#------------------------------------------------------------------------------
#$Date: 2022-10-29 13:15:10 +0100 (Sat, 29 Oct 2022) $
#$Revision: 278876 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244200.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_2244200
loop_
_publ_author_name
'Znovjyak, Kateryna'
'Fritsky, Igor O.'
'Sliva, Tatiana Y.'
'Amirkhanov, Vladimir M.'
'Malinkin, Sergey O.'
'Shova, Sergiu'
'Seredyuk, Maksym'
_publ_section_title
;
Crystal structure of
bis{3-(3-bromo-4-methoxyphenyl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-1,2,4-triazol-3-ato}iron(II)
methanol disolvate
;
_journal_coeditor_code DJ2053
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1138
_journal_page_last 1142
_journal_paper_doi 10.1107/S2056989022010179
_journal_volume 78
_journal_year 2022
_chemical_absolute_configuration ad
_chemical_formula_iupac '[Fe (C17 H12 Br N6 O)2] , 2C H4 O'
_chemical_formula_moiety 'C34 H24 Br2 Fe N12 O2, 2(C H4 O)'
_chemical_formula_sum 'C36 H32 Br2 Fe N12 O4'
_chemical_formula_weight 912.40
_chemical_name_systematic
'Bis{3-(3-bromo-4-methoxyphenyl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-1,2,4-triazol-3-ato}iron(II) methanol disolvate'
_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
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 27.4318(10)
_cell_length_b 12.6723(4)
_cell_length_c 10.6434(3)
_cell_measurement_reflns_used 3167
_cell_measurement_temperature 180.00(14)
_cell_measurement_theta_max 25.7430
_cell_measurement_theta_min 2.1820
_cell_volume 3699.9(2)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 180.00(14)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0612
_diffrn_reflns_av_unetI/netI 0.0967
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 14160
_diffrn_reflns_theta_full 25.027
_diffrn_reflns_theta_max 25.027
_diffrn_reflns_theta_min 1.770
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 2.626
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.77238
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'clear dark red'
_exptl_crystal_density_diffrn 1.638
_exptl_crystal_description plate
_exptl_crystal_F_000 1840
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.246
_refine_diff_density_min -0.620
_refine_ls_abs_structure_details
;
Flack x determined using 1444 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.009(8)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 502
_refine_ls_number_reflns 6227
_refine_ls_number_restraints 7
_refine_ls_restrained_S_all 1.027
_refine_ls_R_factor_all 0.0968
_refine_ls_R_factor_gt 0.0571
_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^)+(0.0468P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1057
_refine_ls_wR_factor_ref 0.1252
_reflns_number_gt 4361
_reflns_number_total 6227
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dj2053sup1.cif
_cod_data_source_block I
_cod_database_code 2244200
_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 0.506
_shelx_estimated_absorpt_t_max 0.902
_shelx_hkl_file
;
0 0 -4 985.54 26.35
0 0 -3 3.19 2.52
0 0 -2 1654.63 23.89
0 0 -1 1.57 0.83
0 0 1 0.49 0.75
0 0 2 1817.40 24.66
0 0 3 -0.05 2.03
0 0 4 1048.95 26.78
0 0 5 2.54 2.41
0 0 6 552.58 20.22
0 0 7 4.54 3.32
0 0 8 682.09 26.65
0 0 9 -0.96 3.61
0 0 10 110.06 12.59
0 0 11 5.93 4.54
0 0 12 92.50 14.05
0 0 13 16.84 7.59
0 0 14 98.84 16.13
0 -1 -7 25.13 6.92
0 -1 -6 -1.78 2.97
0 -1 -5 29.97 6.28
0 -1 -4 -3.68 2.76
0 -1 -3 152.23 9.39
0 -1 -3 170.27 4.26
0 1 -3 171.22 4.32
0 -1 -2 1.37 2.24
0 1 -2 0.14 0.69
0 -1 -2 0.37 0.73
0 -1 -2 1.35 1.31
0 1 -1 3.74 0.87
0 -1 -1 3.35 1.08
0 1 -1 3.65 1.13
0 -1 -1 3.80 0.94
0 1 0 0.53 0.41
0 -1 0 -0.06 0.36
0 1 1 2.34 0.81
0 -1 1 1.87 0.72
0 1 1 2.87 0.99
0 -1 1 1.71 0.72
0 1 2 0.71 0.80
0 1 2 -0.20 1.49
0 1 2 -0.78 1.31
0 -1 2 -0.72 0.71
0 1 3 156.23 9.55
0 1 3 200.74 8.67
0 1 3 182.10 4.40
0 -1 3 177.61 4.31
0 1 4 2.41 2.28
0 -1 4 2.27 2.66
0 1 4 -0.03 1.56
0 1 5 31.12 6.39
0 -1 5 27.51 5.48
0 1 5 25.64 4.17
0 1 6 -0.72 2.52
0 1 7 12.48 4.49
0 1 8 1.93 2.98
0 -1 8 2.23 3.24
0 -1 9 10.12 4.74
0 1 9 14.39 5.58
0 1 10 4.19 4.18
0 -1 10 6.56 4.57
0 1 11 23.85 7.15
0 -1 11 21.89 7.31
0 1 12 8.15 6.01
0 -1 12 5.76 6.26
0 1 13 22.68 8.96
0 -1 13 28.35 8.85
0 -1 14 -5.76 6.44
0 1 14 -4.43 5.35
0 -2 -9 0.47 4.54
0 -2 -8 139.61 15.09
0 -2 -7 -2.31 3.90
0 -2 -6 66.88 9.18
0 2 -6 74.87 3.43
0 -2 -5 -2.61 3.17
0 2 -5 -1.03 0.86
0 -2 -4 47.58 6.62
0 -2 -4 64.55 5.74
0 -2 -4 57.39 3.48
0 2 -4 54.51 3.50
0 -2 -3 2.51 3.34
0 2 -3 1.89 1.38
0 -2 -3 2.30 1.87
0 -2 -3 1.28 1.22
0 -2 -2 643.10 14.44
0 -2 -2 702.85 12.60
0 2 -2 667.87 12.43
0 2 -1 1.83 1.18
0 -2 -1 0.51 1.04
0 2 0 2.54 1.23
0 -2 0 1.05 1.24
0 2 1 -1.67 1.23
0 -2 1 0.63 1.28
0 -2 2 595.47 12.51
0 -2 2 667.95 12.36
0 2 2 677.54 12.31
0 2 3 -0.08 1.18
0 2 3 1.67 2.29
0 -2 3 -0.14 1.00
0 2 4 54.76 5.60
0 -2 4 59.08 3.53
0 2 4 59.69 3.58
0 2 5 0.40 0.81
0 2 5 3.48 2.87
0 2 6 86.95 3.79
0 2 6 103.14 9.15
0 2 7 5.59 3.76
0 2 8 183.26 14.18
0 2 9 1.67 3.58
0 2 10 9.37 4.86
0 -2 10 -3.52 4.01
0 2 11 6.78 4.82
0 -2 11 7.96 5.98
0 2 12 64.52 11.73
0 -2 12 50.15 10.45
0 2 13 4.88 5.22
0 -2 13 0.25 4.78
0 2 14 21.29 8.76
0 -3 -10 0.70 5.03
0 -3 -9 5.28 5.52
0 -3 -8 -4.09 4.41
0 3 -8 -0.87 0.73
0 -3 -7 31.45 6.99
0 3 -7 31.06 3.02
0 -3 -6 -0.89 3.46
0 3 -6 -0.23 1.06
0 -3 -5 93.74 10.10
0 -3 -5 95.04 7.94
0 3 -5 96.23 5.81
0 -3 -5 102.68 5.83
0 -3 -4 1.55 2.94
0 3 -4 0.38 1.19
0 -3 -4 -0.77 1.33
0 -3 -4 0.09 1.64
0 -3 -3 148.96 8.58
0 3 -3 154.18 7.50
0 -3 -3 170.32 7.81
0 3 -2 0.28 1.48
0 3 -2 0.85 1.23
0 -3 -2 2.14 1.65
0 -3 -1 195.37 8.39
0 3 -1 185.48 8.42
0 3 0 -1.40 1.37
0 -3 0 -1.19 1.71
0 -3 1 233.30 9.00
0 3 1 255.08 9.43
0 3 2 -0.53 1.31
0 -3 2 0.20 1.44
0 -3 3 165.99 7.81
0 -3 3 151.76 7.41
0 3 3 172.62 7.83
0 3 4 1.50 1.37
0 3 4 1.77 2.71
0 -3 4 1.78 1.82
0 -3 4 -0.39 1.46
0 -3 5 114.34 8.92
0 3 5 94.11 8.97
0 -3 5 103.47 5.78
0 3 5 94.56 5.70
0 3 6 -0.42 1.16
0 3 6 0.70 2.38
0 3 7 27.42 2.98
0 3 7 34.45 5.95
0 3 8 -0.96 0.91
0 3 8 2.83 4.61
0 3 9 -0.81 3.11
0 3 10 12.54 6.38
0 3 11 12.20 6.18
0 -3 11 6.59 4.95
0 3 12 21.38 8.22
0 -3 12 1.09 4.78
0 3 13 9.91 7.11
0 -3 13 10.51 6.35
0 3 14 16.85 7.88
0 -4 -11 -4.54 7.21
0 -4 -10 -2.96 4.82
0 -4 -9 -3.94 5.14
0 -4 -8 57.79 9.97
0 -4 -7 3.17 3.74
0 4 -7 -2.86 1.81
0 -4 -6 147.92 13.82
0 4 -6 152.06 8.16
0 -4 -6 156.82 8.16
0 -4 -5 2.03 3.15
0 4 -5 -0.28 1.49
0 -4 -5 0.08 1.85
0 -4 -5 -2.28 2.08
0 -4 -4 216.36 11.37
0 4 -4 218.78 10.10
0 -4 -4 226.32 10.08
0 4 -3 1.02 1.76
0 -4 -3 -1.84 2.14
0 4 -3 0.95 1.95
0 -4 -3 0.85 1.84
0 4 -2 72.04 5.34
0 -4 -2 77.89 6.03
0 4 -2 66.62 5.92
0 4 -1 -0.51 1.62
0 -4 -1 0.49 2.01
0 4 0 190.22 9.55
0 -4 0 193.16 9.38
0 4 1 1.26 1.59
0 -4 1 1.23 1.93
0 4 2 46.99 4.95
0 -4 2 47.20 4.75
0 4 3 -0.57 1.51
0 -4 3 0.74 1.65
0 -4 4 255.46 10.81
0 4 4 251.60 10.62
0 -4 4 237.19 10.30
0 4 5 0.72 1.47
0 -4 5 -1.37 1.60
0 -4 5 -1.10 1.87
0 4 6 129.07 11.94
0 -4 6 131.92 9.90
0 4 6 134.63 7.76
0 -4 6 137.27 7.57
0 4 7 -0.80 1.26
0 4 7 1.96 3.03
0 -4 7 1.52 2.45
0 4 8 68.92 5.10
0 -4 8 60.43 8.26
0 4 8 69.47 9.88
0 4 9 -0.77 3.77
0 -4 9 0.24 3.13
0 4 10 0.03 3.71
0 -4 10 12.30 5.84
0 4 11 -4.01 5.64
0 -4 11 -4.25 4.44
0 4 12 11.78 6.45
0 -4 12 21.76 8.23
0 4 13 -0.24 5.52
0 -4 13 0.15 6.04
0 4 14 9.87 7.15
0 -5 -12 -0.38 6.20
0 -5 -11 69.13 14.10
0 -5 -10 5.84 7.07
0 -5 -9 59.93 11.65
0 -5 -8 1.34 4.29
0 -5 -7 106.69 13.35
0 5 -7 110.53 7.94
0 5 -6 0.58 1.60
0 -5 -6 1.70 2.01
0 -5 -5 116.96 12.02
0 -5 -5 134.33 10.40
0 5 -5 117.23 8.43
0 -5 -5 124.88 8.40
0 5 -4 -2.01 2.11
0 -5 -4 0.68 1.73
0 -5 -4 -0.41 2.08
0 5 -3 146.58 8.93
0 5 -3 168.17 9.98
0 -5 -3 169.64 9.92
0 5 -2 -0.37 1.88
0 -5 -2 -1.40 2.53
0 5 -1 23.92 4.21
0 -5 -1 23.97 4.00
0 5 0 -3.11 2.67
0 -5 0 0.82 2.30
0 5 1 33.28 4.63
0 -5 1 37.45 5.06
0 5 2 -0.68 1.77
0 -5 2 -1.36 2.20
0 -5 3 139.76 9.41
0 5 3 151.76 9.42
0 5 4 -1.18 1.85
0 -5 4 1.23 1.79
0 5 5 119.75 8.19
0 -5 5 111.99 7.97
0 5 6 -0.13 1.49
0 -5 6 0.52 1.81
0 -5 6 0.79 1.81
0 5 7 117.11 8.13
0 -5 7 116.70 9.79
0 5 8 -1.31 2.15
0 -5 8 5.60 3.57
0 -5 9 71.49 9.05
0 -5 10 6.51 4.66
0 -5 11 75.36 10.81
0 -5 13 15.24 8.02
0 -6 -12 16.56 8.58
0 -6 -11 10.66 7.86
0 -6 -10 42.20 11.11
0 -6 -9 0.03 4.70
0 -6 -8 237.49 20.84
0 -6 -7 -2.61 3.84
0 6 -7 -2.10 2.37
0 -6 -7 0.97 2.15
0 -6 -6 253.79 19.06
0 6 -6 239.39 12.86
0 -6 -6 248.43 12.97
0 6 -5 -0.01 1.89
0 -6 -5 0.65 2.01
0 6 -4 332.25 15.36
0 -6 -4 367.35 18.25
0 6 -4 410.97 16.87
0 -6 -4 408.63 16.60
0 6 -3 -0.79 1.85
0 6 -3 2.56 2.02
0 -6 -3 1.05 2.08
0 6 -2 1265.78 29.67
0 -6 -2 1260.24 29.61
0 6 -1 1.69 2.31
0 -6 -1 0.64 2.51
0 -6 0 2920.92 45.14
0 6 0 2993.21 45.24
0 6 1 0.68 2.30
0 -6 1 -0.34 2.34
0 -6 2 1276.51 29.60
0 6 2 1301.37 29.84
0 6 3 0.09 2.41
0 -6 3 -1.24 2.78
0 -6 4 328.75 14.90
0 6 4 326.99 15.01
0 6 5 -1.43 1.95
0 -6 5 -3.93 2.96
0 6 6 286.15 13.83
0 -6 6 284.48 13.69
0 6 7 1.38 2.04
0 -6 7 -5.39 3.18
0 -6 8 243.44 14.71
0 -6 9 -2.83 2.81
0 -6 10 62.88 8.60
0 -7 -11 17.76 8.70
0 -7 -10 5.31 5.78
0 -7 -9 21.99 7.91
0 -7 -8 3.47 5.98
0 -7 -7 180.21 18.20
0 -7 -7 192.22 12.60
0 -7 -6 -2.72 3.25
0 -7 -5 169.50 11.71
0 7 -4 0.32 2.05
0 -7 -4 -1.30 2.83
0 7 -3 328.08 14.68
0 -7 -3 338.25 16.61
0 -7 -2 -0.76 2.77
0 -7 -1 415.76 18.55
0 -7 0 1.07 3.43
0 -7 1 378.95 17.73
0 -7 2 -4.37 3.24
0 -7 3 273.72 15.31
0 -7 4 1.52 2.73
0 -7 5 176.79 11.98
0 -7 6 0.50 2.71
0 -7 7 172.05 11.80
0 -8 -11 -5.36 6.12
0 -8 -10 14.86 7.91
0 -8 -9 -4.23 6.02
0 -8 -8 166.50 18.85
0 -8 -7 6.45 6.36
0 -8 -7 0.97 3.31
0 -8 -6 118.05 10.59
0 -8 -5 -1.19 2.97
0 8 -4 130.25 10.55
0 -8 -4 149.13 11.82
0 8 -3 1.59 2.54
0 -8 -3 -2.94 3.39
0 -8 -2 112.28 10.37
0 -8 -1 -5.38 3.62
0 -8 0 2.15 2.85
0 -8 1 1.21 2.80
0 -8 2 108.90 10.16
0 -8 3 -3.93 3.46
0 -8 4 152.30 11.86
0 -8 5 -1.63 3.56
0 -8 6 133.61 11.08
0 -8 7 -3.73 3.42
0 -9 -10 5.74 7.77
0 -9 -9 43.48 11.54
0 -9 -8 0.80 5.70
0 -9 -7 17.11 7.26
0 -9 -7 6.00 3.45
0 -9 -6 2.45 2.66
0 -9 -5 95.14 10.16
0 -9 -4 -0.61 3.29
0 -9 -3 184.34 14.23
0 -9 -2 -3.45 3.80
0 -9 -1 129.55 11.63
0 -9 0 2.63 3.28
0 -9 1 152.92 12.97
0 -9 2 -0.10 2.92
0 -9 3 153.71 12.75
0 -9 4 -2.18 3.38
0 -9 5 74.19 9.35
0 -9 6 -0.16 2.86
0 -9 7 3.08 2.99
0 -10 -10 16.12 9.67
0 -10 -9 5.53 6.93
0 -10 -8 21.43 8.77
0 -10 -7 0.85 3.10
0 -10 -6 39.62 8.05
0 -10 -5 -5.60 3.82
0 -10 -4 6.25 4.19
0 -10 -3 -5.71 4.06
0 -10 -2 9.89 4.81
0 -10 -1 -2.70 4.28
0 -10 0 46.52 7.39
0 -10 1 -4.90 4.11
0 -10 2 9.22 4.42
0 -10 3 -2.47 3.42
0 -10 4 3.09 3.60
0 -10 5 -0.51 3.58
0 -10 6 31.69 6.38
0 -10 7 -2.69 3.78
0 -11 -9 24.32 8.89
0 -11 -8 7.54 8.57
0 -11 -7 37.95 7.66
0 -11 -6 0.64 4.25
0 -11 -5 21.34 5.91
0 -11 -4 -7.14 5.59
0 -11 -3 76.57 10.25
0 -11 -2 -3.43 4.65
0 -11 -1 38.59 7.62
0 -11 0 1.49 4.82
0 -11 1 41.13 7.75
0 -11 2 -4.58 4.06
0 -11 3 68.99 10.01
0 -11 4 -2.67 4.47
0 -11 5 18.30 6.06
0 -11 6 -6.87 5.07
0 -11 7 50.13 8.92
0 -12 -8 2.10 5.94
0 -12 -7 -0.29 4.06
0 -12 -6 -4.38 5.22
0 -12 -5 -5.55 5.47
0 -12 -4 10.45 4.84
0 -12 -3 -6.39 5.47
0 -12 -2 4.77 4.35
0 -12 -1 -0.29 5.03
0 -12 0 16.84 5.63
0 -12 1 -0.71 3.96
0 -12 2 2.25 4.02
0 -12 3 -0.78 4.91
0 -12 4 10.66 5.39
0 -12 5 -1.59 4.37
0 -12 6 -5.73 3.96
0 -12 7 2.38 3.71
0 -13 -7 110.84 13.92
0 -13 -6 -0.06 5.13
0 -13 -5 144.01 15.89
0 -13 -4 -5.43 5.12
0 -13 -3 225.43 19.33
0 -13 -2 0.20 4.67
0 -13 -1 283.69 21.69
0 -13 0 0.49 4.48
0 -13 1 283.28 21.60
0 -13 2 -2.96 5.43
0 -13 3 231.85 19.60
0 -13 4 6.23 5.66
0 -13 5 137.03 15.42
0 -13 6 -6.27 4.42
0 -13 7 127.50 15.28
0 -14 -6 23.26 7.89
0 -14 -5 -0.40 5.25
0 -14 -4 15.77 6.77
0 -14 -3 -5.03 5.16
0 -14 -2 12.17 6.23
0 -14 -1 3.91 4.79
0 -14 0 5.44 6.79
0 -14 1 -4.45 5.03
0 -14 2 8.61 6.00
0 -14 3 -5.50 5.39
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9 -11 8 6.56 5.73
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9 -12 -8 16.98 9.46
9 -12 -8 13.51 7.10
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9 -12 -6 5.66 5.40
9 -12 -5 18.64 6.90
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9 -12 -3 17.28 6.35
9 -12 -2 2.41 3.80
9 -12 -1 31.23 8.05
9 -12 0 -6.67 4.85
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9 -12 5 3.89 4.04
9 -12 6 3.39 4.38
9 -12 7 11.65 6.68
9 -12 8 13.66 6.30
9 -13 -7 6.44 4.94
9 -13 -6 7.74 5.99
9 -13 -5 9.12 5.33
9 -13 -4 -10.01 6.58
9 -13 -3 14.20 6.51
9 -13 -2 19.49 7.44
9 -13 -1 9.43 5.28
9 -13 0 4.52 4.84
9 -13 1 15.89 6.62
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9 -13 4 -0.25 4.37
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9 -14 -7 -3.14 5.00
9 -14 -6 7.28 5.81
9 -14 -5 8.97 7.40
9 -14 -4 12.64 6.70
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9 -14 -2 -0.53 5.10
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10 0 2 266.40 9.50
-10 0 2 256.90 9.28
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10 0 5 0.51 1.84
-10 0 5 0.24 3.33
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-10 0 8 47.39 8.98
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10 -1 -7 9.61 2.54
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10 -1 -6 157.37 9.21
10 -1 -5 53.11 5.72
10 -1 -5 52.41 6.95
-10 -1 -5 42.92 6.56
10 -1 -4 778.24 20.46
-10 -1 -4 810.36 23.71
10 -1 -4 803.59 23.49
10 -1 -3 202.51 10.91
10 -1 -3 171.30 11.24
-10 -1 -3 189.71 10.08
10 -1 -3 191.28 10.13
10 -1 -2 168.64 9.75
10 -1 -2 179.82 10.70
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-10 -1 5 42.12 6.63
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31 3 7 10.96 7.96
31 -3 8 0.06 5.15
31 3 8 4.89 6.67
31 -4 -7 -4.60 6.46
31 4 -7 0.28 4.85
31 -4 -6 11.59 7.47
31 -4 -5 11.27 6.92
31 -4 -4 2.70 7.09
31 -4 -3 3.44 6.23
31 -4 -2 4.98 5.75
31 -4 -1 8.62 6.48
31 -4 0 21.20 8.06
31 -4 1 1.13 5.77
31 -4 2 10.80 7.98
31 4 2 5.30 4.24
31 -4 3 15.83 7.33
31 4 3 3.90 5.74
31 -4 4 7.08 7.55
31 4 4 1.24 4.67
31 -4 5 -1.10 5.32
31 4 5 -0.69 6.41
31 -4 6 11.21 7.49
31 4 6 -10.39 7.28
31 -4 7 -9.60 6.56
-31 -4 7 -10.53 8.52
31 4 7 3.52 5.95
31 -5 -6 5.33 5.28
31 -5 -5 13.96 6.35
31 -5 -4 -2.44 7.99
31 -5 -3 29.72 9.99
31 -5 -2 -15.06 7.68
31 -5 -1 1.80 5.40
31 -5 0 0.01 5.33
31 -5 1 9.97 6.85
31 -5 2 12.31 7.53
31 5 2 -1.43 4.59
31 -5 3 31.39 9.71
31 5 3 44.83 10.17
31 -5 4 4.64 6.11
31 5 4 -10.09 7.38
31 -5 5 10.50 6.37
31 5 5 14.29 7.47
31 -5 6 8.45 6.58
31 5 6 10.26 7.74
31 -6 -4 -3.77 5.83
31 -6 -3 3.45 6.25
31 -6 -2 -0.69 5.23
31 -6 -1 -11.07 7.02
31 -6 0 0.01 5.29
31 -6 1 -2.81 6.12
31 -6 2 -7.57 6.70
31 -6 3 4.09 6.28
31 6 3 -1.98 5.10
31 -6 4 1.01 6.45
31 6 4 -4.18 5.03
31 6 5 6.65 6.15
31 7 4 -5.08 6.06
31 7 5 11.40 7.26
32 0 -7 -9.64 5.74
32 0 -6 5.84 7.47
32 0 -5 -1.81 5.61
32 0 -4 4.07 4.60
32 0 -3 0.18 6.08
32 0 -2 20.72 8.13
32 0 -1 6.20 5.34
32 0 0 6.31 5.85
32 0 1 5.34 5.98
32 0 2 19.36 6.69
32 0 3 23.65 8.60
32 0 3 3.20 5.11
32 0 4 14.66 7.62
32 0 4 4.94 7.23
32 0 5 7.12 6.90
32 0 5 9.24 7.11
32 0 6 0.41 4.73
32 0 7 -5.28 6.35
32 -1 -7 6.94 6.75
32 1 -7 10.05 7.17
32 1 -6 4.18 5.90
32 -1 -6 -17.46 7.74
32 1 -5 11.01 6.97
32 -1 -5 2.79 5.79
32 1 -4 -7.69 6.39
32 -1 -4 3.84 5.58
32 -1 -3 11.08 6.55
32 1 -3 17.71 7.73
32 -1 -2 -3.61 6.11
32 1 -2 7.79 6.74
32 -1 -1 -8.42 6.35
32 1 -1 -0.12 5.41
32 -1 0 11.47 6.54
32 1 0 -9.40 6.22
32 -1 1 17.81 7.65
32 1 1 2.37 5.25
32 -1 2 -0.63 6.00
32 1 2 4.25 5.91
32 1 3 2.61 4.82
32 -1 3 11.07 7.57
32 1 3 2.67 5.52
32 -1 4 7.24 6.83
32 1 4 6.88 6.42
32 1 4 -2.84 4.91
32 -1 4 1.91 4.76
32 -1 5 5.60 6.41
32 1 5 13.35 7.32
32 1 5 1.54 6.99
32 -1 5 -8.39 6.16
32 1 6 -0.92 5.83
32 -1 6 -2.34 5.09
32 -1 7 -0.93 5.80
32 1 7 14.78 6.92
32 -2 -7 5.23 5.99
32 2 -7 1.58 5.48
32 -2 -6 13.35 7.52
32 2 -6 23.96 9.10
32 -2 -5 6.24 6.60
32 2 -5 -4.39 5.54
32 -2 -4 0.28 5.67
32 2 -4 19.07 8.52
32 2 -3 -5.09 5.61
32 -2 -3 7.54 5.18
32 2 -2 25.24 8.92
32 -2 -2 31.96 9.88
32 2 -1 7.39 5.09
32 -2 -1 -3.22 5.30
32 2 0 -7.60 4.84
32 -2 0 -0.59 4.81
32 2 1 -4.87 5.56
32 -2 1 7.86 6.66
32 2 2 47.05 9.95
32 2 2 38.78 10.54
32 -2 2 40.55 11.03
32 2 3 1.40 4.93
32 2 3 0.94 4.86
32 -2 3 14.83 7.07
32 -2 4 14.56 7.39
32 2 4 16.40 7.45
32 2 4 15.73 7.98
32 -2 5 1.38 4.86
32 2 5 8.53 5.90
32 2 5 8.01 6.17
32 -2 6 25.51 9.19
32 2 6 10.64 7.50
32 -2 7 8.88 5.86
32 2 7 0.68 4.73
32 -3 -7 0.03 5.74
32 3 -7 -6.73 6.94
32 -3 -6 6.33 5.40
32 3 -6 0.70 5.13
32 -3 -5 1.77 5.57
32 3 -5 4.60 5.86
32 -3 -4 15.11 8.77
32 3 -4 5.10 5.60
32 -3 -3 14.77 9.01
32 -3 -2 3.97 6.64
32 -3 -1 4.17 5.94
32 -3 0 17.46 7.60
32 -3 1 -3.69 5.62
32 3 1 3.31 5.76
32 -3 2 8.92 6.17
32 3 2 8.70 5.78
32 -3 3 8.04 6.01
32 3 3 -6.29 5.27
32 -3 4 5.52 6.35
32 3 4 5.29 4.91
32 3 4 7.77 6.95
32 -3 5 0.33 5.01
32 3 5 -6.45 5.62
32 3 5 -11.71 6.93
32 -3 6 1.56 4.99
32 3 6 2.34 5.95
32 -4 -6 10.58 7.04
32 -4 -5 3.86 5.60
32 -4 -4 20.88 8.73
32 -4 -3 13.37 8.07
32 -4 -2 56.39 12.84
32 -4 -1 28.30 8.98
32 -4 0 22.24 8.42
32 -4 1 35.93 10.70
32 -4 2 46.09 11.17
32 4 2 51.13 10.60
32 -4 3 14.05 8.34
32 4 3 13.99 6.76
32 -4 4 14.09 8.51
32 4 4 30.27 9.28
32 -4 5 5.39 6.15
32 4 5 3.55 6.98
32 -5 -4 11.00 8.27
32 -5 -3 11.12 6.74
32 -5 -2 7.15 7.34
32 -5 -1 2.75 5.79
32 -5 0 6.31 6.39
32 -5 1 2.09 6.13
32 -5 2 15.87 8.90
32 -5 3 10.01 7.38
32 5 3 1.13 4.38
32 5 4 2.35 5.84
32 5 5 -16.68 8.00
32 6 4 12.81 6.79
32 6 5 -17.87 8.40
32 7 5 17.76 8.85
33 0 -6 0.52 4.86
33 0 -5 -7.78 6.16
33 0 -4 2.12 5.44
33 0 -3 -0.82 6.18
33 0 -2 9.33 6.82
33 0 -1 -8.41 6.29
33 0 0 4.88 6.83
33 0 1 1.53 5.06
33 0 2 7.76 6.69
33 0 3 -10.71 5.99
33 0 4 4.47 5.49
33 0 4 -11.86 6.92
33 0 5 0.32 5.69
33 0 5 9.00 7.01
33 -1 -6 12.58 8.06
33 1 -6 1.20 5.87
33 1 -5 -2.56 6.42
33 -1 -5 6.41 6.56
33 1 -4 -1.57 5.12
33 -1 -4 10.73 7.10
33 1 -3 19.32 7.79
33 -1 -3 24.25 9.41
33 -1 -2 1.59 4.97
33 1 -2 -1.68 5.05
33 -1 -1 -0.56 4.84
33 1 -1 6.25 6.68
33 -1 0 0.37 4.98
33 1 0 -2.84 5.43
33 -1 1 1.23 5.70
33 1 1 6.74 6.84
33 -1 2 15.04 8.09
33 1 2 -7.19 6.40
33 1 3 30.29 9.50
33 1 3 11.84 7.61
33 -1 3 19.50 8.28
33 1 4 12.04 6.68
33 1 4 2.62 5.06
33 -1 4 16.08 7.97
33 -1 5 28.52 10.33
33 1 5 9.94 8.38
33 1 5 11.72 6.93
33 -1 5 1.67 4.98
33 -2 -5 4.87 6.53
33 2 -5 4.09 6.67
33 -2 -4 9.90 7.05
33 2 -4 5.77 5.86
33 2 -3 2.25 5.57
33 -2 -3 0.44 4.99
33 2 -2 -0.86 5.03
33 -2 -2 2.24 5.14
33 2 -1 12.76 7.07
33 -2 -1 4.41 5.78
33 2 0 1.21 6.50
33 -2 0 3.18 5.19
33 2 1 3.06 5.00
33 -2 1 8.13 5.97
33 2 2 5.99 6.83
33 2 2 8.35 6.43
33 -2 2 13.27 6.96
33 2 3 5.21 5.75
33 2 3 -11.76 6.89
33 -2 3 4.42 6.34
33 -2 4 12.10 7.38
33 2 4 10.67 6.56
33 2 4 5.71 6.55
33 2 5 12.88 7.15
33 -3 -4 8.18 6.95
33 3 -4 7.49 6.81
33 -3 -3 49.78 11.68
33 3 -3 24.13 8.38
33 -3 -2 -0.30 5.20
33 3 -2 -12.41 7.16
33 -3 -1 63.91 12.35
33 -3 0 4.18 6.12
33 -3 1 55.95 12.81
33 -3 2 1.18 5.86
33 3 2 1.89 4.45
33 3 2 -1.42 5.41
33 -3 3 34.16 10.69
33 3 3 33.77 10.16
33 3 3 39.49 11.20
33 -3 4 -2.86 5.56
33 3 4 4.78 5.82
33 3 4 15.47 8.08
33 3 5 19.85 8.41
33 -4 -2 9.03 7.36
33 -4 -1 6.96 6.41
33 -4 0 21.35 8.40
33 -4 1 9.20 7.55
33 -4 2 18.90 8.40
33 4 3 5.47 5.45
33 4 4 1.77 5.39
33 4 5 1.05 5.41
33 5 4 -4.78 5.70
33 5 5 22.00 9.55
34 0 -3 -5.22 6.34
34 0 -2 6.91 5.97
34 0 -1 -5.10 6.43
34 0 0 4.75 5.96
34 0 1 0.44 5.15
34 0 2 19.08 8.51
34 0 4 14.94 8.69
34 1 -3 4.80 6.58
34 -1 -3 0.08 5.95
34 1 -2 1.36 6.92
34 -1 -2 -0.22 4.96
34 -1 -1 8.01 7.12
34 1 -1 -3.95 6.48
34 -1 0 7.83 7.03
34 1 0 5.71 6.55
34 -1 1 -0.17 5.29
34 1 1 5.52 6.92
34 1 2 -0.61 6.58
34 -1 2 4.26 6.41
34 1 3 21.27 8.32
34 1 4 1.08 4.90
34 2 -1 5.48 6.13
34 -2 -1 5.48 5.46
34 2 0 13.28 7.86
34 -2 0 -14.59 7.21
34 2 1 14.24 6.79
34 -2 1 14.53 8.20
34 2 3 4.22 7.08
34 2 4 33.87 10.96
34 3 3 4.25 5.14
34 3 4 -1.87 5.17
34 4 3 2.77 4.85
34 4 4 11.87 6.76
35 1 4 9.47 7.36
35 2 3 11.46 7.35
35 2 4 3.98 6.19
35 3 3 7.32 6.87
35 3 4 -12.92 7.09
35 4 4 6.34 6.33
0 0 0 0.00 0.00
TITL shI_5690_SS_autored in Pna2(1)
REM Pna2(1) (#33, found as P2(1)cn in -cba setting)
CELL 0.71073 27.431774 12.672252 10.643360 90.0000 90.0000 90.0000
ZERR 8.00 0.001000 0.000360 0.000344 0.0000 0.0000 0.0000
LATT -1
SYMM -x,-y, z+1/2
SYMM x+1/2,-y+1/2, z
SYMM -x+1/2, y+1/2, z+1/2
SFAC C H N O Fe Br
UNIT 136.00 96.00 48.00 8.00 8.00 8.00
REM CrysAlisPro recorded range (K): Min=179.9; max=180.0; aver:179.9
TEMP -93
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 63675
_shelx_res_file
;
TITL shi_5690_ss_autored_a.res in Pna2(1)
shi_5690_ss_autored.res
created by SHELXL-2018/3 at 13:11:34 on 18-Sep-2022
REM Old TITL shI_5690_SS_autored in Pna21 #33
REM SHELXT solution in Pna2(1): R1 0.187, Rweak 0.050, Alpha 0.057
REM 0.620 for 150 systematic absences, Orientation as input
REM Flack x = 0.100 ( 0.021 ) from 477 Parsons' quotients
REM Formula found by SHELXT: C36 N9 O4 Fe2 Br
CELL 0.71073 27.431774 12.672252 10.64336 90 90 90
ZERR 4 0.001 0.00036 0.000344 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 Br Fe N O
UNIT 144 128 8 4 48 16
ISOR 0.01 0.02 C17
L.S. 10
PLAN 4
SIZE 0.04 0.26 0.3
TEMP -93.15(14)
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
SHEL 999 0.84
OMIT 1 2 1
REM
REM
REM
WGHT 0.046800
FVAR 0.15437
BR1 3 0.939473 0.181788 0.187379 11.00000 0.09816 0.02782 =
0.10066 -0.00299 0.05828 0.01587
BR2 3 0.581171 0.864232 0.165751 11.00000 0.06592 0.02986 =
0.06402 0.01704 -0.02283 0.00334
FE1 4 0.748802 0.513569 0.664877 11.00000 0.02029 0.01126 =
0.01791 0.00057 -0.00046 -0.00092
O1 6 0.984987 0.351189 0.034405 11.00000 0.04787 0.04081 =
0.05007 -0.00978 0.03016 0.00128
O2 6 0.503347 0.717506 0.084469 11.00000 0.04783 0.05035 =
0.07739 0.02962 -0.04353 -0.00984
N1 5 0.792548 0.464153 0.798585 11.00000 0.02323 0.01609 =
0.02318 0.00135 0.00275 -0.00830
N2 5 0.785394 0.361567 0.830956 11.00000 0.02754 0.01089 =
0.01870 0.00734 0.00706 -0.00122
N3 5 0.733073 0.366275 0.668835 11.00000 0.02667 0.01057 =
0.01350 0.00436 0.00771 -0.00291
N4 5 0.698031 0.508955 0.535750 11.00000 0.02803 0.01457 =
0.01334 -0.00075 0.00030 0.00115
N5 5 0.673492 0.577670 0.459118 11.00000 0.02076 0.01041 =
0.03065 0.00883 -0.00083 -0.00457
N6 5 0.642401 0.414420 0.429038 11.00000 0.02509 0.01478 =
0.02166 0.00040 -0.00364 -0.00166
N7 5 0.703031 0.559934 0.795613 11.00000 0.02389 0.00985 =
0.01999 0.00438 0.00802 -0.00212
N8 5 0.709529 0.663707 0.829737 11.00000 0.03006 0.00901 =
0.02191 -0.00693 0.00067 0.00178
N9 5 0.763861 0.660462 0.673265 11.00000 0.02562 0.00874 =
0.01262 -0.00195 -0.00815 -0.00085
N10 5 0.801462 0.520794 0.537626 11.00000 0.01542 0.01635 =
0.01833 0.00152 -0.00397 -0.00035
N11 5 0.825179 0.453758 0.458084 11.00000 0.02733 0.01400 =
0.01741 -0.01017 0.00468 -0.00483
N12 5 0.856075 0.619655 0.435346 11.00000 0.02401 0.01037 =
0.02569 -0.00292 0.00438 -0.00357
C1 1 0.823249 0.502013 0.883822 11.00000 0.01927 0.01301 =
0.03411 -0.00184 -0.00337 -0.00319
AFIX 43
H1 2 0.836027 0.571689 0.884392 11.00000 -1.20000
AFIX 0
C2 1 0.834196 0.422538 0.974405 11.00000 0.03276 0.02201 =
0.02526 0.00069 -0.00576 0.00774
AFIX 43
H2 2 0.854203 0.429649 1.046766 11.00000 -1.20000
AFIX 0
C3 1 0.810288 0.335136 0.936204 11.00000 0.02858 0.01779 =
0.02010 0.00506 -0.00506 0.01090
AFIX 43
H3 2 0.810827 0.267895 0.975646 11.00000 -1.20000
AFIX 0
C4 1 0.753414 0.303049 0.752889 11.00000 0.02534 0.01850 =
0.01506 0.00065 -0.00408 -0.00069
C5 1 0.744352 0.196992 0.760361 11.00000 0.02732 0.01274 =
0.02048 0.00705 0.00274 0.00324
AFIX 43
H5 2 0.760428 0.153348 0.819944 11.00000 -1.20000
AFIX 0
C6 1 0.710352 0.156423 0.676101 11.00000 0.03403 0.01954 =
0.02559 0.00070 0.00657 -0.00537
AFIX 43
H6 2 0.703580 0.082904 0.675727 11.00000 -1.20000
AFIX 0
C7 1 0.686484 0.221900 0.593391 11.00000 0.02821 0.02422 =
0.01778 -0.00487 -0.00453 -0.00014
AFIX 43
H7 2 0.662303 0.194369 0.538543 11.00000 -1.20000
AFIX 0
C8 1 0.697940 0.327798 0.590741 11.00000 0.01766 0.01342 =
0.02172 -0.00582 0.00414 -0.00270
C9 1 0.678991 0.412783 0.515387 11.00000 0.02141 0.01646 =
0.00950 0.00026 -0.00219 0.00084
C10 1 0.640678 0.518103 0.398454 11.00000 0.02549 0.01763 =
0.01786 0.00340 -0.00174 0.00078
C11 1 0.606050 0.565826 0.311696 11.00000 0.02212 0.02083 =
0.02120 0.00330 -0.00167 -0.00505
C12 1 0.568815 0.508707 0.256298 11.00000 0.03936 0.02335 =
0.06407 0.01484 -0.00666 -0.00663
AFIX 43
H12 2 0.566690 0.435012 0.271727 11.00000 -1.20000
AFIX 0
C13 1 0.533885 0.556867 0.177470 11.00000 0.03920 0.04187 =
0.06648 0.01168 -0.03288 -0.01366
AFIX 43
H13 2 0.508661 0.515389 0.141389 11.00000 -1.20000
AFIX 0
C14 1 0.536033 0.663152 0.152461 11.00000 0.02609 0.04078 =
0.03506 0.02120 -0.00854 -0.00195
C15 1 0.573728 0.720301 0.203691 11.00000 0.02640 0.03114 =
0.02811 0.01341 -0.00211 0.00071
C16 1 0.608023 0.672809 0.282401 11.00000 0.02573 0.02079 =
0.03071 -0.00135 -0.00696 -0.00287
AFIX 43
H16 2 0.633427 0.714686 0.316951 11.00000 -1.20000
AFIX 0
C17 1 0.459657 0.660998 0.043725 11.00000 0.06918 0.08127 =
0.10496 0.03239 -0.06525 -0.02657
AFIX 137
H17A 2 0.436960 0.710675 0.004257 11.00000 -1.50000
H17B 2 0.443970 0.628133 0.116611 11.00000 -1.50000
H17C 2 0.468752 0.606305 -0.017004 11.00000 -1.50000
AFIX 0
C18 1 0.669935 0.521811 0.875377 11.00000 0.03110 0.01773 =
0.03245 0.00438 0.00145 0.00008
AFIX 43
H18 2 0.656975 0.452322 0.872907 11.00000 -1.20000
AFIX 0
C19 1 0.656810 0.600718 0.965086 11.00000 0.03872 0.02764 =
0.01706 0.00000 0.00853 0.00606
AFIX 43
H19 2 0.634576 0.593789 1.033020 11.00000 -1.20000
AFIX 0
C20 1 0.682876 0.687843 0.932665 11.00000 0.02720 0.01896 =
0.01903 0.00301 0.00702 0.00924
AFIX 43
H20 2 0.682436 0.753910 0.974832 11.00000 -1.20000
AFIX 0
C21 1 0.742583 0.722675 0.757578 11.00000 0.02210 0.01498 =
0.01878 0.00274 -0.00566 -0.00502
C22 1 0.751008 0.829167 0.766976 11.00000 0.02632 0.02283 =
0.02251 -0.00526 -0.00461 0.00124
AFIX 43
H22 2 0.734218 0.871698 0.826391 11.00000 -1.20000
AFIX 0
C23 1 0.785503 0.871942 0.684827 11.00000 0.04583 0.00900 =
0.02834 -0.00243 -0.00074 -0.00196
AFIX 43
H23 2 0.792262 0.945451 0.686681 11.00000 -1.20000
AFIX 0
C25 1 0.809790 0.807423 0.600905 11.00000 0.03021 0.01849 =
0.02260 0.00480 0.00101 -0.00681
AFIX 43
H25 2 0.833605 0.836305 0.545977 11.00000 -1.20000
AFIX 0
C26 1 0.799331 0.700667 0.597095 11.00000 0.01283 0.01375 =
0.01981 0.00231 -0.00235 -0.00168
C27 1 0.820143 0.616722 0.520745 11.00000 0.02078 0.02100 =
0.00994 -0.00067 0.00316 -0.00678
C28 1 0.857161 0.516775 0.399288 11.00000 0.01634 0.02533 =
0.02343 0.00224 -0.00041 0.00160
C29 1 0.890822 0.475630 0.303375 11.00000 0.01759 0.02464 =
0.01973 -0.00364 0.00020 0.00540
C30 1 0.914148 0.543365 0.219299 11.00000 0.02970 0.02959 =
0.02559 -0.01077 0.00410 -0.00781
AFIX 43
H30 2 0.908122 0.617120 0.223076 11.00000 -1.20000
AFIX 0
C31 1 0.946379 0.503037 0.129458 11.00000 0.02003 0.03774 =
0.02841 -0.00090 0.00317 -0.00720
AFIX 43
H31 2 0.962898 0.550064 0.074511 11.00000 -1.20000
AFIX 0
C32 1 0.954430 0.396933 0.119647 11.00000 0.03288 0.04054 =
0.02833 -0.00495 0.00095 0.00996
C33 1 0.930883 0.328697 0.202342 11.00000 0.05018 0.02805 =
0.03265 -0.00754 0.00439 0.00749
C34 1 0.899347 0.367617 0.292807 11.00000 0.02525 0.03128 =
0.03197 -0.00149 0.01230 -0.00443
AFIX 43
H34 2 0.883359 0.320139 0.348246 11.00000 -1.20000
AFIX 0
C35 1 1.008929 0.417029 -0.055623 11.00000 0.07232 0.05677 =
0.05647 -0.00538 0.03823 -0.00690
AFIX 137
H35A 2 1.026381 0.372877 -0.116380 11.00000 -1.50000
H35B 2 1.032148 0.463288 -0.012460 11.00000 -1.50000
H35C 2 0.984662 0.460036 -0.099718 11.00000 -1.50000
AFIX 0
O3 6 0.894562 0.813174 0.350116 11.00000 0.06712 0.02322 =
0.07016 0.01252 0.00869 -0.00899
AFIX 147
H3A 2 0.889770 0.749515 0.368323 11.00000 -1.50000
AFIX 0
C36 1 0.935455 0.849501 0.413374 11.00000 0.05840 0.06538 =
0.17857 0.02472 -0.01548 -0.02286
AFIX 137
H36A 2 0.964669 0.816116 0.378324 11.00000 -1.50000
H36B 2 0.932720 0.831820 0.502734 11.00000 -1.50000
H36C 2 0.937869 0.926235 0.403763 11.00000 -1.50000
AFIX 0
O4 6 0.617282 0.209218 0.339148 11.00000 0.04427 0.02139 =
0.05330 -0.01246 -0.01785 0.00267
AFIX 147
H4 2 0.620155 0.274742 0.348513 11.00000 -1.50000
AFIX 0
C24 1 0.579619 0.188484 0.256176 11.00000 0.06018 0.04705 =
0.05613 -0.02163 -0.01889 0.01201
AFIX 137
H24A 2 0.581928 0.115298 0.227028 11.00000 -1.50000
H24B 2 0.581953 0.236323 0.184082 11.00000 -1.50000
H24C 2 0.548314 0.199154 0.298680 11.00000 -1.50000
AFIX 0
HKLF 4
REM shi_5690_ss_autored_a.res in Pna2(1)
REM wR2 = 0.1252, GooF = S = 1.026, Restrained GooF = 1.027 for all data
REM R1 = 0.0571 for 4361 Fo > 4sig(Fo) and 0.0968 for all 6227 data
REM 502 parameters refined using 7 restraints
END
WGHT 0.0467 0.0000
REM Highest difference peak 1.246, deepest hole -0.620, 1-sigma level 0.095
Q1 1 0.5510 0.8204 0.1823 11.00000 0.05 1.25
Q2 1 0.9502 0.1853 0.2103 11.00000 0.05 0.50
Q3 1 0.9084 0.1403 0.1636 11.00000 0.05 0.48
Q4 1 0.5317 0.5980 -0.0933 11.00000 0.05 0.41
;
_shelx_res_checksum 86007
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
Br Br1 0.93947(6) 0.18179(10) 0.18738(16) 0.0755(6) Uani d 1 . .
Br Br2 0.58117(5) 0.86423(9) 0.16575(14) 0.0533(4) Uani d 1 . .
Fe Fe1 0.74880(4) 0.51357(9) 0.66488(14) 0.0165(3) Uani d 1 . .
O O1 0.9850(3) 0.3512(6) 0.0344(7) 0.046(2) Uani d 1 . .
O O2 0.5033(3) 0.7175(7) 0.0845(8) 0.059(3) Uani d 1 . .
N N1 0.7925(3) 0.4642(7) 0.7986(7) 0.021(2) Uani d 1 . .
N N2 0.7854(3) 0.3616(6) 0.8310(6) 0.0190(19) Uani d 1 . .
N N3 0.7331(2) 0.3663(5) 0.6688(8) 0.0169(16) Uani d 1 . .
N N4 0.6980(3) 0.5090(7) 0.5358(7) 0.019(2) Uani d 1 . .
N N5 0.6735(3) 0.5777(6) 0.4591(7) 0.021(2) Uani d 1 . .
N N6 0.6424(3) 0.4144(6) 0.4290(7) 0.021(2) Uani d 1 . .
N N7 0.7030(3) 0.5599(6) 0.7956(7) 0.0179(19) Uani d 1 . .
N N8 0.7095(3) 0.6637(6) 0.8297(7) 0.0203(19) Uani d 1 . .
N N9 0.7639(2) 0.6605(5) 0.6733(7) 0.0157(16) Uani d 1 . .
N N10 0.8015(3) 0.5208(7) 0.5376(7) 0.0167(19) Uani d 1 . .
N N11 0.8252(3) 0.4538(7) 0.4581(7) 0.020(2) Uani d 1 . .
N N12 0.8561(3) 0.6197(6) 0.4353(7) 0.020(2) Uani d 1 . .
C C1 0.8232(4) 0.5020(9) 0.8838(9) 0.022(3) Uani d 1 . .
H H1 0.836027 0.571689 0.884392 0.027 Uiso calc 1 . .
C C2 0.8342(4) 0.4225(8) 0.9744(9) 0.027(3) Uani d 1 . .
H H2 0.854203 0.429649 1.046766 0.032 Uiso calc 1 . .
C C3 0.8103(3) 0.3351(8) 0.9362(9) 0.022(2) Uani d 1 . .
H H3 0.810827 0.267895 0.975646 0.027 Uiso calc 1 . .
C C4 0.7534(3) 0.3030(8) 0.7529(8) 0.020(2) Uani d 1 . .
C C5 0.7444(3) 0.1970(8) 0.7604(8) 0.020(2) Uani d 1 . .
H H5 0.760428 0.153348 0.819944 0.024 Uiso calc 1 . .
C C6 0.7104(3) 0.1564(7) 0.6761(9) 0.026(2) Uani d 1 . .
H H6 0.703580 0.082904 0.675727 0.032 Uiso calc 1 . .
C C7 0.6865(3) 0.2219(8) 0.5934(8) 0.023(2) Uani d 1 . .
H H7 0.662303 0.194369 0.538543 0.028 Uiso calc 1 . .
C C8 0.6979(3) 0.3278(8) 0.5907(8) 0.018(2) Uani d 1 . .
C C9 0.6790(3) 0.4128(8) 0.5154(7) 0.016(2) Uani d 1 . .
C C10 0.6407(4) 0.5181(8) 0.3985(8) 0.020(2) Uani d 1 . .
C C11 0.6061(3) 0.5658(8) 0.3117(8) 0.021(2) Uani d 1 . .
C C12 0.5688(4) 0.5087(9) 0.2563(10) 0.042(3) Uani d 1 . .
H H12 0.566690 0.435012 0.271727 0.051 Uiso calc 1 . .
C C13 0.5339(4) 0.5569(9) 0.1775(13) 0.049(3) Uani d 1 . .
H H13 0.508661 0.515389 0.141389 0.059 Uiso calc 1 . .
C C14 0.5360(4) 0.6632(9) 0.1525(11) 0.034(3) Uani d 1 . .
C C15 0.5737(3) 0.7203(9) 0.2037(9) 0.029(3) Uani d 1 . .
C C16 0.6080(4) 0.6728(8) 0.2824(9) 0.026(3) Uani d 1 . .
H H16 0.633427 0.714686 0.316951 0.031 Uiso calc 1 . .
C C17 0.4597(5) 0.6610(12) 0.0437(14) 0.085(6) Uani d 1 . .
H H17A 0.436960 0.710675 0.004257 0.128 Uiso calc 1 . .
H H17B 0.443970 0.628133 0.116611 0.128 Uiso calc 1 . .
H H17C 0.468752 0.606305 -0.017004 0.128 Uiso calc 1 . .
C C18 0.6699(4) 0.5218(9) 0.8754(9) 0.027(3) Uani d 1 . .
H H18 0.656975 0.452322 0.872907 0.033 Uiso calc 1 . .
C C19 0.6568(4) 0.6007(9) 0.9651(9) 0.028(3) Uani d 1 . .
H H19 0.634576 0.593789 1.033020 0.033 Uiso calc 1 . .
C C20 0.6829(4) 0.6878(8) 0.9327(9) 0.022(2) Uani d 1 . .
H H20 0.682436 0.753910 0.974832 0.026 Uiso calc 1 . .
C C21 0.7426(3) 0.7227(8) 0.7576(8) 0.019(2) Uani d 1 . .
C C22 0.7510(4) 0.8292(8) 0.7670(9) 0.024(2) Uani d 1 . .
H H22 0.734218 0.871698 0.826391 0.029 Uiso calc 1 . .
C C23 0.7855(3) 0.8719(7) 0.6848(9) 0.028(2) Uani d 1 . .
H H23 0.792262 0.945451 0.686681 0.033 Uiso calc 1 . .
C C25 0.8098(4) 0.8074(8) 0.6009(9) 0.024(2) Uani d 1 . .
H H25 0.833605 0.836305 0.545977 0.029 Uiso calc 1 . .
C C26 0.7993(3) 0.7007(8) 0.5971(8) 0.015(2) Uani d 1 . .
C C27 0.8201(3) 0.6167(8) 0.5207(8) 0.017(2) Uani d 1 . .
C C28 0.8572(3) 0.5168(9) 0.3993(8) 0.022(2) Uani d 1 . .
C C29 0.8908(3) 0.4756(8) 0.3034(9) 0.021(2) Uani d 1 . .
C C30 0.9141(4) 0.5434(9) 0.2193(8) 0.028(3) Uani d 1 . .
H H30 0.908122 0.617120 0.223076 0.034 Uiso calc 1 . .
C C31 0.9464(4) 0.5030(10) 0.1295(9) 0.029(3) Uani d 1 . .
H H31 0.962898 0.550064 0.074511 0.034 Uiso calc 1 . .
C C32 0.9544(4) 0.3969(10) 0.1196(9) 0.034(3) Uani d 1 . .
C C33 0.9309(4) 0.3287(9) 0.2023(10) 0.037(3) Uani d 1 . .
C C34 0.8993(4) 0.3676(9) 0.2928(9) 0.029(3) Uani d 1 . .
H H34 0.883359 0.320139 0.348246 0.035 Uiso calc 1 . .
C C35 1.0089(5) 0.4170(10) -0.0556(11) 0.062(4) Uani d 1 . .
H H35A 1.026381 0.372877 -0.116380 0.093 Uiso calc 1 . .
H H35B 1.032148 0.463288 -0.012460 0.093 Uiso calc 1 . .
H H35C 0.984662 0.460036 -0.099718 0.093 Uiso calc 1 . .
O O3 0.8946(3) 0.8132(7) 0.3501(8) 0.054(2) Uani d 1 . .
H H3A 0.889770 0.749515 0.368323 0.080 Uiso calc 1 . .
C C36 0.9355(6) 0.8495(13) 0.4134(18) 0.101(6) Uani d 1 . .
H H36A 0.964669 0.816116 0.378324 0.151 Uiso calc 1 . .
H H36B 0.932720 0.831820 0.502734 0.151 Uiso calc 1 . .
H H36C 0.937869 0.926235 0.403763 0.151 Uiso calc 1 . .
O O4 0.6173(3) 0.2092(6) 0.3391(7) 0.040(2) Uani d 1 . .
H H4 0.620155 0.274742 0.348513 0.059 Uiso calc 1 . .
C C24 0.5796(4) 0.1885(10) 0.2562(11) 0.054(4) Uani d 1 . .
H H24A 0.581928 0.115298 0.227028 0.082 Uiso calc 1 . .
H H24B 0.581953 0.236323 0.184082 0.082 Uiso calc 1 . .
H H24C 0.548314 0.199154 0.298680 0.082 Uiso calc 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
Br1 0.0982(11) 0.0278(8) 0.1007(13) 0.0159(8) 0.0583(11) -0.0030(9)
Br2 0.0659(8) 0.0299(7) 0.0640(8) 0.0033(6) -0.0228(9) 0.0170(8)
Fe1 0.0203(6) 0.0113(7) 0.0179(6) -0.0009(6) -0.0005(7) 0.0006(8)
O1 0.048(5) 0.041(6) 0.050(5) 0.001(4) 0.030(4) -0.010(4)
O2 0.048(5) 0.050(6) 0.077(6) -0.010(5) -0.044(4) 0.030(5)
N1 0.023(5) 0.016(5) 0.023(5) -0.008(4) 0.003(4) 0.001(4)
N2 0.028(5) 0.011(5) 0.019(4) -0.001(4) 0.007(3) 0.007(4)
N3 0.027(4) 0.011(4) 0.013(4) -0.003(3) 0.008(4) 0.004(4)
N4 0.028(5) 0.015(5) 0.013(4) 0.001(4) 0.000(3) -0.001(4)
N5 0.021(5) 0.010(5) 0.031(5) -0.005(4) -0.001(4) 0.009(4)
N6 0.025(5) 0.015(5) 0.022(5) -0.002(4) -0.004(4) 0.000(4)
N7 0.024(5) 0.010(5) 0.020(4) -0.002(4) 0.008(4) 0.004(4)
N8 0.030(5) 0.009(5) 0.022(5) 0.002(4) 0.001(4) -0.007(4)
N9 0.026(4) 0.009(4) 0.013(4) -0.001(3) -0.008(4) -0.002(4)
N10 0.015(4) 0.016(5) 0.018(4) 0.000(4) -0.004(3) 0.002(4)
N11 0.027(5) 0.014(5) 0.017(5) -0.005(4) 0.005(4) -0.010(4)
N12 0.024(5) 0.010(5) 0.026(5) -0.004(4) 0.004(4) -0.003(4)
C1 0.019(6) 0.013(6) 0.034(6) -0.003(5) -0.003(5) -0.002(5)
C2 0.033(6) 0.022(7) 0.025(6) 0.008(6) -0.006(5) 0.001(5)
C3 0.029(6) 0.018(6) 0.020(5) 0.011(5) -0.005(4) 0.005(4)
C4 0.025(6) 0.018(6) 0.015(5) -0.001(5) -0.004(4) 0.001(4)
C5 0.027(6) 0.013(6) 0.020(5) 0.003(5) 0.003(4) 0.007(4)
C6 0.034(5) 0.020(5) 0.026(6) -0.005(5) 0.007(6) 0.001(6)
C7 0.028(6) 0.024(7) 0.018(5) 0.000(5) -0.005(4) -0.005(5)
C8 0.018(5) 0.013(6) 0.022(5) -0.003(5) 0.004(4) -0.006(4)
C9 0.021(6) 0.016(6) 0.009(5) 0.001(5) -0.002(4) 0.000(4)
C10 0.025(6) 0.018(7) 0.018(5) 0.001(5) -0.002(4) 0.003(4)
C11 0.022(6) 0.021(6) 0.021(5) -0.005(5) -0.002(4) 0.003(5)
C12 0.039(8) 0.023(7) 0.064(8) -0.007(6) -0.007(6) 0.015(6)
C13 0.039(6) 0.042(8) 0.066(8) -0.014(6) -0.033(7) 0.012(8)
C14 0.026(5) 0.041(7) 0.035(6) -0.002(5) -0.009(5) 0.021(6)
C15 0.026(6) 0.031(7) 0.028(6) 0.001(5) -0.002(5) 0.013(5)
C16 0.026(6) 0.021(6) 0.031(6) -0.003(5) -0.007(5) -0.001(5)
C17 0.069(10) 0.081(12) 0.105(11) -0.027(9) -0.065(9) 0.032(9)
C18 0.031(7) 0.018(7) 0.032(6) 0.000(6) 0.001(5) 0.004(5)
C19 0.039(7) 0.028(7) 0.017(5) 0.006(6) 0.009(5) 0.000(5)
C20 0.027(6) 0.019(6) 0.019(5) 0.009(5) 0.007(4) 0.003(5)
C21 0.022(6) 0.015(6) 0.019(5) -0.005(5) -0.006(4) 0.003(4)
C22 0.026(6) 0.023(6) 0.023(5) 0.001(5) -0.005(4) -0.005(5)
C23 0.046(6) 0.009(5) 0.028(6) -0.002(5) -0.001(6) -0.002(5)
C25 0.030(6) 0.018(6) 0.023(5) -0.007(5) 0.001(4) 0.005(5)
C26 0.013(5) 0.014(6) 0.020(5) -0.002(5) -0.002(4) 0.002(4)
C27 0.021(5) 0.021(6) 0.010(5) -0.007(5) 0.003(4) -0.001(4)
C28 0.016(5) 0.025(7) 0.023(6) 0.002(5) 0.000(4) 0.002(5)
C29 0.018(5) 0.025(7) 0.020(5) 0.005(5) 0.000(4) -0.004(5)
C30 0.030(6) 0.030(7) 0.026(5) -0.008(6) 0.004(5) -0.011(5)
C31 0.020(6) 0.038(8) 0.028(6) -0.007(6) 0.003(4) -0.001(5)
C32 0.033(7) 0.041(8) 0.028(6) 0.010(6) 0.001(5) -0.005(5)
C33 0.050(7) 0.028(7) 0.033(7) 0.007(6) 0.004(6) -0.008(5)
C34 0.025(6) 0.031(7) 0.032(6) -0.004(6) 0.012(5) -0.001(5)
C35 0.072(10) 0.057(11) 0.056(8) -0.007(9) 0.038(8) -0.005(8)
O3 0.067(6) 0.023(5) 0.070(6) -0.009(5) 0.009(5) 0.013(4)
C36 0.058(11) 0.065(13) 0.179(18) -0.023(10) -0.015(12) 0.025(12)
O4 0.044(5) 0.021(5) 0.053(5) 0.003(4) -0.018(4) -0.012(4)
C24 0.060(9) 0.047(10) 0.056(9) 0.012(8) -0.019(7) -0.022(7)
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'
Br Br -0.2901 2.4595 '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'
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_
_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 N7 . . 88.4(3) ?
N1 Fe1 N10 . . 93.7(3) ?
N3 Fe1 N1 . . 79.1(3) ?
N3 Fe1 N4 . . 80.0(3) ?
N3 Fe1 N7 . . 97.6(3) ?
N3 Fe1 N10 . . 102.9(3) ?
N4 Fe1 N1 . . 159.1(4) ?
N4 Fe1 N7 . . 93.0(3) ?
N4 Fe1 N10 . . 92.3(3) ?
N7 Fe1 N10 . . 159.4(3) ?
N9 Fe1 N1 . . 98.3(3) ?
N9 Fe1 N3 . . 176.0(4) ?
N9 Fe1 N4 . . 102.5(3) ?
N9 Fe1 N7 . . 79.3(3) ?
N9 Fe1 N10 . . 80.2(3) ?
C32 O1 C35 . . 118.7(10) ?
C14 O2 C17 . . 117.1(10) ?
N2 N1 Fe1 . . 113.6(6) ?
C1 N1 Fe1 . . 140.1(8) ?
C1 N1 N2 . . 105.3(8) ?
N1 N2 C4 . . 116.2(7) ?
C3 N2 N1 . . 111.9(8) ?
C3 N2 C4 . . 131.9(8) ?
C4 N3 Fe1 . . 120.6(6) ?
C4 N3 C8 . . 119.6(8) ?
C8 N3 Fe1 . . 119.6(6) ?
N5 N4 Fe1 . . 138.5(7) ?
C9 N4 Fe1 . . 114.6(6) ?
C9 N4 N5 . . 106.8(8) ?
C10 N5 N4 . . 105.0(8) ?
C10 N6 C9 . . 101.7(8) ?
N8 N7 Fe1 . . 113.0(6) ?
C18 N7 Fe1 . . 141.1(7) ?
C18 N7 N8 . . 105.5(8) ?
N7 N8 C21 . . 116.6(7) ?
C20 N8 N7 . . 111.1(8) ?
C20 N8 C21 . . 132.2(8) ?
C21 N9 Fe1 . . 121.0(6) ?
C21 N9 C26 . . 119.5(8) ?
C26 N9 Fe1 . . 119.4(6) ?
N11 N10 Fe1 . . 138.0(7) ?
C27 N10 Fe1 . . 114.5(6) ?
C27 N10 N11 . . 107.5(8) ?
C28 N11 N10 . . 103.3(8) ?
C27 N12 C28 . . 100.4(8) ?
N1 C1 H1 . . 125.1 ?
N1 C1 C2 . . 109.9(10) ?
C2 C1 H1 . . 125.1 ?
C1 C2 H2 . . 127.1 ?
C3 C2 C1 . . 105.9(9) ?
C3 C2 H2 . . 127.1 ?
N2 C3 H3 . . 126.5 ?
C2 C3 N2 . . 106.9(9) ?
C2 C3 H3 . . 126.5 ?
N3 C4 N2 . . 109.9(8) ?
N3 C4 C5 . . 123.8(8) ?
C5 C4 N2 . . 126.3(8) ?
C4 C5 H5 . . 121.7 ?
C4 C5 C6 . . 116.5(9) ?
C6 C5 H5 . . 121.7 ?
C5 C6 H6 . . 119.7 ?
C7 C6 C5 . . 120.6(9) ?
C7 C6 H6 . . 119.7 ?
C6 C7 H7 . . 120.3 ?
C6 C7 C8 . . 119.5(9) ?
C8 C7 H7 . . 120.3 ?
N3 C8 C7 . . 119.8(9) ?
N3 C8 C9 . . 109.1(8) ?
C7 C8 C9 . . 131.1(9) ?
N4 C9 N6 . . 112.4(8) ?
N4 C9 C8 . . 116.6(8) ?
N6 C9 C8 . . 130.8(9) ?
N5 C10 N6 . . 114.0(9) ?
N5 C10 C11 . . 120.6(9) ?
N6 C10 C11 . . 125.3(9) ?
C12 C11 C10 . . 122.3(10) ?
C12 C11 C16 . . 116.3(9) ?
C16 C11 C10 . . 121.4(9) ?
C11 C12 H12 . . 119.1 ?
C11 C12 C13 . . 121.9(10) ?
C13 C12 H12 . . 119.1 ?
C12 C13 H13 . . 119.7 ?
C14 C13 C12 . . 120.6(10) ?
C14 C13 H13 . . 119.7 ?
O2 C14 C13 . . 125.4(10) ?
O2 C14 C15 . . 116.5(10) ?
C13 C14 C15 . . 118.1(10) ?
C14 C15 Br2 . . 120.5(7) ?
C14 C15 C16 . . 121.2(10) ?
C16 C15 Br2 . . 118.3(8) ?
C11 C16 C15 . . 121.9(9) ?
C11 C16 H16 . . 119.1 ?
C15 C16 H16 . . 119.1 ?
O2 C17 H17A . . 109.5 ?
O2 C17 H17B . . 109.5 ?
O2 C17 H17C . . 109.5 ?
H17A C17 H17B . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
N7 C18 H18 . . 125.0 ?
N7 C18 C19 . . 110.1(10) ?
C19 C18 H18 . . 125.0 ?
C18 C19 H19 . . 127.3 ?
C20 C19 C18 . . 105.4(9) ?
C20 C19 H19 . . 127.3 ?
N8 C20 C19 . . 107.8(9) ?
N8 C20 H20 . . 126.1 ?
C19 C20 H20 . . 126.1 ?
N9 C21 N8 . . 109.7(8) ?
N9 C21 C22 . . 123.9(9) ?
C22 C21 N8 . . 126.3(9) ?
C21 C22 H22 . . 121.6 ?
C21 C22 C23 . . 116.7(9) ?
C23 C22 H22 . . 121.6 ?
C22 C23 H23 . . 120.0 ?
C25 C23 C22 . . 120.1(9) ?
C25 C23 H23 . . 120.0 ?
C23 C25 H25 . . 120.1 ?
C23 C25 C26 . . 119.8(9) ?
C26 C25 H25 . . 120.1 ?
N9 C26 C25 . . 119.7(8) ?
N9 C26 C27 . . 109.8(8) ?
C25 C26 C27 . . 130.5(9) ?
N10 C27 N12 . . 113.6(9) ?
N10 C27 C26 . . 116.2(8) ?
N12 C27 C26 . . 130.3(9) ?
N11 C28 N12 . . 115.1(9) ?
N11 C28 C29 . . 121.5(10) ?
N12 C28 C29 . . 123.3(9) ?
C30 C29 C28 . . 121.0(10) ?
C34 C29 C28 . . 120.6(9) ?
C34 C29 C30 . . 118.4(9) ?
C29 C30 H30 . . 119.9 ?
C29 C30 C31 . . 120.2(11) ?
C31 C30 H30 . . 119.9 ?
C30 C31 H31 . . 119.5 ?
C32 C31 C30 . . 120.9(10) ?
C32 C31 H31 . . 119.5 ?
O1 C32 C31 . . 124.6(10) ?
O1 C32 C33 . . 116.2(11) ?
C31 C32 C33 . . 119.2(10) ?
C32 C33 Br1 . . 120.2(8) ?
C34 C33 Br1 . . 119.3(9) ?
C34 C33 C32 . . 120.5(11) ?
C29 C34 H34 . . 119.6 ?
C33 C34 C29 . . 120.7(10) ?
C33 C34 H34 . . 119.6 ?
O1 C35 H35A . . 109.5 ?
O1 C35 H35B . . 109.5 ?
O1 C35 H35C . . 109.5 ?
H35A C35 H35B . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
C36 O3 H3A . . 109.5 ?
O3 C36 H36A . . 109.5 ?
O3 C36 H36B . . 109.5 ?
O3 C36 H36C . . 109.5 ?
H36A C36 H36B . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C24 O4 H4 . . 109.5 ?
O4 C24 H24A . . 109.5 ?
O4 C24 H24B . . 109.5 ?
O4 C24 H24C . . 109.5 ?
H24A C24 H24B . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
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
Br1 C33 . 1.883(11) ?
Br2 C15 . 1.879(11) ?
Fe1 N1 . 1.964(8) ?
Fe1 N3 . 1.916(7) ?
Fe1 N4 . 1.958(8) ?
Fe1 N7 . 1.964(8) ?
Fe1 N9 . 1.909(6) ?
Fe1 N10 . 1.982(8) ?
O1 C32 . 1.364(12) ?
O1 C35 . 1.430(13) ?
O2 C14 . 1.342(11) ?
O2 C17 . 1.462(14) ?
N1 N2 . 1.359(10) ?
N1 C1 . 1.328(12) ?
N2 C3 . 1.354(11) ?
N2 C4 . 1.418(12) ?
N3 C4 . 1.324(11) ?
N3 C8 . 1.363(11) ?
N4 N5 . 1.370(11) ?
N4 C9 . 1.344(12) ?
N5 C10 . 1.340(12) ?
N6 C9 . 1.361(11) ?
N6 C10 . 1.354(12) ?
N7 N8 . 1.376(10) ?
N7 C18 . 1.334(12) ?
N8 C20 . 1.352(11) ?
N8 C21 . 1.404(11) ?
N9 C21 . 1.329(11) ?
N9 C26 . 1.365(11) ?
N10 N11 . 1.364(11) ?
N10 C27 . 1.331(12) ?
N11 C28 . 1.341(12) ?
N12 C27 . 1.341(11) ?
N12 C28 . 1.359(12) ?
C1 H1 . 0.9500 ?
C1 C2 . 1.426(13) ?
C2 H2 . 0.9500 ?
C2 C3 . 1.350(14) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.369(12) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.392(13) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.376(13) ?
C7 H7 . 0.9500 ?
C7 C8 . 1.379(13) ?
C8 C9 . 1.440(13) ?
C10 C11 . 1.456(13) ?
C11 C12 . 1.384(14) ?
C11 C16 . 1.392(13) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.412(14) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.374(14) ?
C14 C15 . 1.375(13) ?
C15 C16 . 1.396(13) ?
C16 H16 . 0.9500 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
C18 H18 . 0.9500 ?
C18 C19 . 1.429(14) ?
C19 H19 . 0.9500 ?
C19 C20 . 1.360(14) ?
C20 H20 . 0.9500 ?
C21 C22 . 1.373(13) ?
C22 H22 . 0.9500 ?
C22 C23 . 1.398(13) ?
C23 H23 . 0.9500 ?
C23 C25 . 1.382(13) ?
C25 H25 . 0.9500 ?
C25 C26 . 1.384(13) ?
C26 C27 . 1.455(13) ?
C28 C29 . 1.472(13) ?
C29 C30 . 1.395(14) ?
C29 C34 . 1.393(13) ?
C30 H30 . 0.9500 ?
C30 C31 . 1.399(12) ?
C31 H31 . 0.9500 ?
C31 C32 . 1.367(15) ?
C32 C33 . 1.393(15) ?
C33 C34 . 1.385(14) ?
C34 H34 . 0.9500 ?
C35 H35A . 0.9800 ?
C35 H35B . 0.9800 ?
C35 H35C . 0.9800 ?
O3 H3A . 0.8400 ?
O3 C36 . 1.387(16) ?
C36 H36A . 0.9800 ?
C36 H36B . 0.9800 ?
C36 H36C . 0.9800 ?
O4 H4 . 0.8400 ?
O4 C24 . 1.384(12) ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
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
C17 . N6 2_664 . . 3.201(16) .
O3 H3A N12 . 0.84 2.02 2.820(12) 160
O4 H4 N6 . 0.84 2.06 2.855(11) 158
C1 H1 O4 4_655 0.95 2.22 3.128(14) 161
C18 H18 O3 4_645 0.95 2.27 3.192(14) 163
C35 H35A C30 2_764 0.98 2.62 3.233(16) 121
C3 H3 N5 4_645 0.95 2.45 3.301(13) 148
C7 H7 O4 . 0.95 2.46 3.310(11) 148
C22 H22 N11 4_655 0.95 2.39 3.317(13) 166
C20 H20 N11 4_655 0.95 2.55 3.389(13) 148
C5 H5 N5 4_645 0.95 2.53 3.440(12) 161
C17 H17A O4 2_664 0.98 2.52 3.451(17) 159
C34 H34 C20 4_644 0.95 2.63 3.535(15) 159
C25 H25 O3 . 0.95 2.69 3.542(13) 150
C18 H18 C36 4_645 0.95 2.88 3.65(2) 138
C2 H2 C31 1_556 0.95 2.84 3.639(15) 143
C2 H2 C32 1_556 0.95 2.89 3.656(15) 139
C2 H2 C30 1_556 0.95 2.86 3.734(11) 154
C2 H2 Cg2 1_556 0.95 2.57 3.501(11) 168
C19 H19 Cg1 1_556 0.95 2.74 3.681(11) 169
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
Br1 C33 C34 C29 . . . . -177.7(8) ?
Br2 C15 C16 C11 . . . . -177.8(7) ?
Fe1 N1 N2 C3 . . . . -169.9(6) ?
Fe1 N1 N2 C4 . . . . 8.8(10) ?
Fe1 N1 C1 C2 . . . . 165.1(8) ?
Fe1 N3 C4 N2 . . . . 0.4(10) ?
Fe1 N3 C4 C5 . . . . -179.2(7) ?
Fe1 N3 C8 C7 . . . . -179.9(7) ?
Fe1 N3 C8 C9 . . . . 0.5(10) ?
Fe1 N4 N5 C10 . . . . -176.2(7) ?
Fe1 N4 C9 N6 . . . . 177.2(6) ?
Fe1 N4 C9 C8 . . . . 0.5(10) ?
Fe1 N7 N8 C20 . . . . -170.3(6) ?
Fe1 N7 N8 C21 . . . . 7.5(9) ?
Fe1 N7 C18 C19 . . . . 167.7(8) ?
Fe1 N9 C21 N8 . . . . -1.0(10) ?
Fe1 N9 C21 C22 . . . . -178.6(7) ?
Fe1 N9 C26 C25 . . . . 178.7(7) ?
Fe1 N9 C26 C27 . . . . -0.7(10) ?
Fe1 N10 N11 C28 . . . . 180.0(7) ?
Fe1 N10 C27 N12 . . . . 179.3(6) ?
Fe1 N10 C27 C26 . . . . -0.1(10) ?
O1 C32 C33 Br1 . . . . -3.1(13) ?
O1 C32 C33 C34 . . . . 179.6(10) ?
O2 C14 C15 Br2 . . . . -5.6(14) ?
O2 C14 C15 C16 . . . . 176.0(10) ?
N1 N2 C3 C2 . . . . 0.3(11) ?
N1 N2 C4 N3 . . . . -6.1(11) ?
N1 N2 C4 C5 . . . . 173.6(9) ?
N1 C1 C2 C3 . . . . 2.4(12) ?
N2 N1 C1 C2 . . . . -2.2(11) ?
N2 C4 C5 C6 . . . . 178.2(8) ?
N3 C4 C5 C6 . . . . -2.2(14) ?
N3 C8 C9 N4 . . . . -0.6(11) ?
N3 C8 C9 N6 . . . . -176.7(8) ?
N4 N5 C10 N6 . . . . -0.7(11) ?
N4 N5 C10 C11 . . . . 177.2(8) ?
N5 N4 C9 N6 . . . . -0.5(10) ?
N5 N4 C9 C8 . . . . -177.3(8) ?
N5 C10 C11 C12 . . . . -173.9(9) ?
N5 C10 C11 C16 . . . . 4.5(15) ?
N6 C10 C11 C12 . . . . 3.9(15) ?
N6 C10 C11 C16 . . . . -177.7(9) ?
N7 N8 C20 C19 . . . . -2.3(11) ?
N7 N8 C21 N9 . . . . -4.4(11) ?
N7 N8 C21 C22 . . . . 173.2(9) ?
N7 C18 C19 C20 . . . . 1.4(12) ?
N8 N7 C18 C19 . . . . -2.7(11) ?
N8 C21 C22 C23 . . . . -179.6(8) ?
N9 C21 C22 C23 . . . . -2.4(14) ?
N9 C26 C27 N10 . . . . 0.4(11) ?
N9 C26 C27 N12 . . . . -178.8(9) ?
N10 N11 C28 N12 . . . . 0.3(11) ?
N10 N11 C28 C29 . . . . -180.0(8) ?
N11 N10 C27 N12 . . . . -1.0(10) ?
N11 N10 C27 C26 . . . . 179.6(8) ?
N11 C28 C29 C30 . . . . 162.3(9) ?
N11 C28 C29 C34 . . . . -16.3(14) ?
N12 C28 C29 C30 . . . . -18.0(15) ?
N12 C28 C29 C34 . . . . 163.4(9) ?
C1 N1 N2 C3 . . . . 1.2(10) ?
C1 N1 N2 C4 . . . . 180.0(8) ?
C1 C2 C3 N2 . . . . -1.6(11) ?
C3 N2 C4 N3 . . . . 172.4(9) ?
C3 N2 C4 C5 . . . . -8.0(16) ?
C4 N2 C3 C2 . . . . -178.2(9) ?
C4 N3 C8 C7 . . . . -4.9(13) ?
C4 N3 C8 C9 . . . . 175.6(8) ?
C4 C5 C6 C7 . . . . -2.0(13) ?
C5 C6 C7 C8 . . . . 2.7(14) ?
C6 C7 C8 N3 . . . . 0.7(14) ?
C6 C7 C8 C9 . . . . -179.8(9) ?
C7 C8 C9 N4 . . . . 179.9(9) ?
C7 C8 C9 N6 . . . . 3.8(17) ?
C8 N3 C4 N2 . . . . -174.6(7) ?
C8 N3 C4 C5 . . . . 5.7(14) ?
C9 N4 N5 C10 . . . . 0.7(10) ?
C9 N6 C10 N5 . . . . 0.4(11) ?
C9 N6 C10 C11 . . . . -177.5(9) ?
C10 N6 C9 N4 . . . . 0.1(10) ?
C10 N6 C9 C8 . . . . 176.3(10) ?
C10 C11 C12 C13 . . . . 176.6(10) ?
C10 C11 C16 C15 . . . . -177.1(9) ?
C11 C12 C13 C14 . . . . 0.4(19) ?
C12 C11 C16 C15 . . . . 1.3(15) ?
C12 C13 C14 O2 . . . . -176.3(11) ?
C12 C13 C14 C15 . . . . 1.6(19) ?
C13 C14 C15 Br2 . . . . 176.3(9) ?
C13 C14 C15 C16 . . . . -2.1(17) ?
C14 C15 C16 C11 . . . . 0.6(16) ?
C16 C11 C12 C13 . . . . -1.9(16) ?
C17 O2 C14 C13 . . . . 6.0(19) ?
C17 O2 C14 C15 . . . . -171.9(11) ?
C18 N7 N8 C20 . . . . 3.1(10) ?
C18 N7 N8 C21 . . . . -179.0(8) ?
C18 C19 C20 N8 . . . . 0.6(12) ?
C20 N8 C21 N9 . . . . 172.9(9) ?
C20 N8 C21 C22 . . . . -9.5(16) ?
C21 N8 C20 C19 . . . . -179.8(9) ?
C21 N9 C26 C25 . . . . -5.5(12) ?
C21 N9 C26 C27 . . . . 175.1(8) ?
C21 C22 C23 C25 . . . . -1.0(14) ?
C22 C23 C25 C26 . . . . 1.0(14) ?
C23 C25 C26 N9 . . . . 2.3(13) ?
C23 C25 C26 C27 . . . . -178.5(9) ?
C25 C26 C27 N10 . . . . -178.9(9) ?
C25 C26 C27 N12 . . . . 1.9(17) ?
C26 N9 C21 N8 . . . . -176.6(7) ?
C26 N9 C21 C22 . . . . 5.7(14) ?
C27 N10 N11 C28 . . . . 0.4(10) ?
C27 N12 C28 N11 . . . . -0.9(11) ?
C27 N12 C28 C29 . . . . 179.4(8) ?
C28 N12 C27 N10 . . . . 1.1(10) ?
C28 N12 C27 C26 . . . . -179.6(9) ?
C28 C29 C30 C31 . . . . 179.4(8) ?
C28 C29 C34 C33 . . . . 179.8(9) ?
C29 C30 C31 C32 . . . . 2.1(15) ?
C30 C29 C34 C33 . . . . 1.1(15) ?
C30 C31 C32 O1 . . . . 179.6(9) ?
C30 C31 C32 C33 . . . . -1.4(15) ?
C31 C32 C33 Br1 . . . . 177.8(8) ?
C31 C32 C33 C34 . . . . 0.6(16) ?
C32 C33 C34 C29 . . . . -0.4(16) ?
C34 C29 C30 C31 . . . . -1.9(14) ?
C35 O1 C32 C31 . . . . -3.0(16) ?
C35 O1 C32 C33 . . . . 178.0(10) ?
_cod_database_fobs_code 2244200