#------------------------------------------------------------------------------
#$Date: 2023-12-07 12:47:44 +0100 (Thu, 07 Dec 2023) $
#$Revision: 288128 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022929.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_2022929
loop_
_publ_author_name
'Näther, Christian'
'Müller-Meinhard, Asmus'
'Jess, Inke'
_publ_section_title
;
Synthesis, crystal structure and properties of
tetra-kis-(pyridine-3-carbo-nitrile)-dithio-cyanatoiron(II) and of
diaqua-bis-(pyridine-3-carbo-nitrile)-di-thio-cyanatoiron(II)
pyridine-3-carbo-nitrile monosolvate.
;
_journal_coeditor_code HB8079
_journal_issue 'Pt 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)4]'
_chemical_formula_moiety 'C26 H16 Fe N10 S2'
_chemical_formula_sum 'C26 H16 Fe N10 S2'
_chemical_formula_weight 588.46
_chemical_name_systematic
;
Tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II)
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 33
_space_group_name_Hall 'P 2c -2n'
_space_group_name_H-M_alt 'P n a 21'
_atom_sites_solution_hydrogens geom
_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 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 20.3549(2)
_cell_length_b 10.20840(10)
_cell_length_c 13.03100(10)
_cell_measurement_reflns_used 22008
_cell_measurement_temperature 99.99(10)
_cell_measurement_theta_max 79.6930
_cell_measurement_theta_min 4.3390
_cell_volume 2707.72(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.90a (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 1.000
_diffrn_measured_fraction_theta_max 0.990
_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 1.54178
_diffrn_reflns_av_R_equivalents 0.0186
_diffrn_reflns_av_unetI/netI 0.0146
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 26794
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 80.105
_diffrn_reflns_theta_min 4.344
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 6.207
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.74504
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.444
_exptl_crystal_description block
_exptl_crystal_F_000 1200
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.236
_refine_diff_density_min -0.293
_refine_ls_abs_structure_details
;
Classical Flack method preferred over Parsons because s.u. lower
;
_refine_ls_abs_structure_Flack -0.001(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 352
_refine_ls_number_reflns 5727
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0269
_refine_ls_R_factor_gt 0.0267
_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^)+(0.0521P)^2^+0.7383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0736
_refine_ls_wR_factor_ref 0.0738
_reflns_number_gt 5676
_reflns_number_total 5727
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8079sup1.cif
_cod_data_source_block 1
_cod_depositor_comments
'Adding full bibliography for 2022929--2022930.cif.'
_cod_database_code 2022929
_cod_database_fobs_code 2022929
_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 11 0.60 1.10
0 0 10 472.15 9.50
0 0 9 1.20 0.80
0 0 9 0.40 0.90
0 0 8 2597.94 45.50
0 0 8 2493.55 45.40
0 0 7 0.10 0.60
0 0 7 0.60 0.60
0 0 6 171.48 3.60
0 0 5 -0.10 0.40
0 0 4 476.25 8.70
0 0 3 0.20 0.30
0 0 2 6009.60 105.39
0 0 1 0.00 0.10
0 0 -1 0.30 0.10
0 0 -1 0.10 0.10
0 0 -2 6103.59 106.99
0 0 -3 0.20 0.30
0 0 -4 281.47 5.30
0 0 -5 0.00 0.40
0 0 -6 288.07 5.70
0 0 -7 1.00 0.70
0 0 -7 0.10 0.70
0 0 -8 2392.96 42.80
0 0 -8 2391.26 42.80
0 0 -9 2.10 1.00
0 0 -9 -0.60 1.00
0 0 -10 359.36 7.60
0 0 -10 354.16 7.50
0 0 -11 0.60 0.80
0 0 -11 0.60 0.70
0 0 -11 0.00 0.80
0 0 -11 2.50 1.30
0 0 -11 -0.20 1.20
0 0 -12 784.92 14.30
0 0 -12 800.82 14.30
0 0 -12 795.22 14.30
0 0 -13 0.10 0.90
0 0 -13 -1.10 0.90
0 0 -13 -0.50 0.90
0 0 -14 621.34 11.10
0 0 -14 604.94 11.10
0 0 -14 620.54 11.10
0 0 -15 -0.10 0.60
0 0 -16 524.05 9.30
0 1 11 10.70 1.30
0 -1 10 0.80 1.00
0 -1 10 0.40 1.00
0 1 10 0.30 1.00
0 1 9 89.89 2.60
0 -1 9 88.79 2.60
0 -1 9 93.69 2.70
0 1 9 93.39 2.70
0 1 8 -0.10 0.80
0 -1 8 0.50 0.80
0 1 7 15.30 0.90
0 -1 7 13.50 0.90
0 1 7 14.50 0.90
0 1 6 0.30 0.50
0 -1 6 1.00 0.60
0 1 6 0.40 0.50
0 1 5 563.84 10.30
0 1 5 555.54 10.20
0 1 4 0.20 0.10
0 1 4 0.00 0.30
0 -1 4 0.10 0.30
0 1 4 0.30 0.30
0 1 3 543.15 9.50
0 1 3 539.45 9.70
0 1 3 530.35 9.70
0 -1 3 533.45 9.70
0 1 2 0.10 0.10
0 1 2 -0.10 0.20
0 1 1 465.25 8.30
0 -1 1 467.65 8.30
0 1 0 0.60 0.10
0 1 -1 471.65 8.50
0 1 -1 481.35 8.50
0 -1 -1 478.55 8.50
0 1 -2 0.20 0.10
0 -1 -2 0.10 0.20
0 1 -2 0.00 0.20
0 1 -2 0.20 0.20
0 1 -3 490.65 2.30
0 -1 -3 413.46 0.90
0 -1 -4 -0.30 0.40
0 1 -4 0.50 0.40
0 1 -4 0.30 0.10
0 -1 -5 516.75 9.50
0 1 -5 513.85 9.50
0 1 -6 0.50 0.60
0 -1 -6 -0.20 0.50
0 1 -7 32.00 1.30
0 -1 -7 32.60 1.30
0 1 -7 35.30 1.30
0 -1 -7 33.60 1.30
0 -1 -8 -0.30 0.90
0 1 -8 -0.10 0.80
0 1 -8 -0.10 0.80
0 -1 -8 0.30 0.80
0 -1 -9 38.80 1.70
0 1 -9 35.20 1.60
0 -1 -9 36.90 1.70
0 1 -9 32.50 1.60
0 -1 -10 -0.70 1.10
0 1 -10 1.10 1.10
0 -1 -10 0.10 1.10
0 -1 -11 6.10 1.40
0 -1 -11 7.20 1.30
0 1 -11 6.60 1.40
0 -1 -11 8.60 0.80
0 -1 -11 7.30 0.90
0 1 -11 7.10 0.90
0 1 -11 7.60 0.90
0 -1 -11 7.40 0.90
0 1 -11 6.80 0.80
0 1 -11 6.80 0.80
0 -1 -12 -0.30 0.80
0 1 -12 0.00 0.80
0 1 -12 0.40 0.90
0 -1 -12 0.20 0.90
0 1 -12 0.20 0.90
0 -1 -12 0.10 0.80
0 -1 -13 13.70 1.00
0 1 -13 14.70 1.00
0 1 -13 14.40 1.00
0 -1 -13 13.60 1.00
0 -1 -13 13.80 0.90
0 -1 -14 -0.20 0.70
0 1 -14 -0.70 0.80
0 1 -14 -0.50 0.70
0 -1 -14 0.40 0.80
0 -1 -14 0.20 0.80
0 1 -15 1.30 0.60
0 -1 -15 1.70 0.60
0 1 -16 0.00 0.40
0 -1 -16 0.30 0.40
0 2 11 0.40 1.20
0 -2 10 55.89 2.20
0 -2 10 52.99 2.10
0 2 10 48.50 2.10
0 -2 9 0.10 0.90
0 2 9 0.00 1.00
0 -2 8 871.31 16.10
0 2 8 850.21 16.10
0 -2 7 0.40 0.70
0 2 7 2.20 0.70
0 2 6 583.84 10.90
0 -2 6 583.74 10.90
0 2 5 0.40 0.50
0 2 5 0.10 0.20
0 -2 5 0.20 0.50
0 2 4 279.07 5.30
0 -2 4 277.87 5.40
0 2 3 0.30 0.30
0 2 3 -0.10 0.30
0 2 2 457.25 8.30
0 2 1 0.10 0.30
0 2 0 419.06 7.60
0 2 -1 0.10 0.20
0 2 -1 0.10 0.10
0 -2 -1 0.10 0.10
0 2 -2 530.45 9.60
0 2 -2 532.75 9.60
0 2 -3 0.40 0.30
0 2 -3 0.50 0.30
0 -2 -3 0.10 0.40
0 2 -4 334.07 4.80
0 -2 -4 334.37 4.80
0 2 -4 328.37 4.50
0 2 -5 0.50 0.20
0 -2 -5 0.10 0.50
0 -2 -6 495.95 9.40
0 -2 -6 502.45 9.40
0 2 -6 496.35 9.30
0 2 -7 0.60 0.70
0 -2 -7 1.00 0.70
0 -2 -7 0.40 0.70
0 -2 -7 0.30 0.40
0 -2 -8 699.33 13.30
0 -2 -8 728.23 13.30
0 -2 -8 690.73 12.60
0 2 -8 719.63 13.20
0 -2 -9 -0.50 1.00
0 2 -9 0.20 1.00
0 -2 -9 0.80 0.90
0 -2 -10 10.80 1.30
0 2 -10 10.80 1.30
0 -2 -10 11.00 1.30
0 -2 -10 10.90 0.80
0 2 -10 11.20 0.80
0 2 -11 0.10 0.80
0 2 -11 0.80 1.20
0 -2 -11 -0.20 1.20
0 -2 -11 0.30 1.20
0 -2 -11 1.30 0.70
0 2 -11 -0.40 0.80
0 2 -11 0.30 0.80
0 -2 -11 0.40 0.80
0 -2 -11 -0.30 0.80
0 2 -11 -0.40 0.70
0 2 -11 0.00 0.70
0 2 -12 320.97 6.10
0 -2 -12 330.77 6.10
0 2 -12 324.77 6.10
0 2 -12 317.97 6.10
0 -2 -12 327.37 6.10
0 2 -12 321.27 6.10
0 2 -12 323.97 6.10
0 2 -12 331.17 6.10
0 2 -13 1.50 0.90
0 -2 -13 0.40 0.80
0 2 -13 0.50 0.80
0 2 -13 -0.50 0.80
0 -2 -13 0.00 0.80
0 2 -14 213.08 4.10
0 2 -14 209.58 4.10
0 -2 -14 215.28 4.10
0 2 -14 215.78 4.10
0 -2 -14 217.98 4.10
0 -2 -14 216.68 4.10
0 2 -15 0.10 0.60
0 -2 -15 0.10 0.50
0 -2 -15 0.20 0.50
0 2 -15 -0.40 0.50
0 2 -16 43.20 0.90
0 -3 10 -1.20 1.10
0 3 10 -0.20 1.20
0 -3 9 35.10 1.80
0 3 9 39.00 1.80
0 -3 8 0.40 0.90
0 3 8 0.00 0.90
0 3 7 125.29 3.10
0 -3 6 0.10 0.70
0 3 6 0.10 0.70
0 3 5 367.36 6.90
0 -3 5 370.06 7.00
0 3 5 346.67 6.70
0 3 4 -0.10 0.50
0 3 4 0.50 0.40
0 -3 4 -0.20 0.50
0 3 3 777.12 13.90
0 3 3 758.22 13.80
0 3 2 0.90 0.40
0 3 2 0.60 0.40
0 3 1 1572.64 28.60
0 3 1 1651.23 28.60
0 3 0 0.10 0.40
0 3 -1 1312.17 19.50
0 3 -1 1363.46 19.30
0 3 -2 0.30 0.30
0 3 -2 0.20 0.20
0 3 -2 0.10 0.40
0 -3 -2 0.20 0.20
0 3 -3 996.50 17.90
0 3 -3 993.30 17.80
0 -3 -3 1000.10 17.80
0 3 -3 1016.90 17.90
0 -3 -3 996.50 18.00
0 3 -4 0.30 0.40
0 3 -4 -0.10 0.40
0 -3 -4 0.10 0.50
0 -3 -4 -0.30 0.40
0 3 -4 0.20 0.40
0 3 -5 420.26 7.90
0 -3 -5 422.56 7.90
0 3 -5 428.86 7.80
0 -3 -6 1.10 0.60
0 3 -6 1.20 0.60
0 -3 -6 0.50 0.70
0 -3 -7 36.00 1.30
0 -3 -7 36.00 0.90
0 3 -7 37.10 1.40
0 -3 -8 0.00 0.50
0 -3 -8 0.30 0.80
0 -3 -8 0.90 0.90
0 3 -8 0.50 0.80
0 -3 -9 1.60 0.60
0 3 -9 0.70 0.90
0 -3 -9 1.20 1.10
0 -3 -9 0.90 0.90
0 -3 -10 0.40 1.10
0 -3 -10 0.30 1.20
0 3 -10 0.40 1.10
0 3 -10 0.30 0.60
0 3 -10 0.20 0.70
0 -3 -10 0.10 0.60
0 -3 -10 -0.10 0.70
0 3 -10 0.20 0.70
0 3 -10 0.50 0.70
0 3 -11 365.66 6.70
0 -3 -11 365.76 6.70
0 -3 -11 361.76 6.70
0 3 -11 353.66 6.70
0 3 -11 365.96 6.80
0 3 -11 363.16 6.70
0 3 -12 0.30 0.70
0 3 -12 2.20 0.70
0 -3 -12 0.60 0.80
0 -3 -12 1.90 0.80
0 3 -12 -0.10 0.70
0 3 -12 0.60 0.70
0 3 -12 0.70 0.80
0 3 -12 0.10 0.80
0 3 -13 384.36 7.20
0 3 -13 403.66 7.30
0 -3 -13 397.96 7.30
0 3 -13 395.36 7.30
0 3 -13 397.16 7.30
0 -3 -13 398.36 7.30
0 3 -14 0.50 0.60
0 -3 -14 0.50 0.60
0 3 -14 0.60 0.70
0 -3 -14 0.00 0.70
0 -3 -15 102.39 2.00
0 -3 -15 104.79 2.10
0 3 -15 107.89 2.10
0 4 14 71.09 1.50
0 4 12 125.29 2.50
0 -4 10 120.59 3.60
0 4 10 122.49 3.60
0 -4 9 -0.40 1.10
0 4 9 0.00 1.10
0 4 8 202.78 4.70
0 4 7 0.30 0.90
0 -4 7 -0.10 0.90
0 4 6 382.26 7.50
0 -4 6 373.26 7.70
0 -4 5 0.30 0.80
0 4 5 1.10 0.50
0 4 5 0.70 0.70
0 -4 4 122.69 3.10
0 4 4 128.09 2.90
0 4 4 128.29 2.80
0 4 3 0.10 0.60
0 4 3 0.00 0.50
0 4 2 42.50 1.30
0 4 2 41.50 1.30
0 4 1 -0.20 0.50
0 4 0 1004.70 18.10
0 4 0 1045.40 18.40
0 4 -1 0.30 0.50
0 4 -1 0.20 0.30
0 4 -2 53.19 1.40
0 4 -2 49.50 1.20
0 4 -3 0.80 0.50
0 -4 -3 0.30 0.30
0 4 -3 0.10 0.30
0 -4 -3 0.70 0.60
0 4 -3 1.10 0.40
0 4 -4 94.29 2.20
0 -4 -4 95.39 2.00
0 4 -4 92.19 2.00
0 4 -4 95.19 2.20
0 -4 -5 0.30 0.70
0 4 -5 -0.10 0.50
0 4 -5 0.20 0.50
0 -4 -5 0.30 0.50
0 -4 -6 237.08 4.70
0 4 -6 236.18 4.70
0 4 -6 234.68 4.60
0 -4 -7 -0.10 0.50
0 4 -7 -0.40 0.70
0 -4 -7 0.30 0.70
0 -4 -7 -0.20 0.90
0 -4 -8 155.58 3.70
0 4 -8 155.28 3.70
0 -4 -8 160.68 3.20
0 -4 -8 157.78 4.00
0 4 -9 0.10 0.70
0 -4 -9 -0.10 0.90
0 4 -9 0.80 0.90
0 -4 -9 0.20 1.10
0 -4 -9 0.00 0.70
0 4 -10 136.79 3.70
0 -4 -10 146.69 4.00
0 4 -10 146.29 2.90
0 4 -10 149.09 2.90
0 4 -10 146.59 2.90
0 4 -10 158.58 3.10
0 -4 -11 -0.30 0.70
0 4 -11 -0.60 0.70
0 -4 -11 0.30 0.70
0 4 -11 -0.30 0.70
0 4 -11 0.10 0.70
0 4 -11 0.20 0.80
0 -4 -12 93.69 2.10
0 4 -12 96.99 2.00
0 -4 -12 96.29 2.10
0 4 -12 90.19 2.00
0 4 -12 94.69 2.00
0 4 -12 100.49 2.20
0 4 -13 0.10 0.60
0 -4 -13 0.20 0.60
0 4 -13 0.40 0.70
0 4 -13 -0.40 0.80
0 4 -13 0.00 0.60
0 -4 -14 61.09 1.30
0 4 -14 57.19 1.30
0 -4 -15 0.30 0.40
0 4 -15 -0.50 0.40
0 5 14 -0.20 0.40
0 5 12 -0.30 0.60
0 5 12 0.50 0.60
0 5 10 0.60 0.60
0 -5 9 353.06 7.90
0 5 9 367.46 7.80
0 5 8 1.00 1.10
0 -5 7 83.79 2.70
0 5 7 78.99 2.60
0 5 6 1.00 0.90
0 -5 6 -0.40 1.00
0 -5 5 638.14 12.00
0 5 5 630.94 11.80
0 5 4 1.30 0.80
0 -5 4 -0.10 0.90
0 5 3 358.66 7.10
0 5 3 358.36 7.00
0 5 2 -0.10 0.70
0 5 2 1.10 0.70
0 5 1 855.31 15.70
0 5 0 0.70 0.60
0 5 0 0.30 0.30
0 5 0 0.30 0.60
0 5 -1 777.02 13.30
0 5 -1 695.13 12.90
0 5 -2 0.30 0.40
0 5 -2 0.40 0.60
0 5 -3 336.97 6.50
0 5 -3 351.16 6.70
0 5 -4 -0.20 0.60
0 5 -4 1.00 0.70
0 -5 -4 -0.40 0.70
0 -5 -5 493.05 10.00
0 5 -5 526.05 9.70
0 5 -6 0.20 0.60
0 -5 -7 54.99 2.10
0 -5 -7 55.89 1.40
0 -5 -8 0.40 1.10
0 -5 -8 0.20 0.70
0 -5 -9 429.76 9.30
0 -5 -9 443.86 8.30
0 5 -9 458.25 8.30
0 5 -9 456.65 8.30
0 5 -10 -0.30 0.80
0 5 -10 1.00 0.80
0 -5 -10 0.20 0.70
0 5 -10 0.30 0.80
0 5 -11 201.38 4.00
0 5 -12 -0.70 0.80
0 -5 -12 -0.30 0.80
0 5 -13 313.47 5.80
0 5 -13 318.27 5.80
0 -5 -13 321.87 5.80
0 5 -14 -0.30 0.50
0 -5 -14 -0.20 0.60
0 5 -14 0.10 0.40
0 -5 -15 7.70 0.40
0 6 13 0.00 0.40
0 6 12 15.80 0.80
0 6 12 14.30 0.70
0 6 11 0.30 0.70
0 6 11 0.00 0.60
0 6 10 20.30 0.90
0 6 9 -0.20 0.60
0 6 8 744.63 14.50
0 -6 7 0.50 1.20
0 6 7 1.40 1.20
0 -6 6 358.46 7.70
0 6 6 344.37 7.40
0 6 5 1.20 0.80
0 -6 5 -0.10 1.10
0 6 5 0.20 1.00
0 -6 4 253.67 5.50
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-22 -2 -1 18.70 0.90
-22 2 -1 19.00 0.80
-22 -2 -2 41.20 1.10
-22 2 -2 41.30 1.10
-22 2 -2 41.80 1.10
22 -2 -2 39.90 1.00
-22 2 -2 40.50 1.10
-22 -2 -2 42.30 1.20
-22 2 -3 6.10 0.60
-22 -2 -3 6.80 0.60
22 -2 -3 6.00 0.50
-22 2 -3 6.40 0.60
-22 2 -3 7.00 0.70
22 -2 -3 6.00 0.60
-22 2 -3 6.10 0.60
-22 -2 -3 6.30 0.60
22 -2 -4 41.30 1.00
-22 2 -4 42.00 1.10
22 -2 -4 40.40 1.10
-22 2 -4 40.90 1.10
-22 -2 -4 41.20 1.10
22 -2 -5 24.20 0.70
-22 2 -5 25.20 0.80
22 -2 -5 24.40 0.80
-22 2 -5 25.30 0.80
-22 -2 -5 25.40 0.80
22 -2 -6 7.10 0.50
-22 2 -6 6.20 0.50
22 -2 -6 6.50 0.50
22 2 -6 7.10 0.50
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22 -2 -7 23.10 0.60
22 2 -7 22.20 0.60
22 -2 -8 15.70 0.40
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-22 3 6 7.20 0.50
-22 3 5 11.60 0.60
-22 -3 5 10.50 0.50
-22 3 4 5.50 0.60
-22 -3 4 5.80 0.50
-22 3 3 3.90 0.60
-22 3 3 3.40 0.40
-22 3 3 4.30 0.50
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-22 3 2 3.50 0.50
-22 -3 2 4.20 0.50
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-22 3 1 236.08 4.30
-22 -3 1 236.68 4.30
-22 3 1 224.28 4.30
-22 3 0 5.60 0.70
-22 3 0 4.00 0.50
-22 -3 0 5.10 0.60
-22 3 0 5.10 0.50
-22 -3 0 5.10 0.60
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-22 3 -1 225.98 4.30
-22 -3 -1 231.78 4.30
-22 -3 -1 228.68 4.30
-22 3 -1 234.08 4.30
-22 3 -2 15.00 0.70
-22 3 -2 14.00 0.70
-22 -3 -2 15.30 0.70
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-22 3 -2 14.20 0.60
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-22 3 -3 34.00 0.90
-22 3 -3 33.50 0.90
-22 -3 -3 31.50 0.90
-22 3 -3 33.70 0.90
-22 -3 -3 32.50 0.90
22 -3 -4 14.40 0.50
-22 3 -4 14.50 0.60
-22 -3 -4 15.00 0.60
-22 3 -5 0.70 0.40
22 -3 -5 1.20 0.40
-22 3 -5 1.70 0.50
22 3 -6 2.30 0.40
22 -3 -6 2.10 0.30
-22 3 -6 2.00 0.40
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-22 3 -7 65.79 1.20
-22 4 6 14.50 0.40
-22 4 5 1.50 0.40
-22 -4 4 48.00 1.10
-22 4 4 50.79 1.10
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-22 -4 2 31.40 0.80
-22 -4 1 0.80 0.50
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-22 4 0 27.30 0.80
-22 4 -1 2.10 0.50
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-22 4 -2 24.20 0.80
-22 4 -2 24.90 0.80
-22 4 -3 2.90 0.50
-22 4 -3 2.40 0.50
-22 4 -3 2.10 0.40
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-22 4 -4 37.60 0.90
-22 4 -5 0.70 0.40
-22 4 -7 0.50 0.20
-22 5 5 11.00 0.30
-22 5 4 37.30 0.80
-22 5 3 29.90 0.70
-22 5 3 24.70 0.60
-22 5 2 28.20 0.80
-22 5 2 26.90 0.70
-22 5 1 51.59 1.10
-22 5 1 49.00 1.10
-22 5 0 20.60 0.70
-22 5 0 20.50 0.60
-22 5 -1 34.00 0.90
-22 5 -1 31.60 0.80
-22 5 -2 20.00 0.60
-22 5 -2 21.80 0.70
-22 5 -3 20.70 0.60
-22 5 -3 20.60 0.60
-22 5 -3 20.30 0.60
-22 5 -4 36.60 0.80
-22 5 -4 36.40 0.80
-22 5 -5 14.40 0.40
-22 5 -5 17.00 0.50
-22 5 -6 55.59 1.10
-22 6 3 0.90 0.20
-22 6 2 34.70 0.80
-22 6 1 18.90 0.60
-22 6 0 3.40 0.20
-22 6 0 5.30 0.40
-22 6 -1 8.20 0.30
-22 6 -1 11.90 0.40
-22 6 -2 3.50 0.30
-22 6 -2 2.60 0.20
-22 6 -3 2.50 0.30
-22 6 -3 2.30 0.20
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-22 6 -4 70.19 1.30
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-23 0 5 0.30 0.50
-23 0 4 0.10 0.50
-23 0 3 0.20 0.50
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-23 0 2 0.10 0.50
-23 0 1 -0.20 0.60
-23 0 1 0.40 0.50
-23 0 1 0.00 0.50
-23 0 0 0.00 0.60
-23 0 0 -0.10 0.50
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-23 0 -1 -0.20 0.60
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-23 0 -2 0.10 0.50
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23 0 -3 0.10 0.50
-23 0 -3 -0.20 0.50
-23 0 -3 -0.50 0.50
-23 0 -4 0.40 0.50
23 0 -4 0.10 0.50
23 0 -5 0.10 0.40
23 0 -5 0.00 0.40
23 0 -6 0.20 0.40
23 0 -6 -0.10 0.40
23 0 -7 -0.20 0.30
23 0 -7 0.40 0.30
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-23 -1 7 164.98 3.10
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-23 1 6 7.30 0.40
-23 -1 6 7.30 0.40
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-23 -1 1 96.69 2.00
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-23 -1 1 98.19 2.00
-23 1 1 97.59 2.00
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-23 1 0 1.20 0.50
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-23 1 0 1.90 0.50
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-23 1 -1 58.69 1.30
-23 -1 -1 58.09 1.40
-23 1 -1 57.59 1.40
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-23 1 -2 8.80 0.60
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-23 -1 -2 8.50 0.60
-23 1 -2 8.60 0.60
23 -1 -3 8.90 0.50
23 1 -3 9.40 0.50
-23 1 -3 8.30 0.60
-23 -1 -3 8.80 0.60
23 -1 -3 8.70 0.50
-23 1 -3 9.00 0.60
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-23 1 -3 8.50 0.60
-23 1 -4 22.70 0.70
23 -1 -4 22.10 0.70
23 1 -4 22.70 0.70
-23 1 -4 23.70 0.80
-23 -1 -4 24.00 0.80
23 -1 -4 23.40 0.70
23 -1 -5 30.70 0.80
-23 1 -5 30.00 0.80
23 -1 -5 31.60 0.80
-23 1 -5 31.80 0.80
-23 -1 -5 32.70 0.80
23 -1 -6 0.80 0.40
23 1 -6 0.90 0.40
23 -1 -6 0.30 0.30
23 1 -6 0.30 0.40
23 -1 -7 156.38 2.90
23 1 -7 156.48 2.90
-23 2 7 10.40 0.30
-23 2 6 77.29 1.50
-23 2 5 10.30 0.40
-23 2 5 12.20 0.50
-23 2 4 56.39 1.20
-23 2 3 12.60 0.50
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-23 2 2 5.90 0.50
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-23 2 -1 112.49 2.20
-23 -2 -1 117.99 2.30
-23 -2 -1 112.69 2.30
-23 2 -1 117.99 2.30
-23 2 -1 114.59 2.20
-23 2 -2 6.60 0.50
-23 -2 -2 6.70 0.60
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23 2 -3 10.00 0.60
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23 2 -4 44.00 1.00
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23 2 -5 3.70 0.40
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23 2 -6 66.79 1.20
-23 2 -6 61.09 1.20
23 2 -7 16.60 0.40
23 2 -7 16.00 0.40
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23 3 -6 3.80 0.30
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-23 4 4 77.79 1.60
-23 4 3 3.10 0.30
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-23 4 2 97.39 1.90
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-23 4 -1 33.60 0.80
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-23 4 -1 33.60 0.90
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-23 4 -2 143.19 2.70
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-23 4 -3 9.50 0.40
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23 4 -5 37.40 0.80
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24 0 -3 23.10 0.60
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24 0 -4 26.50 0.70
24 0 -5 23.90 0.60
24 0 -5 20.70 0.50
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24 1 -4 18.20 0.60
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0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 21818
_shelx_res_file
;
TITL amm31_a_a.res in Pna2(1)
amm31.res
created by SHELXL-2016/6 at 15:35:07 on 21-Sep-2023
REM Old TITL amm31_a in Pnma
REM SHELXT solution in Pna2(1)
REM R1 0.090, Rweak 0.016, Alpha 0.002, Orientation a'=-a, b'=c, c'=b
REM Flack x = -0.214 ( 0.037 ) from Parsons' quotients
REM Formula found by SHELXT: C26 N10 S2 Fe
CELL 1.54178 20.3549 10.2084 13.031 90 90 90
ZERR 4 0.0002 0.0001 0.0001 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,0.5+Z
SFAC C H Fe N S
UNIT 104 64 4 40 8
EQIV $1 1-X,-Y,-0.5+Z
EQIV $2 1-X,1-Y,0.5+Z
EQIV $3 1-X,1-Y,-0.5+Z
EQIV $4 1.5-X,0.5+Y,0.5+Z
L.S. 10
PLAN 1
TEMP -273.15
HTAB C11 N1
HTAB C15 N2
HTAB C21 N2
HTAB C24 N22_$1
HTAB C25 N1
HTAB C31 N1
HTAB C35 N2
HTAB C35 N12_$2
HTAB C41 N22_$3
HTAB C44 S1_$4
HTAB C45 N2
BOND $H
HTAB
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.052100 0.738300
FVAR 0.33630
FE1 3 0.616437 0.577149 0.502081 11.00000 0.01820 0.01806 =
0.01250 0.00084 0.00061 -0.00105
N1 4 0.609471 0.580261 0.344039 11.00000 0.02733 0.02407 =
0.01468 0.00037 -0.00050 0.00009
C1 1 0.604372 0.572233 0.254877 11.00000 0.01542 0.01652 =
0.02255 0.00161 0.00182 0.00064
S1 5 0.597566 0.560508 0.131178 11.00000 0.02461 0.02783 =
0.01452 -0.00176 -0.00007 0.00403
N2 4 0.622053 0.573467 0.660625 11.00000 0.02333 0.02197 =
0.01667 0.00096 -0.00130 -0.00014
C2 1 0.610597 0.587191 0.747408 11.00000 0.02085 0.01594 =
0.01849 0.00243 -0.00290 -0.00198
S2 5 0.592680 0.606261 0.867790 11.00000 0.04669 0.02347 =
0.01615 -0.00073 0.00552 -0.00191
N11 4 0.519763 0.685786 0.515926 11.00000 0.01949 0.01687 =
0.01959 0.00017 0.00078 -0.00214
C11 1 0.474637 0.679426 0.441723 11.00000 0.02222 0.01828 =
0.01751 0.00107 0.00076 -0.00189
AFIX 43
H11 2 0.485160 0.634024 0.380244 11.00000 -1.20000
AFIX 0
C12 1 0.412487 0.736867 0.450766 11.00000 0.02102 0.01873 =
0.02103 0.00083 -0.00019 -0.00230
C13 1 0.396338 0.802666 0.540480 11.00000 0.02329 0.01769 =
0.02430 0.00063 0.00016 -0.00007
AFIX 43
H13 2 0.354112 0.840674 0.549291 11.00000 -1.20000
AFIX 0
C14 1 0.443486 0.811392 0.616822 11.00000 0.02855 0.01895 =
0.02061 -0.00398 -0.00036 0.00117
AFIX 43
H14 2 0.434368 0.856933 0.678783 11.00000 -1.20000
AFIX 0
C15 1 0.504227 0.752731 0.601613 11.00000 0.02512 0.01931 =
0.01986 -0.00130 -0.00212 -0.00220
AFIX 43
H15 2 0.536372 0.760156 0.654147 11.00000 -1.20000
AFIX 0
C16 1 0.365871 0.727124 0.368127 11.00000 0.02598 0.01951 =
0.02455 0.00014 -0.00016 0.00177
N12 4 0.327753 0.723087 0.302983 11.00000 0.03243 0.02985 =
0.03139 -0.00300 -0.01005 0.00197
N21 4 0.574909 0.370543 0.505759 11.00000 0.01870 0.01996 =
0.01823 -0.00001 0.00065 -0.00091
C21 1 0.549897 0.319845 0.591966 11.00000 0.01966 0.01967 =
0.02013 -0.00203 0.00154 -0.00053
AFIX 43
H21 2 0.547628 0.373602 0.651370 11.00000 -1.20000
AFIX 0
C22 1 0.526996 0.191241 0.598254 11.00000 0.01966 0.02028 =
0.02297 0.00181 0.00393 0.00060
C23 1 0.530705 0.110316 0.512175 11.00000 0.02636 0.01926 =
0.02757 -0.00107 0.00381 -0.00096
AFIX 43
H23 2 0.516095 0.021992 0.514719 11.00000 -1.20000
AFIX 0
C24 1 0.556326 0.162948 0.423185 11.00000 0.03269 0.02037 =
0.02438 -0.00373 0.00356 -0.00133
AFIX 43
H24 2 0.559409 0.111195 0.362787 11.00000 -1.20000
AFIX 0
C25 1 0.577553 0.292228 0.422739 11.00000 0.02837 0.02190 =
0.01914 0.00005 0.00369 0.00006
AFIX 43
H25 2 0.594798 0.327145 0.360763 11.00000 -1.20000
AFIX 0
C26 1 0.497119 0.146109 0.691823 11.00000 0.02842 0.01848 =
0.02801 -0.00191 0.00601 -0.00036
N22 4 0.471356 0.110450 0.765171 11.00000 0.04165 0.02248 =
0.03333 0.00106 0.01406 -0.00153
N31 4 0.715450 0.478301 0.493418 11.00000 0.02079 0.02072 =
0.02102 0.00055 0.00048 0.00060
C31 1 0.754129 0.486888 0.410411 11.00000 0.02194 0.02062 =
0.02316 -0.00102 0.00205 -0.00202
AFIX 43
H31 2 0.738616 0.533481 0.352142 11.00000 -1.20000
AFIX 0
C32 1 0.816166 0.429984 0.406606 11.00000 0.02227 0.02159 =
0.02738 -0.00496 0.00377 -0.00167
C33 1 0.840212 0.363354 0.492115 11.00000 0.02460 0.02549 =
0.03237 -0.00630 -0.00254 0.00681
AFIX 43
H33 2 0.882745 0.325046 0.491573 11.00000 -1.20000
AFIX 0
C34 1 0.800293 0.354677 0.577791 11.00000 0.03280 0.02871 =
0.02626 -0.00020 -0.00371 0.01025
AFIX 43
H34 2 0.815036 0.310288 0.637584 11.00000 -1.20000
AFIX 0
C35 1 0.738254 0.411856 0.575179 11.00000 0.02782 0.02479 =
0.02191 -0.00013 0.00263 0.00478
AFIX 43
H35 2 0.710769 0.403611 0.633745 11.00000 -1.20000
AFIX 0
C36 1 0.854430 0.439510 0.313557 11.00000 0.02337 0.02573 =
0.03625 -0.00493 0.00578 0.00049
N32 4 0.883996 0.446902 0.238923 11.00000 0.03329 0.03155 =
0.04558 -0.00314 0.01461 0.00100
N41 4 0.670374 0.767691 0.499031 11.00000 0.01815 0.01928 =
0.01960 0.00182 -0.00111 -0.00124
C41 1 0.666332 0.853804 0.421875 11.00000 0.01954 0.02242 =
0.02167 0.00110 -0.00028 0.00106
AFIX 43
H41 2 0.635285 0.838771 0.368733 11.00000 -1.20000
AFIX 0
C42 1 0.706111 0.964878 0.416741 11.00000 0.02120 0.02278 =
0.02212 0.00417 0.00368 0.00029
C43 1 0.751407 0.989246 0.494252 11.00000 0.02312 0.02706 =
0.02876 0.00228 0.00068 -0.00691
AFIX 43
H43 2 0.779162 1.064013 0.492090 11.00000 -1.20000
AFIX 0
C44 1 0.754730 0.900825 0.574799 11.00000 0.02400 0.03291 =
0.02497 0.00252 -0.00471 -0.00795
AFIX 43
H44 2 0.784604 0.914585 0.629764 11.00000 -1.20000
AFIX 0
C45 1 0.713977 0.792156 0.574212 11.00000 0.02299 0.02416 =
0.02151 0.00277 -0.00303 -0.00176
AFIX 43
H45 2 0.716965 0.731957 0.629611 11.00000 -1.20000
AFIX 0
C46 1 0.700857 1.052316 0.329758 11.00000 0.02410 0.02409 =
0.02970 0.00391 0.00409 -0.00115
N42 4 0.696446 1.120967 0.260986 11.00000 0.03394 0.03557 =
0.03563 0.01301 0.00476 -0.00058
HKLF 4
REM amm31_a_a.res in Pna2(1)
REM R1 = 0.0267 for 5676 Fo > 4sig(Fo) and 0.0269 for all 5727 data
REM 352 parameters refined using 1 restraints
END
WGHT 0.0521 0.7342
REM Instructions for potential hydrogen bonds
HTAB C11 N1
HTAB C15 N2
HTAB C21 N2
HTAB C24 N22_$1
HTAB C25 N1
HTAB C31 N1
HTAB C35 N2
HTAB C35 N12_$2
HTAB C41 N22_$3
HTAB C44 S1_$4
HTAB C45 N2
REM Highest difference peak 0.236, deepest hole -0.293, 1-sigma level 0.043
Q1 1 0.6104 0.5814 0.3979 11.00000 0.05 0.24
;
_shelx_res_checksum 77165
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'
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 0.61644(2) 0.57715(4) 0.50208(3) 0.01625(10) Uani d 1 . .
N N1 0.60947(11) 0.5803(2) 0.34404(18) 0.0220(5) Uani d 1 . .
C C1 0.60437(12) 0.5722(2) 0.2549(2) 0.0182(5) Uani d 1 . .
S S1 0.59757(3) 0.56051(6) 0.13118(5) 0.02232(13) Uani d 1 . .
N N2 0.62205(11) 0.5735(2) 0.66062(18) 0.0207(5) Uani d 1 . .
C C2 0.61060(12) 0.5872(2) 0.7474(2) 0.0184(5) Uani d 1 . .
S S2 0.59268(4) 0.60626(6) 0.86779(5) 0.02877(15) Uani d 1 . .
N N11 0.51976(9) 0.68579(19) 0.51593(16) 0.0186(4) Uani d 1 . .
C C11 0.47464(12) 0.6794(2) 0.44172(17) 0.0193(4) Uani d 1 . .
H H11 0.485160 0.634024 0.380244 0.023 Uiso calc 1 . .
C C12 0.41249(12) 0.7369(2) 0.45077(19) 0.0203(5) Uani d 1 . .
C C13 0.39634(12) 0.8027(2) 0.5405(2) 0.0218(5) Uani d 1 . .
H H13 0.354112 0.840674 0.549291 0.026 Uiso calc 1 . .
C C14 0.44349(12) 0.8114(2) 0.61682(19) 0.0227(5) Uani d 1 . .
H H14 0.434368 0.856933 0.678783 0.027 Uiso calc 1 . .
C C15 0.50423(12) 0.7527(2) 0.60161(18) 0.0214(5) Uani d 1 . .
H H15 0.536372 0.760156 0.654147 0.026 Uiso calc 1 . .
C C16 0.36587(13) 0.7271(2) 0.3681(2) 0.0233(5) Uani d 1 . .
N N12 0.32775(12) 0.7231(2) 0.30298(19) 0.0312(5) Uani d 1 . .
N N21 0.57491(9) 0.37054(19) 0.50576(17) 0.0190(4) Uani d 1 . .
C C21 0.54990(11) 0.3198(2) 0.59197(19) 0.0198(4) Uani d 1 . .
H H21 0.547628 0.373602 0.651370 0.024 Uiso calc 1 . .
C C22 0.52700(11) 0.1912(2) 0.59825(19) 0.0210(5) Uani d 1 . .
C C23 0.53071(12) 0.1103(2) 0.5122(2) 0.0244(5) Uani d 1 . .
H H23 0.516095 0.021992 0.514719 0.029 Uiso calc 1 . .
C C24 0.55633(13) 0.1629(2) 0.4232(2) 0.0258(5) Uani d 1 . .
H H24 0.559409 0.111195 0.362787 0.031 Uiso calc 1 . .
C C25 0.57755(13) 0.2922(2) 0.4227(2) 0.0231(5) Uani d 1 . .
H H25 0.594798 0.327145 0.360763 0.028 Uiso calc 1 . .
C C26 0.49712(13) 0.1461(3) 0.6918(2) 0.0250(5) Uani d 1 . .
N N22 0.47136(13) 0.1104(2) 0.7652(2) 0.0325(5) Uani d 1 . .
N N31 0.71545(9) 0.4783(2) 0.49342(16) 0.0208(4) Uani d 1 . .
C C31 0.75413(12) 0.4869(2) 0.4104(2) 0.0219(5) Uani d 1 . .
H H31 0.738616 0.533481 0.352142 0.026 Uiso calc 1 . .
C C32 0.81617(13) 0.4300(2) 0.4066(2) 0.0237(5) Uani d 1 . .
C C33 0.84021(12) 0.3634(3) 0.4921(2) 0.0275(5) Uani d 1 . .
H H33 0.882745 0.325046 0.491573 0.033 Uiso calc 1 . .
C C34 0.80029(14) 0.3547(3) 0.5778(2) 0.0293(5) Uani d 1 . .
H H34 0.815036 0.310288 0.637584 0.035 Uiso calc 1 . .
C C35 0.73825(13) 0.4119(2) 0.5752(2) 0.0248(5) Uani d 1 . .
H H35 0.710769 0.403611 0.633745 0.030 Uiso calc 1 . .
C C36 0.85443(14) 0.4395(3) 0.3136(2) 0.0285(6) Uani d 1 . .
N N32 0.88400(12) 0.4469(3) 0.2389(2) 0.0368(6) Uani d 1 . .
N N41 0.67037(9) 0.76769(19) 0.49903(17) 0.0190(4) Uani d 1 . .
C C41 0.66633(11) 0.8538(2) 0.42188(19) 0.0212(4) Uani d 1 . .
H H41 0.635285 0.838771 0.368733 0.025 Uiso calc 1 . .
C C42 0.70611(12) 0.9649(3) 0.4167(2) 0.0220(5) Uani d 1 . .
C C43 0.75141(12) 0.9892(3) 0.4943(2) 0.0263(5) Uani d 1 . .
H H43 0.779162 1.064013 0.492090 0.032 Uiso calc 1 . .
C C44 0.75473(13) 0.9008(3) 0.5748(2) 0.0273(5) Uani d 1 . .
H H44 0.784604 0.914585 0.629764 0.033 Uiso calc 1 . .
C C45 0.71398(12) 0.7922(3) 0.5742(2) 0.0229(5) Uani d 1 . .
H H45 0.716965 0.731957 0.629611 0.027 Uiso calc 1 . .
C C46 0.70086(13) 1.0523(3) 0.3298(2) 0.0260(5) Uani d 1 . .
N N42 0.69645(12) 1.1210(3) 0.2610(2) 0.0350(6) 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
Fe1 0.01820(17) 0.01806(17) 0.01250(17) -0.00105(13) 0.00061(15) 0.00084(13)
N1 0.0273(11) 0.0241(11) 0.0147(12) 0.0001(8) -0.0005(8) 0.0004(7)
C1 0.0154(10) 0.0165(11) 0.0225(15) 0.0006(8) 0.0018(9) 0.0016(9)
S1 0.0246(3) 0.0278(3) 0.0145(3) 0.0040(2) -0.0001(2) -0.0018(2)
N2 0.0233(10) 0.0220(11) 0.0167(11) -0.0001(8) -0.0013(7) 0.0010(7)
C2 0.0208(11) 0.0159(11) 0.0185(14) -0.0020(8) -0.0029(9) 0.0024(9)
S2 0.0467(4) 0.0235(3) 0.0162(3) -0.0019(3) 0.0055(3) -0.0007(3)
N11 0.0195(8) 0.0169(9) 0.0196(10) -0.0021(7) 0.0008(7) 0.0002(7)
C11 0.0222(11) 0.0183(10) 0.0175(11) -0.0019(8) 0.0008(8) 0.0011(8)
C12 0.0210(11) 0.0187(11) 0.0210(12) -0.0023(8) -0.0002(9) 0.0008(9)
C13 0.0233(11) 0.0177(11) 0.0243(12) -0.0001(9) 0.0002(9) 0.0006(9)
C14 0.0286(12) 0.0189(11) 0.0206(12) 0.0012(9) -0.0004(9) -0.0040(9)
C15 0.0251(11) 0.0193(10) 0.0199(11) -0.0022(9) -0.0021(9) -0.0013(9)
C16 0.0260(12) 0.0195(11) 0.0245(12) 0.0018(9) -0.0002(10) 0.0001(10)
N12 0.0324(12) 0.0298(11) 0.0314(13) 0.0020(10) -0.0101(10) -0.0030(9)
N21 0.0187(8) 0.0200(9) 0.0182(9) -0.0009(7) 0.0006(7) 0.0000(8)
C21 0.0197(10) 0.0197(11) 0.0201(11) -0.0005(8) 0.0015(8) -0.0020(9)
C22 0.0197(10) 0.0203(11) 0.0230(12) 0.0006(8) 0.0039(9) 0.0018(9)
C23 0.0264(11) 0.0193(11) 0.0276(13) -0.0010(9) 0.0038(10) -0.0011(10)
C24 0.0327(13) 0.0204(12) 0.0244(12) -0.0013(10) 0.0036(10) -0.0037(10)
C25 0.0284(12) 0.0219(12) 0.0191(11) 0.0001(9) 0.0037(9) 0.0001(9)
C26 0.0284(12) 0.0185(11) 0.0280(13) -0.0004(9) 0.0060(10) -0.0019(10)
N22 0.0417(14) 0.0225(11) 0.0333(13) -0.0015(9) 0.0141(10) 0.0011(9)
N31 0.0208(9) 0.0207(9) 0.0210(10) 0.0006(7) 0.0005(8) 0.0005(8)
C31 0.0219(11) 0.0206(11) 0.0232(11) -0.0020(9) 0.0021(9) -0.0010(9)
C32 0.0223(12) 0.0216(12) 0.0274(14) -0.0017(9) 0.0038(10) -0.0050(9)
C33 0.0246(11) 0.0255(11) 0.0324(14) 0.0068(10) -0.0025(10) -0.0063(10)
C34 0.0328(13) 0.0287(13) 0.0263(13) 0.0102(11) -0.0037(10) -0.0002(11)
C35 0.0278(12) 0.0248(11) 0.0219(12) 0.0048(10) 0.0026(10) -0.0001(10)
C36 0.0234(13) 0.0257(12) 0.0363(15) 0.0005(9) 0.0058(11) -0.0049(11)
N32 0.0333(13) 0.0315(12) 0.0456(16) 0.0010(9) 0.0146(11) -0.0031(11)
N41 0.0182(8) 0.0193(9) 0.0196(8) -0.0012(7) -0.0011(8) 0.0018(8)
C41 0.0195(10) 0.0224(11) 0.0217(11) 0.0011(9) -0.0003(9) 0.0011(10)
C42 0.0212(10) 0.0228(11) 0.0221(12) 0.0003(9) 0.0037(9) 0.0042(10)
C43 0.0231(11) 0.0271(12) 0.0288(13) -0.0069(9) 0.0007(10) 0.0023(10)
C44 0.0240(12) 0.0329(13) 0.0250(13) -0.0080(10) -0.0047(10) 0.0025(11)
C45 0.0230(11) 0.0242(11) 0.0215(11) -0.0018(9) -0.0030(9) 0.0028(10)
C46 0.0241(12) 0.0241(12) 0.0297(14) -0.0011(9) 0.0041(10) 0.0039(11)
N42 0.0339(12) 0.0356(13) 0.0356(14) -0.0006(10) 0.0048(10) 0.0130(11)
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'
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 N2 . . 179.21(9) y
N1 Fe1 N11 . . 90.70(8) y
N1 Fe1 N21 . . 90.56(8) y
N1 Fe1 N31 . . 91.05(8) y
N1 Fe1 N41 . . 90.15(9) y
N2 Fe1 N11 . . 88.70(8) y
N2 Fe1 N21 . . 89.00(8) y
N2 Fe1 N31 . . 89.57(8) y
N2 Fe1 N41 . . 90.37(8) y
N11 Fe1 N21 . . 97.44(7) y
N31 Fe1 N11 . . 176.72(7) y
N31 Fe1 N21 . . 85.31(7) y
N41 Fe1 N11 . . 90.12(7) y
N41 Fe1 N21 . . 172.40(7) y
N41 Fe1 N31 . . 87.11(7) y
Fe1 N1 C1 . . 175.0(2) y
N1 C1 S1 . . 179.7(3) ?
Fe1 N2 C2 . . 163.2(2) y
N2 C2 S2 . . 178.6(2) ?
C11 N11 Fe1 . . 121.06(16) ?
C11 N11 C15 . . 117.6(2) ?
C15 N11 Fe1 . . 121.22(16) ?
N11 C11 H11 . . 118.6 ?
N11 C11 C12 . . 122.7(2) ?
C12 C11 H11 . . 118.6 ?
C11 C12 C16 . . 120.3(2) ?
C13 C12 C11 . . 119.2(2) ?
C13 C12 C16 . . 120.5(2) ?
C12 C13 H13 . . 120.9 ?
C14 C13 C12 . . 118.2(2) ?
C14 C13 H13 . . 120.9 ?
C13 C14 H14 . . 120.4 ?
C13 C14 C15 . . 119.1(2) ?
C15 C14 H14 . . 120.4 ?
N11 C15 C14 . . 123.1(2) ?
N11 C15 H15 . . 118.4 ?
C14 C15 H15 . . 118.4 ?
N12 C16 C12 . . 177.8(3) ?
C21 N21 Fe1 . . 121.22(16) ?
C21 N21 C25 . . 117.4(2) ?
C25 N21 Fe1 . . 121.28(17) ?
N21 C21 H21 . . 118.6 ?
N21 C21 C22 . . 122.7(2) ?
C22 C21 H21 . . 118.6 ?
C21 C22 C26 . . 119.5(2) ?
C23 C22 C21 . . 119.5(2) ?
C23 C22 C26 . . 121.0(2) ?
C22 C23 H23 . . 121.1 ?
C24 C23 C22 . . 117.7(2) ?
C24 C23 H23 . . 121.1 ?
C23 C24 H24 . . 120.3 ?
C23 C24 C25 . . 119.4(2) ?
C25 C24 H24 . . 120.3 ?
N21 C25 C24 . . 123.3(2) ?
N21 C25 H25 . . 118.4 ?
C24 C25 H25 . . 118.4 ?
N22 C26 C22 . . 177.9(3) ?
C31 N31 Fe1 . . 122.38(17) ?
C31 N31 C35 . . 118.0(2) ?
C35 N31 Fe1 . . 119.59(17) ?
N31 C31 H31 . . 118.8 ?
N31 C31 C32 . . 122.3(2) ?
C32 C31 H31 . . 118.8 ?
C31 C32 C33 . . 119.6(2) ?
C31 C32 C36 . . 119.4(3) ?
C33 C32 C36 . . 121.0(2) ?
C32 C33 H33 . . 121.0 ?
C34 C33 C32 . . 118.0(2) ?
C34 C33 H33 . . 121.0 ?
C33 C34 H34 . . 120.5 ?
C33 C34 C35 . . 119.1(3) ?
C35 C34 H34 . . 120.5 ?
N31 C35 C34 . . 122.9(3) ?
N31 C35 H35 . . 118.5 ?
C34 C35 H35 . . 118.5 ?
N32 C36 C32 . . 179.0(3) ?
C41 N41 Fe1 . . 123.72(16) ?
C41 N41 C45 . . 117.8(2) ?
C45 N41 Fe1 . . 118.22(16) ?
N41 C41 H41 . . 118.8 ?
N41 C41 C42 . . 122.3(2) ?
C42 C41 H41 . . 118.8 ?
C41 C42 C46 . . 119.7(2) ?
C43 C42 C41 . . 119.7(2) ?
C43 C42 C46 . . 120.5(2) ?
C42 C43 H43 . . 121.1 ?
C44 C43 C42 . . 117.8(2) ?
C44 C43 H43 . . 121.1 ?
C43 C44 H44 . . 120.4 ?
C45 C44 C43 . . 119.2(2) ?
C45 C44 H44 . . 120.4 ?
N41 C45 C44 . . 123.2(2) ?
N41 C45 H45 . . 118.4 ?
C44 C45 H45 . . 118.4 ?
N42 C46 C42 . . 179.7(3) ?
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 . 2.065(2) y
Fe1 N2 . 2.069(2) y
Fe1 N11 . 2.2660(19) y
Fe1 N21 . 2.273(2) y
Fe1 N31 . 2.257(2) y
Fe1 N41 . 2.2339(19) y
N1 C1 . 1.169(4) ?
C1 S1 . 1.622(3) ?
N2 C2 . 1.163(4) ?
C2 S2 . 1.622(3) ?
N11 C11 . 1.335(3) ?
N11 C15 . 1.347(3) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.399(3) ?
C12 C13 . 1.388(3) ?
C12 C16 . 1.439(3) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.385(4) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.388(3) ?
C15 H15 . 0.9500 ?
C16 N12 . 1.151(4) ?
N21 C21 . 1.338(3) ?
N21 C25 . 1.346(3) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.396(3) ?
C22 C23 . 1.395(3) ?
C22 C26 . 1.438(3) ?
C23 H23 . 0.9500 ?
C23 C24 . 1.380(4) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.389(4) ?
C25 H25 . 0.9500 ?
C26 N22 . 1.149(4) ?
N31 C31 . 1.341(3) ?
N31 C35 . 1.346(3) ?
C31 H31 . 0.9500 ?
C31 C32 . 1.391(4) ?
C32 C33 . 1.394(4) ?
C32 C36 . 1.444(4) ?
C33 H33 . 0.9500 ?
C33 C34 . 1.384(4) ?
C34 H34 . 0.9500 ?
C34 C35 . 1.392(4) ?
C35 H35 . 0.9500 ?
C36 N32 . 1.146(4) ?
N41 C41 . 1.338(3) ?
N41 C45 . 1.345(3) ?
C41 H41 . 0.9500 ?
C41 C42 . 1.395(4) ?
C42 C43 . 1.390(4) ?
C42 C46 . 1.447(4) ?
C43 H43 . 0.9500 ?
C43 C44 . 1.386(4) ?
C44 H44 . 0.9500 ?
C44 C45 . 1.385(4) ?
C45 H45 . 0.9500 ?
C46 N42 . 1.141(4) ?
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
C11 H11 N1 . 0.95 2.63 3.190(3) 118
C15 H15 N2 . 0.95 2.58 3.113(3) 115
C21 H21 N2 . 0.95 2.54 3.108(3) 118
C24 H24 N22 2_654 0.95 2.67 3.514(4) 148
C25 H25 N1 . 0.95 2.61 3.181(3) 119
C31 H31 N1 . 0.95 2.67 3.214(3) 117
C35 H35 N2 . 0.95 2.53 3.091(3) 118
C35 H35 N12 2_665 0.95 2.67 3.538(4) 151
C41 H41 N22 2_664 0.95 2.61 3.487(3) 154
C44 H44 S1 4_655 0.95 2.82 3.498(3) 129
C45 H45 N2 . 0.95 2.55 3.123(3) 119