . . 0.17(18) ?
C21 C22 C23 C24 . . . . 0.31(18) ?
C22 C23 C24 C25 . . . . -0.28(19) ?
C23 C24 C25 N21 . . . . 0.04(19) ?
C25 N21 C21 C22 . . . . -0.14(18) ?
C26 C22 C23 C24 . . . . -179.96(12) ?
_cod_database_fobs_code 2022930