#------------------------------------------------------------------------------
#$Date: 2021-12-17 04:58:28 +0200 (Fri, 17 Dec 2021) $
#$Revision: 271492 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243951.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_2243951
loop_
_publ_author_name
'Brennessel, William W.'
'Ellis, John E.'
_publ_section_title
;
Crystal structures of two novel iron isocyanides from the reaction of
2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate({-}1)
;
_journal_coeditor_code YZ2014
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S205698902101313X
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac '[Fe (C14 H10) (C9 H9 N)3]'
_chemical_formula_moiety 'C41 H37 Fe N3'
_chemical_formula_sum 'C41 H37 Fe N3'
_chemical_formula_weight 627.58
_chemical_name_systematic
;
[(1,2,3,4-\h)-Anthracene]tris(2,6-dimethylphenyl isocyanide)iron
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 93.057(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.8528(11)
_cell_length_b 10.9022(10)
_cell_length_c 24.927(2)
_cell_measurement_reflns_used 2566
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 24.29
_cell_measurement_theta_min 2.48
_cell_volume 3216.5(5)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare et al., 1999)
;
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Siemens SMART CCD platform'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0873
_diffrn_reflns_av_unetI/netI 0.0747
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 24459
_diffrn_reflns_theta_full 25.065
_diffrn_reflns_theta_max 25.065
_diffrn_reflns_theta_min 1.636
_diffrn_source 'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu 0.503
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8202
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.296
_exptl_crystal_description block
_exptl_crystal_F_000 1320
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.363
_refine_diff_density_min -0.347
_refine_ls_extinction_coef 0.0108(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 429
_refine_ls_number_reflns 5687
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.050
_refine_ls_R_factor_all 0.0968
_refine_ls_R_factor_gt 0.0597
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+1.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1089
_refine_ls_wR_factor_ref 0.1202
_reflns_number_gt 4023
_reflns_number_total 5687
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2014sup1.cif
_cod_data_source_block 1
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2243951
_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 0.893
_shelx_estimated_absorpt_t_max 0.961
_shelx_hkl_file
;
-1 0 0 4.67 1.08 3
1 0 0 4.90 1.43 4
-1 0 0 3.45 1.37 2
1 0 0 5.53 1.09 1
-2 0 0 3996.55 193.84 2
2 0 0 3970.86 194.77 4
2 0 0 3722.12 163.42 1
3 0 0 2.64 5.22 4
-3 0 0 3.25 4.09 3
3 0 0 3.71 4.05 1
-4 0 0 44.29 6.33 2
-4 0 0 42.28 4.94 3
4 0 0 38.12 4.70 1
5 0 0 -0.28 4.63 1
-5 0 0 1.78 4.77 3
6 0 0 1.20 5.22 1
-6 0 0 14.40 5.90 3
7 0 0 -2.95 5.93 1
-7 0 0 -1.03 6.26 3
-7 0 0 -1.48 6.59 2
-8 0 0 322.14 18.54 3
8 0 0 334.03 16.76 1
-8 0 0 320.31 20.42 2
-9 0 0 5.24 8.17 3
-9 0 0 -4.24 7.89 2
9 0 0 5.48 7.41 1
-10 0 0 111.90 12.08 2
10 0 0 111.04 10.57 1
-11 0 0 9.59 8.87 2
11 0 0 -1.24 8.73 1
-12 0 0 23.87 9.11 2
-13 0 0 13.78 10.40 2
-14 0 0 60.62 11.92 2
0 1 0 2.18 1.39 3
0 -1 0 1.74 1.42 1
0 -1 0 2.28 0.78 2
-1 1 0 18.04 1.64 2
1 -1 0 18.30 2.10 1
-1 1 0 14.79 2.30 3
1 1 0 19.56 2.46 4
-1 -1 0 15.55 2.20 1
-1 -1 0 18.56 2.45 2
-2 -1 0 33.33 3.58 1
2 -1 0 39.63 3.61 1
2 1 0 31.60 3.98 4
-2 -1 0 34.84 4.52 2
-2 1 0 29.23 3.78 2
-2 1 0 36.88 4.01 3
-3 1 0 695.44 35.29 3
-3 1 0 716.61 37.13 2
-3 -1 0 725.39 37.45 2
-3 -1 0 724.71 31.31 1
3 -1 0 758.79 31.34 1
4 1 0 423.52 23.46 4
4 -1 0 408.40 19.47 1
-4 -1 0 424.20 23.55 2
-4 -1 0 438.45 19.61 1
-4 1 0 450.88 23.32 2
-4 1 0 458.41 22.13 3
-5 -1 0 172.40 9.45 3
5 1 0 158.39 9.11 1
-5 1 0 177.48 10.62 3
5 -1 0 168.60 9.23 1
-5 1 0 155.07 10.91 2
5 1 0 169.13 11.16 4
-5 -1 0 147.44 11.11 2
6 -1 0 124.17 8.04 1
-6 -1 0 86.22 9.41 2
6 1 0 109.18 9.58 4
-6 -1 0 113.99 7.86 3
-6 1 0 111.60 9.20 3
-6 1 0 93.10 9.31 2
6 1 0 119.50 7.94 1
-7 -1 0 98.28 10.00 2
-7 1 0 104.80 9.40 3
-7 1 0 100.32 9.50 2
7 1 0 109.59 10.48 4
7 -1 0 102.67 8.14 1
-7 -1 0 104.44 8.17 3
7 1 0 101.54 8.14 1
-8 -1 0 270.02 18.38 2
-8 1 0 306.67 17.27 3
-8 -1 0 275.25 15.81 3
8 -1 0 272.50 15.26 1
-8 1 0 276.13 18.01 2
8 1 0 280.06 15.16 1
-9 -1 0 33.79 9.39 2
-9 1 0 31.60 9.06 2
9 -1 0 44.64 8.82 1
-9 1 0 49.50 9.63 3
9 1 0 42.93 8.56 1
-10 1 0 36.53 10.39 3
10 1 0 51.84 8.92 1
-10 1 0 37.63 9.59 2
10 -1 0 74.24 9.95 1
-10 -1 0 44.50 10.06 2
-11 -1 0 19.98 9.25 2
-11 1 0 23.60 8.94 2
11 -1 0 30.13 9.97 1
11 1 0 9.03 8.97 1
-12 -1 0 59.72 10.53 2
-12 1 0 70.34 10.97 2
-13 -1 0 9.69 10.05 2
-13 1 0 17.66 10.04 2
-14 1 0 40.67 11.61 2
-14 -1 0 30.55 11.30 2
0 2 0 1366.91 65.00 3
1 2 0 1948.53 96.91 4
1 -2 0 1884.77 81.32 1
-1 -2 0 1954.36 81.41 1
-2 -2 0 5.13 5.50 2
2 2 0 24.37 5.15 4
-2 2 0 31.32 3.87 2
-2 -2 0 9.48 4.22 1
2 -2 0 13.96 5.24 1
3 2 0 3.04 5.09 4
-3 2 0 -0.03 5.10 3
-3 -2 0 -0.57 5.18 2
3 -2 0 6.72 4.76 1
-3 -2 0 2.23 4.50 1
-4 2 0 28.52 6.18 3
-4 -2 0 17.14 5.67 2
4 2 0 26.56 5.50 4
-4 2 0 18.56 4.72 2
4 -2 0 33.65 5.09 1
-4 -2 0 35.08 4.93 1
-5 -2 0 165.46 9.66 1
5 2 0 174.87 11.89 4
5 -2 0 179.84 9.84 1
-5 2 0 180.43 11.18 2
-5 -2 0 163.62 11.81 2
-5 2 0 175.19 11.39 3
-6 2 0 158.60 10.83 2
6 -2 0 159.07 9.53 1
-6 -2 0 143.81 11.36 2
-6 2 0 162.47 11.19 3
-6 -2 0 142.01 8.61 3
6 2 0 139.96 11.31 4
-6 -2 0 155.14 9.45 1
7 -2 0 45.96 7.01 1
-7 -2 0 42.75 8.01 2
-7 2 0 42.98 8.43 3
7 2 0 23.67 8.27 4
-7 2 0 51.54 7.30 2
-7 -2 0 40.73 5.46 3
7 2 0 46.78 6.97 1
8 2 0 417.41 20.01 1
-8 2 0 413.00 23.37 2
8 -2 0 383.28 19.81 1
8 2 0 391.72 23.64 4
-8 -2 0 381.29 23.95 2
-8 2 0 396.49 22.75 3
-9 2 0 89.14 11.09 2
9 2 0 113.69 9.95 1
-9 2 0 107.48 12.08 3
9 -2 0 119.48 10.35 1
9 2 0 112.67 12.20 4
-9 -2 0 90.24 11.58 2
-10 2 0 72.95 11.29 3
10 -2 0 81.33 10.34 1
-10 -2 0 62.21 10.58 2
10 2 0 59.22 11.84 4
10 2 0 59.80 9.49 1
-10 2 0 72.28 9.92 2
11 2 0 -11.50 8.55 1
-11 2 0 11.52 8.44 2
-11 -2 0 0.31 8.50 2
-11 2 0 25.95 11.09 3
12 2 0 8.12 9.56 1
-12 2 0 33.44 10.01 2
-12 -2 0 25.07 9.77 2
-13 2 0 26.25 10.09 2
-13 -2 0 14.67 10.47 2
0 -3 0 -2.92 5.12 1
0 3 0 1.14 5.26 3
-1 -3 0 2067.45 98.29 2
1 3 0 1908.30 99.17 4
-1 -3 0 1927.59 83.34 1
-2 3 0 373.93 20.52 3
-2 -3 0 400.58 18.28 1
2 3 0 375.75 21.47 4
-2 -3 0 399.23 21.07 2
2 3 0 435.85 19.44 3
2 -3 0 374.84 18.23 1
-2 3 0 413.05 20.15 2
3 -3 0 39.81 5.94 1
-3 -3 0 35.89 5.69 2
-3 3 0 41.05 4.01 2
3 3 0 43.00 6.13 4
-3 -3 0 45.40 5.53 1
-3 3 0 37.43 6.43 3
-4 3 0 234.55 13.85 3
4 3 0 209.60 13.83 4
-4 -3 0 226.99 13.90 2
4 -3 0 223.16 12.08 1
-4 3 0 232.96 12.84 2
-4 -3 0 228.96 12.06 1
-5 -3 0 14.21 6.37 2
-5 -3 0 15.11 5.87 1
5 3 0 17.44 6.23 4
5 -3 0 14.18 6.06 1
-5 3 0 30.49 7.63 3
-5 3 0 26.69 5.23 2
6 3 0 197.37 13.99 4
-6 -3 0 221.35 11.85 1
-6 3 0 200.05 12.81 2
6 -3 0 209.86 12.10 1
-6 -3 0 192.93 13.87 2
-6 3 0 209.74 13.93 3
-7 3 0 3.58 8.41 3
-7 -3 0 17.67 6.74 1
-7 -3 0 1.38 7.52 2
-7 3 0 4.29 6.03 2
7 3 0 23.69 8.49 4
7 -3 0 2.58 7.76 1
-8 3 0 141.00 11.43 2
-8 3 0 137.88 13.37 3
8 3 0 139.60 10.87 1
8 -3 0 154.79 11.54 1
-8 -3 0 124.81 12.53 2
8 3 0 155.31 12.92 4
9 -3 0 19.44 9.86 1
-9 -3 0 7.17 9.03 2
9 3 0 4.64 8.16 1
9 3 0 4.15 9.83 4
-9 3 0 0.91 10.63 3
10 3 0 80.87 11.80 4
10 -3 0 107.78 12.03 1
-10 3 0 107.83 12.57 3
10 3 0 116.07 10.61 1
-10 -3 0 76.71 11.07 2
-10 3 0 96.31 10.67 2
11 3 0 123.35 13.87 4
-11 -3 0 112.26 12.65 2
11 3 0 119.08 11.54 1
-11 3 0 127.95 14.78 3
-11 3 0 127.19 12.56 2
-12 3 0 41.58 10.11 2
-12 -3 0 26.36 9.57 2
12 3 0 29.66 10.30 1
-13 -3 0 19.36 10.39 2
-13 3 0 16.14 10.03 2
0 -4 0 332.29 15.76 2
0 4 0 279.77 16.10 3
0 -4 0 297.11 14.80 1
1 4 0 -4.02 4.64 3
1 4 0 2.21 5.23 4
1 -4 0 7.87 5.35 1
-1 4 0 0.05 5.49 3
-1 -4 0 -4.94 5.28 1
-2 4 0 670.96 35.81 3
-2 -4 0 700.27 31.93 1
-2 -4 0 746.36 37.08 2
2 -4 0 713.31 31.87 1
2 4 0 772.72 37.93 4
-3 -4 0 -1.38 5.87 1
3 4 0 -4.74 5.47 4
-3 4 0 1.43 2.21 2
-3 4 0 -2.40 6.40 3
3 4 0 -1.34 3.24 3
-4 -4 0 76.92 7.82 2
4 -4 0 82.59 7.85 1
4 4 0 101.13 8.67 4
-4 4 0 79.43 8.90 3
-4 4 0 82.79 5.87 2
-4 -4 0 75.42 7.45 1
-5 4 0 131.93 10.91 3
-5 -4 0 112.02 9.91 2
-5 -4 0 128.03 9.17 1
5 -4 0 120.78 9.30 1
-5 4 0 119.92 8.31 2
5 4 0 127.98 10.31 4
6 4 0 73.22 8.57 4
-6 -4 0 68.07 8.72 2
-6 4 0 69.06 9.73 3
-6 -4 0 79.23 8.15 1
-6 4 0 68.85 6.91 2
6 -4 0 61.07 8.39 1
7 4 0 37.63 8.57 4
-7 4 0 39.27 10.06 3
7 -4 0 40.11 8.81 1
-7 -4 0 49.65 8.76 2
-7 -4 0 57.22 7.75 1
-7 4 0 53.82 7.15 2
8 -4 0 188.65 13.19 1
-8 4 0 190.11 15.38 3
-8 4 0 187.20 13.30 2
8 4 0 202.87 15.37 4
-8 -4 0 166.75 14.61 2
-8 -4 0 203.27 12.68 1
9 -4 0 -9.58 9.49 1
-9 -4 0 -0.43 8.19 1
9 4 0 -8.74 9.20 4
-9 -4 0 -2.03 8.73 2
-9 4 0 -2.47 10.46 3
-9 4 0 -2.70 7.24 2
10 4 0 309.62 21.42 4
10 4 0 342.63 18.32 1
-10 4 0 323.53 20.17 2
-10 -4 0 289.22 21.04 2
-10 4 0 323.24 21.07 3
10 -4 0 316.56 18.36 1
11 4 0 10.43 9.30 1
-11 -4 0 3.38 8.99 2
-11 4 0 7.31 12.06 3
-11 4 0 12.17 8.49 2
11 4 0 6.83 9.88 4
12 4 0 9.25 10.07 1
-12 4 0 11.94 12.98 3
12 4 0 15.42 11.57 4
-12 -4 0 7.07 9.60 2
13 4 0 8.09 12.97 4
-13 -4 0 28.12 11.33 2
0 -5 0 -4.17 6.13 1
0 -5 0 2.82 2.99 2
1 5 0 40.84 7.12 4
-1 5 0 39.35 6.85 3
1 5 0 43.60 6.36 3
-1 -5 0 49.45 6.97 1
1 -5 0 33.55 6.63 1
-1 -5 0 47.32 4.89 2
-2 5 0 1192.85 60.46 3
-2 -5 0 1286.00 62.81 2
2 -5 0 1161.80 53.68 1
-2 -5 0 1232.66 53.89 1
2 5 0 1350.81 59.61 3
2 5 0 1218.16 63.92 4
-3 -5 0 97.96 8.34 1
3 5 0 78.87 8.68 4
3 -5 0 90.04 8.32 1
-3 5 0 87.11 9.39 3
-3 -5 0 82.26 7.64 2
3 5 0 97.36 6.63 3
-4 5 0 480.68 23.24 2
4 5 0 447.55 25.84 4
-4 5 0 458.43 24.87 3
4 -5 0 431.33 21.67 1
-4 -5 0 433.44 21.71 1
-4 -5 0 462.90 24.94 2
-5 -5 0 61.48 7.76 1
-5 -5 0 54.81 7.54 2
5 5 0 50.40 8.71 4
5 -5 0 60.93 8.03 1
-5 5 0 51.54 4.92 2
-5 5 0 46.05 9.56 3
-6 -5 0 25.20 7.82 1
6 -5 0 51.21 8.86 1
6 5 0 26.19 8.03 4
-6 5 0 35.58 5.38 2
-6 -5 0 34.13 7.63 2
-6 5 0 32.56 10.02 3
-7 5 0 61.53 6.96 2
7 5 0 57.18 9.57 4
-7 5 0 63.90 11.19 3
-7 -5 0 57.47 8.48 1
-7 -5 0 47.09 8.73 2
7 -5 0 47.26 9.29 1
-8 5 0 136.32 10.20 2
-8 5 0 147.50 14.22 3
-8 -5 0 115.64 10.33 1
8 -5 0 110.91 11.64 1
8 5 0 124.06 12.80 4
-8 -5 0 132.49 12.30 2
-9 5 0 19.53 11.13 3
9 5 0 19.57 9.66 4
-9 -5 0 25.46 9.41 2
9 -5 0 24.32 9.79 1
-9 -5 0 12.48 8.71 1
10 -5 0 0.33 10.04 1
-10 5 0 8.64 11.14 3
-10 -5 0 3.70 8.81 1
10 5 0 15.79 10.19 4
-10 -5 0 24.48 9.08 2
11 5 0 49.28 10.44 1
11 5 0 31.72 11.56 4
-11 -5 0 45.65 10.33 2
-11 5 0 47.53 13.60 3
-12 5 0 55.83 14.52 3
12 5 0 44.19 11.32 1
12 5 0 58.93 12.24 4
-12 -5 0 56.46 11.31 2
-13 -5 0 19.64 11.10 2
13 5 0 -2.81 12.19 4
-13 5 0 11.64 15.70 3
0 6 0 101.96 9.05 3
0 -6 0 107.39 9.23 1
-1 -6 0 34.83 7.71 1
-1 6 0 52.35 7.66 3
1 -6 0 40.77 7.55 1
1 6 0 47.20 7.18 3
-1 -6 0 42.08 4.97 2
1 6 0 40.67 7.65 4
2 -6 0 242.51 14.19 1
-2 6 0 249.60 15.67 3
2 6 0 262.99 14.33 3
-2 -6 0 240.70 14.43 2
2 6 0 240.36 15.82 4
-2 -6 0 258.51 14.28 1
3 6 0 149.94 11.75 4
-3 -6 0 143.58 10.91 1
3 -6 0 150.63 11.01 1
-3 6 0 160.19 12.47 3
3 6 0 152.56 9.93 3
-3 -6 0 157.27 10.59 2
-4 -6 0 1.22 7.31 1
-4 -6 0 0.57 6.03 2
4 6 0 -4.77 4.98 3
4 6 0 -2.67 7.30 4
4 -6 0 13.41 7.94 1
-4 6 0 0.94 8.63 3
5 -6 0 123.31 10.49 1
-5 -6 0 100.01 10.20 2
-5 6 0 123.36 12.37 3
5 6 0 133.51 12.29 4
-5 -6 0 113.93 10.39 1
-6 -6 0 21.48 7.47 2
6 -6 0 29.13 9.17 1
-6 -6 0 24.93 8.34 1
6 6 0 32.86 8.98 4
-6 6 0 26.04 10.69 3
-7 6 0 53.50 11.90 3
-7 -6 0 45.76 9.39 1
7 -6 0 55.54 9.59 1
-7 -6 0 42.71 9.04 2
7 6 0 43.75 9.70 4
-8 -6 0 137.01 12.65 2
8 -6 0 147.15 12.45 1
-8 -6 0 127.23 11.51 1
8 6 0 126.99 13.04 4
-8 6 0 154.02 15.22 3
-9 -6 0 79.31 9.96 1
-9 -6 0 110.35 11.62 2
9 6 0 109.22 12.34 4
9 -6 0 107.04 12.32 1
-9 6 0 106.02 13.37 3
10 6 0 270.08 19.67 4
-10 -6 0 269.66 16.94 1
-10 -6 0 243.71 18.61 2
10 -6 0 262.80 17.23 1
-10 6 0 247.43 19.82 3
11 6 0 25.81 10.70 1
-11 -6 0 20.41 10.74 1
-11 6 0 33.26 13.62 3
-11 -6 0 23.82 10.41 2
11 6 0 19.40 11.19 4
12 6 0 10.19 11.05 1
-12 -6 0 11.59 10.36 2
-12 6 0 20.53 14.78 3
0 -7 0 -8.65 7.93 1
0 7 0 -5.09 7.50 3
0 7 0 11.61 7.46 4
1 7 0 414.52 22.61 3
1 7 0 419.24 24.68 4
1 -7 0 430.02 21.47 1
-1 7 0 410.68 23.18 3
-1 -7 0 428.80 21.51 1
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_shelx_res_file
;
TITL 02252 in P2(1)/n
02252.res
created by SHELXL-2018/3 at 10:11:14 on 06-Dec-2021
CELL 0.71073 11.8528 10.9022 24.9268 90.000 93.057 90.000
ZERR 4.00 0.0011 0.0010 0.0023 0.000 0.002 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N FE
UNIT 164 148 12 4
TEMP -100
SIZE 0.23 0.14 0.08
L.S. 12
BOND $H
FMAP 2
PLAN 18
ACTA
CONF
LIST 4
HTAB
WGHT 0.050500 1.149100
EXTI 0.010768
FVAR 0.33370
FE1 4 0.312142 0.234187 0.062057 11.00000 0.02478 0.01934 =
0.03844 -0.00136 -0.00097 -0.00325
C1 1 0.359657 0.137448 -0.009484 11.00000 0.02988 0.02433 =
0.05007 -0.00725 0.01097 -0.00452
H1A 2 0.427306 0.156795 -0.027057 11.00000 0.04887
C2 1 0.369709 0.067121 0.038260 11.00000 0.03412 0.01998 =
0.05850 -0.00623 -0.00497 0.00087
H2A 2 0.437487 0.038153 0.053481 11.00000 0.03961
C3 1 0.270619 0.053503 0.065787 11.00000 0.03888 0.01872 =
0.04565 0.00002 -0.00266 -0.00783
H3A 2 0.267185 0.007149 0.097690 11.00000 0.05264
C4 1 0.173986 0.115065 0.042810 11.00000 0.02836 0.02268 =
0.03518 0.00018 0.00471 -0.00706
H4A 2 0.112757 0.116260 0.063053 11.00000 0.03158
C5 1 -0.063767 0.147567 -0.127858 11.00000 0.04972 0.02821 =
0.04372 0.00193 -0.00336 -0.01235
AFIX 43
H5A 2 -0.131036 0.146436 -0.108779 11.00000 -1.20000
AFIX 0
C6 1 -0.071260 0.160566 -0.182781 11.00000 0.07089 0.03604 =
0.04184 0.00464 -0.01413 -0.01427
AFIX 43
H6A 2 -0.143118 0.167987 -0.201270 11.00000 -1.20000
AFIX 0
C7 1 0.026812 0.162849 -0.211346 11.00000 0.09222 0.03848 =
0.03308 -0.00100 -0.00421 -0.01962
AFIX 43
H7A 2 0.021654 0.171483 -0.249322 11.00000 -1.20000
AFIX 0
C8 1 0.129961 0.152717 -0.184866 11.00000 0.07563 0.03343 =
0.04056 -0.00760 0.02046 -0.01538
AFIX 43
H8A 2 0.195912 0.154133 -0.204906 11.00000 -1.20000
AFIX 0
C9 1 0.248120 0.136673 -0.099234 11.00000 0.04345 0.02624 =
0.04617 -0.01036 0.01670 -0.00768
AFIX 43
H9A 2 0.315408 0.138178 -0.118294 11.00000 -1.20000
AFIX 0
C10 1 0.051294 0.123512 -0.042678 11.00000 0.03432 0.02286 =
0.03235 -0.00019 0.00612 -0.01065
AFIX 43
H10A 2 -0.015070 0.117228 -0.023102 11.00000 -1.20000
AFIX 0
C11 1 0.255537 0.131213 -0.044385 11.00000 0.03293 0.01967 =
0.04192 -0.00461 0.00878 -0.00544
C12 1 0.155156 0.120466 -0.015710 11.00000 0.03172 0.01605 =
0.03519 -0.00425 0.00469 -0.00774
C13 1 0.041541 0.135865 -0.099172 11.00000 0.04589 0.02017 =
0.03287 -0.00212 0.00223 -0.01092
C14 1 0.141554 0.140150 -0.128371 11.00000 0.05437 0.01832 =
0.03230 -0.00471 0.00889 -0.01298
C15 1 0.263043 0.374146 0.026213 11.00000 0.02687 0.02632 =
0.03742 -0.00599 0.00336 -0.00817
N1 3 0.230449 0.462654 0.004117 11.00000 0.03820 0.02578 =
0.04318 0.00587 0.00624 0.00252
C16 1 0.194197 0.572069 -0.020912 11.00000 0.03067 0.02349 =
0.03633 0.00304 0.00960 0.00254
C17 1 0.103011 0.568275 -0.058814 11.00000 0.02990 0.03381 =
0.03363 -0.00288 0.00649 -0.00083
C18 1 0.070464 0.677554 -0.082703 11.00000 0.03323 0.04478 =
0.03478 -0.00129 0.00022 0.00290
AFIX 43
H18A 2 0.008746 0.678274 -0.108631 11.00000 -1.20000
AFIX 0
C19 1 0.125694 0.786314 -0.069765 11.00000 0.04928 0.02927 =
0.03880 0.00464 0.00888 0.01065
AFIX 43
H19A 2 0.101896 0.860406 -0.086943 11.00000 -1.20000
AFIX 0
C20 1 0.214341 0.787540 -0.032369 11.00000 0.04444 0.02750 =
0.03745 -0.00317 0.00651 -0.00390
AFIX 43
H20A 2 0.251753 0.862681 -0.023879 11.00000 -1.20000
AFIX 0
C21 1 0.250595 0.680130 -0.006531 11.00000 0.03216 0.03012 =
0.03380 -0.00069 0.00272 -0.00093
C22 1 0.044762 0.448876 -0.072977 11.00000 0.04992 0.04171 =
0.05436 -0.00752 0.00038 -0.01512
AFIX 137
H22A 2 -0.015053 0.463279 -0.100939 11.00000 -1.50000
H22B 2 0.011639 0.414999 -0.040972 11.00000 -1.50000
H22C 2 0.099809 0.390683 -0.086233 11.00000 -1.50000
AFIX 0
C23 1 0.347448 0.681072 0.034989 11.00000 0.04749 0.05540 =
0.05687 0.00152 -0.00901 -0.01087
AFIX 137
H23A 2 0.327591 0.632025 0.066055 11.00000 -1.50000
H23B 2 0.363206 0.765629 0.046433 11.00000 -1.50000
H23C 2 0.414650 0.646176 0.019532 11.00000 -1.50000
AFIX 0
C24 1 0.451051 0.286033 0.089740 11.00000 0.03116 0.02145 =
0.04254 -0.00051 0.00406 0.00116
N2 3 0.536124 0.316834 0.111206 11.00000 0.02941 0.03931 =
0.04634 -0.00906 -0.00113 -0.00585
C25 1 0.631522 0.360605 0.140587 11.00000 0.02188 0.03263 =
0.03440 -0.00498 0.00215 -0.00395
C26 1 0.653925 0.486282 0.139168 11.00000 0.03463 0.03240 =
0.03521 -0.00242 0.00350 -0.00443
C27 1 0.747251 0.528420 0.169427 11.00000 0.04332 0.03760 =
0.04741 -0.01040 0.00642 -0.01478
AFIX 43
H27A 2 0.764292 0.613569 0.169569 11.00000 -1.20000
AFIX 0
C28 1 0.815596 0.449744 0.199198 11.00000 0.03297 0.06947 =
0.03815 -0.01983 0.00065 -0.01062
AFIX 43
H28A 2 0.879716 0.480378 0.219426 11.00000 -1.20000
AFIX 0
C29 1 0.791214 0.326069 0.199770 11.00000 0.03337 0.05952 =
0.03509 -0.00044 -0.00011 0.00771
AFIX 43
H29A 2 0.838982 0.272388 0.220648 11.00000 -1.20000
AFIX 0
C30 1 0.698553 0.278340 0.170555 11.00000 0.03371 0.03333 =
0.03803 -0.00034 0.00707 0.00047
C31 1 0.580046 0.569787 0.104842 11.00000 0.05256 0.03988 =
0.06865 0.00663 -0.00293 0.00181
AFIX 137
H31A 2 0.575586 0.539425 0.067785 11.00000 -1.50000
H31B 2 0.612114 0.652662 0.105700 11.00000 -1.50000
H31C 2 0.504147 0.571857 0.118604 11.00000 -1.50000
AFIX 0
C32 1 0.672021 0.144232 0.170886 11.00000 0.05847 0.03536 =
0.07404 0.01137 0.00758 0.00193
AFIX 137
H32A 2 0.731368 0.100511 0.192037 11.00000 -1.50000
H32B 2 0.668099 0.113055 0.133959 11.00000 -1.50000
H32C 2 0.599212 0.131257 0.186880 11.00000 -1.50000
AFIX 0
C33 1 0.249564 0.273173 0.124042 11.00000 0.02751 0.02539 =
0.04089 -0.00109 -0.00897 -0.00438
N3 3 0.201040 0.294538 0.163158 11.00000 0.03422 0.04084 =
0.04007 -0.00760 -0.00335 -0.00384
C34 1 0.155762 0.346330 0.207810 11.00000 0.02797 0.03499 =
0.03269 -0.00702 -0.00597 0.00434
C35 1 0.179916 0.468905 0.219153 11.00000 0.03381 0.04176 =
0.04704 -0.00854 -0.01579 0.00072
C36 1 0.139754 0.516904 0.265961 11.00000 0.04622 0.04967 =
0.06328 -0.02469 -0.01837 0.01155
AFIX 43
H36A 2 0.154918 0.600200 0.274916 11.00000 -1.20000
AFIX 0
C37 1 0.078675 0.446777 0.299571 11.00000 0.04205 0.08538 =
0.04688 -0.02663 -0.00931 0.02679
AFIX 43
H37A 2 0.054290 0.480930 0.332048 11.00000 -1.20000
AFIX 0
C38 1 0.052114 0.325668 0.286398 11.00000 0.03602 0.06983 =
0.04235 0.00225 -0.00377 0.01274
AFIX 43
H38A 2 0.008566 0.278127 0.309637 11.00000 -1.20000
AFIX 0
C39 1 0.088812 0.274062 0.239601 11.00000 0.03074 0.03916 =
0.03877 0.00114 -0.00593 0.01076
C40 1 0.246254 0.543162 0.181509 11.00000 0.06775 0.04887 =
0.07299 0.00496 -0.01695 -0.01840
AFIX 137
H40B 2 0.251798 0.627969 0.194415 11.00000 -1.50000
H40C 2 0.208241 0.541810 0.145624 11.00000 -1.50000
H40D 2 0.322229 0.508409 0.179802 11.00000 -1.50000
AFIX 0
C41 1 0.056903 0.145878 0.222337 11.00000 0.04276 0.04234 =
0.05987 0.00529 -0.00019 0.00038
AFIX 137
H41B 2 0.125365 0.099304 0.215470 11.00000 -1.50000
H41C 2 0.007835 0.149243 0.189459 11.00000 -1.50000
H41D 2 0.016726 0.105596 0.250836 11.00000 -1.50000
AFIX 0
HKLF 4
REM 02252 in P2(1)/n
REM wR2 = 0.120204, GooF = S = 1.04976, Restrained GooF = 1.04976 for all data
REM R1 = 0.059680 for 4023 Fo > 4sig(Fo) and 0.096814 for all 5687 data
REM 429 parameters refined using 0 restraints
END
WGHT 0.0504 1.1509
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.363, deepest hole -0.347, 1-sigma level 0.069
Q1 1 0.3361 0.1477 0.0423 11.00000 0.05 0.36
Q2 1 0.3213 0.3046 0.0948 11.00000 0.05 0.35
Q3 1 0.2053 0.6333 0.0017 11.00000 0.05 0.30
Q4 1 0.3053 0.4752 0.0311 11.00000 0.05 0.30
Q5 1 0.3573 0.3149 0.0413 11.00000 0.05 0.30
Q6 1 0.3258 0.3396 0.0429 11.00000 0.05 0.28
Q7 1 0.2091 0.5268 -0.0117 11.00000 0.05 0.28
Q8 1 0.2668 0.1535 0.0805 11.00000 0.05 0.27
Q9 1 0.3005 0.3065 0.0228 11.00000 0.05 0.27
Q10 1 0.1221 0.5552 -0.0307 11.00000 0.05 0.26
Q11 1 0.1860 0.8760 -0.0119 11.00000 0.05 0.25
Q12 1 0.1836 0.5781 -0.0492 11.00000 0.05 0.25
Q13 1 0.2444 0.6198 -0.0215 11.00000 0.05 0.25
Q14 1 0.4031 0.2235 0.0587 11.00000 0.05 0.25
Q15 1 0.4145 0.1583 -0.1052 11.00000 0.05 0.24
Q16 1 0.5108 0.6433 0.1249 11.00000 0.05 0.24
Q17 1 0.2371 0.3029 0.0512 11.00000 0.05 0.24
Q18 1 0.2070 0.7653 -0.0655 11.00000 0.05 0.24
;
_shelx_res_checksum 21634
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.31214(4) 0.23419(4) 0.06206(2) 0.02761(16) Uani d 1 . .
C C1 0.3597(3) 0.1374(3) -0.00948(15) 0.0344(9) Uani d 1 . .
H H1A 0.427(3) 0.157(3) -0.0271(14) 0.049(11) Uiso d 1 . .
C C2 0.3697(3) 0.0671(3) 0.03826(16) 0.0378(9) Uani d 1 . .
H H2A 0.437(3) 0.038(3) 0.0535(14) 0.040(10) Uiso d 1 . .
C C3 0.2706(3) 0.0535(3) 0.06579(16) 0.0346(9) Uani d 1 . .
H H3A 0.267(3) 0.007(3) 0.0977(15) 0.053(12) Uiso d 1 . .
C C4 0.1740(3) 0.1151(3) 0.04281(14) 0.0286(8) Uani d 1 . .
H H4A 0.113(3) 0.116(3) 0.0631(13) 0.032(9) Uiso d 1 . .
C C5 -0.0638(3) 0.1476(3) -0.12786(15) 0.0408(9) Uani d 1 . .
H H5A -0.131036 0.146436 -0.108779 0.049 Uiso calc 1 . .
C C6 -0.0713(4) 0.1606(3) -0.18278(16) 0.0502(11) Uani d 1 . .
H H6A -0.143118 0.167987 -0.201270 0.060 Uiso calc 1 . .
C C7 0.0268(4) 0.1628(3) -0.21135(16) 0.0549(12) Uani d 1 . .
H H7A 0.021654 0.171483 -0.249322 0.066 Uiso calc 1 . .
C C8 0.1300(4) 0.1527(3) -0.18487(15) 0.0493(11) Uani d 1 . .
H H8A 0.195912 0.154133 -0.204906 0.059 Uiso calc 1 . .
C C9 0.2481(3) 0.1367(3) -0.09923(15) 0.0381(9) Uani d 1 . .
H H9A 0.315408 0.138178 -0.118294 0.046 Uiso calc 1 . .
C C10 0.0513(3) 0.1235(3) -0.04268(13) 0.0297(8) Uani d 1 . .
H H10A -0.015070 0.117228 -0.023102 0.036 Uiso calc 1 . .
C C11 0.2555(3) 0.1312(3) -0.04438(14) 0.0313(8) Uani d 1 . .
C C12 0.1552(3) 0.1205(3) -0.01571(13) 0.0276(8) Uani d 1 . .
C C13 0.0415(3) 0.1359(3) -0.09917(13) 0.0330(8) Uani d 1 . .
C C14 0.1416(3) 0.1402(3) -0.12837(14) 0.0348(9) Uani d 1 . .
C C15 0.2630(3) 0.3741(3) 0.02621(14) 0.0301(8) Uani d 1 . .
N N1 0.2304(2) 0.4627(2) 0.00412(12) 0.0356(7) Uani d 1 . .
C C16 0.1942(3) 0.5721(3) -0.02091(13) 0.0299(8) Uani d 1 . .
C C17 0.1030(3) 0.5683(3) -0.05881(13) 0.0323(8) Uani d 1 . .
C C18 0.0705(3) 0.6776(3) -0.08270(14) 0.0377(9) Uani d 1 . .
H H18A 0.008746 0.678274 -0.108631 0.045 Uiso calc 1 . .
C C19 0.1257(3) 0.7863(3) -0.06976(14) 0.0389(9) Uani d 1 . .
H H19A 0.101896 0.860406 -0.086943 0.047 Uiso calc 1 . .
C C20 0.2143(3) 0.7875(3) -0.03237(14) 0.0363(8) Uani d 1 . .
H H20A 0.251753 0.862681 -0.023879 0.044 Uiso calc 1 . .
C C21 0.2506(3) 0.6801(3) -0.00653(13) 0.0320(8) Uani d 1 . .
C C22 0.0448(3) 0.4489(3) -0.07298(16) 0.0487(10) Uani d 1 . .
H H22A -0.015053 0.463279 -0.100939 0.073 Uiso calc 1 . .
H H22B 0.011639 0.414999 -0.040972 0.073 Uiso calc 1 . .
H H22C 0.099809 0.390683 -0.086233 0.073 Uiso calc 1 . .
C C23 0.3474(3) 0.6811(4) 0.03499(17) 0.0537(11) Uani d 1 . .
H H23A 0.327591 0.632025 0.066055 0.081 Uiso calc 1 . .
H H23B 0.363206 0.765629 0.046433 0.081 Uiso calc 1 . .
H H23C 0.414650 0.646176 0.019532 0.081 Uiso calc 1 . .
C C24 0.4511(3) 0.2860(3) 0.08974(14) 0.0316(8) Uani d 1 . .
N N2 0.5361(2) 0.3168(3) 0.11121(12) 0.0385(7) Uani d 1 . .
C C25 0.6315(3) 0.3606(3) 0.14059(13) 0.0296(8) Uani d 1 . .
C C26 0.6539(3) 0.4863(3) 0.13917(14) 0.0340(8) Uani d 1 . .
C C27 0.7473(3) 0.5284(3) 0.16943(15) 0.0426(9) Uani d 1 . .
H H27A 0.764292 0.613569 0.169569 0.051 Uiso calc 1 . .
C C28 0.8156(3) 0.4497(4) 0.19920(15) 0.0469(10) Uani d 1 . .
H H28A 0.879716 0.480378 0.219426 0.056 Uiso calc 1 . .
C C29 0.7912(3) 0.3261(4) 0.19977(14) 0.0427(9) Uani d 1 . .
H H29A 0.838982 0.272388 0.220648 0.051 Uiso calc 1 . .
C C30 0.6986(3) 0.2783(3) 0.17056(14) 0.0348(8) Uani d 1 . .
C C31 0.5800(3) 0.5698(3) 0.10484(17) 0.0539(11) Uani d 1 . .
H H31A 0.575586 0.539425 0.067785 0.081 Uiso calc 1 . .
H H31B 0.612114 0.652662 0.105700 0.081 Uiso calc 1 . .
H H31C 0.504147 0.571857 0.118604 0.081 Uiso calc 1 . .
C C32 0.6720(4) 0.1442(3) 0.17089(18) 0.0558(12) Uani d 1 . .
H H32A 0.731368 0.100511 0.192037 0.084 Uiso calc 1 . .
H H32B 0.668099 0.113055 0.133959 0.084 Uiso calc 1 . .
H H32C 0.599212 0.131257 0.186880 0.084 Uiso calc 1 . .
C C33 0.2496(3) 0.2732(3) 0.12404(14) 0.0316(8) Uani d 1 . .
N N3 0.2010(2) 0.2945(3) 0.16316(12) 0.0386(7) Uani d 1 . .
C C34 0.1558(3) 0.3463(3) 0.20781(14) 0.0322(8) Uani d 1 . .
C C35 0.1799(3) 0.4689(3) 0.21915(15) 0.0415(9) Uani d 1 . .
C C36 0.1398(3) 0.5169(4) 0.26596(18) 0.0538(11) Uani d 1 . .
H H36A 0.154918 0.600200 0.274916 0.065 Uiso calc 1 . .
C C37 0.0787(3) 0.4468(4) 0.29957(17) 0.0585(13) Uani d 1 . .
H H37A 0.054290 0.480930 0.332048 0.070 Uiso calc 1 . .
C C38 0.0521(3) 0.3257(4) 0.28640(16) 0.0496(10) Uani d 1 . .
H H38A 0.008566 0.278127 0.309637 0.060 Uiso calc 1 . .
C C39 0.0888(3) 0.2741(3) 0.23960(14) 0.0365(8) Uani d 1 . .
C C40 0.2463(4) 0.5432(4) 0.18151(18) 0.0639(13) Uani d 1 . .
H H40B 0.251798 0.627969 0.194415 0.096 Uiso calc 1 . .
H H40C 0.208241 0.541810 0.145624 0.096 Uiso calc 1 . .
H H40D 0.322229 0.508409 0.179802 0.096 Uiso calc 1 . .
C C41 0.0569(3) 0.1459(3) 0.22234(17) 0.0484(10) Uani d 1 . .
H H41B 0.125365 0.099304 0.215470 0.073 Uiso calc 1 . .
H H41C 0.007835 0.149243 0.189459 0.073 Uiso calc 1 . .
H H41D 0.016726 0.105596 0.250836 0.073 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
Fe1 0.0248(3) 0.0193(2) 0.0384(3) -0.0033(2) -0.0010(2) -0.0014(2)
C1 0.030(2) 0.0243(17) 0.050(2) -0.0045(15) 0.0110(19) -0.0073(16)
C2 0.034(2) 0.0200(17) 0.058(3) 0.0009(15) -0.005(2) -0.0062(17)
C3 0.039(2) 0.0187(17) 0.046(2) -0.0078(14) -0.0027(19) 0.0000(16)
C4 0.028(2) 0.0227(17) 0.035(2) -0.0071(14) 0.0047(17) 0.0002(14)
C5 0.050(2) 0.0282(19) 0.044(2) -0.0124(16) -0.003(2) 0.0019(16)
C6 0.071(3) 0.036(2) 0.042(2) -0.0143(19) -0.014(2) 0.0046(18)
C7 0.092(4) 0.038(2) 0.033(2) -0.020(2) -0.004(3) -0.0010(18)
C8 0.076(3) 0.033(2) 0.041(2) -0.015(2) 0.020(2) -0.0076(17)
C9 0.043(2) 0.0262(18) 0.046(2) -0.0077(16) 0.0167(19) -0.0104(16)
C10 0.034(2) 0.0229(17) 0.0324(19) -0.0107(14) 0.0061(16) -0.0002(14)
C11 0.033(2) 0.0197(16) 0.042(2) -0.0054(14) 0.0088(17) -0.0046(14)
C12 0.032(2) 0.0161(15) 0.035(2) -0.0077(13) 0.0047(16) -0.0042(13)
C13 0.046(2) 0.0202(16) 0.033(2) -0.0109(15) 0.0022(18) -0.0021(14)
C14 0.054(2) 0.0183(16) 0.032(2) -0.0130(15) 0.0089(18) -0.0047(14)
C15 0.0269(19) 0.0263(18) 0.037(2) -0.0082(14) 0.0034(16) -0.0060(16)
N1 0.0382(17) 0.0258(16) 0.0432(18) 0.0025(13) 0.0062(14) 0.0059(13)
C16 0.0307(19) 0.0235(17) 0.036(2) 0.0025(14) 0.0096(16) 0.0030(14)
C17 0.0299(19) 0.0338(19) 0.034(2) -0.0008(15) 0.0065(16) -0.0029(15)
C18 0.033(2) 0.045(2) 0.035(2) 0.0029(17) 0.0002(17) -0.0013(17)
C19 0.049(2) 0.029(2) 0.039(2) 0.0106(16) 0.0089(19) 0.0046(16)
C20 0.044(2) 0.0275(19) 0.037(2) -0.0039(15) 0.0065(18) -0.0032(15)
C21 0.032(2) 0.0301(18) 0.0338(19) -0.0009(15) 0.0027(16) -0.0007(15)
C22 0.050(2) 0.042(2) 0.054(3) -0.0151(18) 0.000(2) -0.0075(19)
C23 0.047(2) 0.055(2) 0.057(3) -0.011(2) -0.009(2) 0.002(2)
C24 0.0312(19) 0.0214(17) 0.043(2) 0.0012(14) 0.0041(17) -0.0005(15)
N2 0.0294(17) 0.0393(17) 0.0463(19) -0.0059(14) -0.0011(15) -0.0091(14)
C25 0.0219(18) 0.0326(18) 0.0344(19) -0.0039(14) 0.0021(15) -0.0050(15)
C26 0.035(2) 0.0324(19) 0.035(2) -0.0044(15) 0.0035(16) -0.0024(15)
C27 0.043(2) 0.038(2) 0.047(2) -0.0148(18) 0.006(2) -0.0104(18)
C28 0.033(2) 0.069(3) 0.038(2) -0.011(2) 0.0007(18) -0.020(2)
C29 0.033(2) 0.060(3) 0.035(2) 0.0077(18) -0.0001(18) -0.0004(18)
C30 0.0337(19) 0.0333(18) 0.038(2) 0.0005(15) 0.0071(16) -0.0003(16)
C31 0.053(3) 0.040(2) 0.069(3) 0.0018(19) -0.003(2) 0.007(2)
C32 0.058(3) 0.035(2) 0.074(3) 0.0019(19) 0.008(2) 0.011(2)
C33 0.0275(18) 0.0254(17) 0.041(2) -0.0044(14) -0.0090(17) -0.0011(16)
N3 0.0342(17) 0.0408(18) 0.0401(19) -0.0038(13) -0.0034(15) -0.0076(14)
C34 0.0280(19) 0.0350(19) 0.033(2) 0.0043(15) -0.0060(16) -0.0070(16)
C35 0.034(2) 0.042(2) 0.047(2) 0.0007(17) -0.0158(18) -0.0085(18)
C36 0.046(3) 0.050(2) 0.063(3) 0.012(2) -0.018(2) -0.025(2)
C37 0.042(3) 0.085(3) 0.047(3) 0.027(2) -0.009(2) -0.027(2)
C38 0.036(2) 0.070(3) 0.042(2) 0.013(2) -0.0038(19) 0.002(2)
C39 0.0307(19) 0.039(2) 0.039(2) 0.0108(16) -0.0059(16) 0.0011(17)
C40 0.068(3) 0.049(3) 0.073(3) -0.018(2) -0.017(3) 0.005(2)
C41 0.043(2) 0.042(2) 0.060(3) 0.0004(18) 0.000(2) 0.0053(19)
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'
N N 0.0061 0.0033 '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'
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
C33 Fe1 C24 . . 90.40(14) y
C33 Fe1 C15 . . 94.97(14) y
C24 Fe1 C15 . . 100.38(14) y
C33 Fe1 C3 . . 94.45(15) ?
C24 Fe1 C3 . . 119.62(14) ?
C15 Fe1 C3 . . 138.74(14) ?
C33 Fe1 C2 . . 128.22(15) ?
C24 Fe1 C2 . . 94.40(14) ?
C15 Fe1 C2 . . 134.22(15) ?
C3 Fe1 C2 . . 40.14(14) ?
C33 Fe1 C4 . . 89.44(14) ?
C24 Fe1 C4 . . 159.38(13) ?
C15 Fe1 C4 . . 100.17(13) ?
C3 Fe1 C4 . . 39.90(13) ?
C2 Fe1 C4 . . 69.82(14) ?
C33 Fe1 C1 . . 162.98(14) ?
C24 Fe1 C1 . . 101.02(14) ?
C15 Fe1 C1 . . 95.33(14) ?
C3 Fe1 C1 . . 68.97(14) ?
C2 Fe1 C1 . . 39.09(14) ?
C4 Fe1 C1 . . 75.42(14) ?
C2 C1 C11 . . 120.1(3) ?
C2 C1 Fe1 . . 65.6(2) ?
C11 C1 Fe1 . . 105.2(2) ?
C2 C1 H1A . . 118(2) ?
C11 C1 H1A . . 116(2) ?
Fe1 C1 H1A . . 122(2) ?
C3 C2 C1 . . 115.8(3) ?
C3 C2 Fe1 . . 69.5(2) ?
C1 C2 Fe1 . . 75.3(2) ?
C3 C2 H2A . . 120(2) ?
C1 C2 H2A . . 124(2) ?
Fe1 C2 H2A . . 119(2) ?
C2 C3 C4 . . 115.6(3) ?
C2 C3 Fe1 . . 70.33(19) ?
C4 C3 Fe1 . . 73.50(19) ?
C2 C3 H3A . . 123(2) ?
C4 C3 H3A . . 121(2) ?
Fe1 C3 H3A . . 125(2) ?
C3 C4 C12 . . 119.8(3) ?
C3 C4 Fe1 . . 66.60(18) ?
C12 C4 Fe1 . . 106.0(2) ?
C3 C4 H4A . . 116(2) ?
C12 C4 H4A . . 118(2) ?
Fe1 C4 H4A . . 120(2) ?
C6 C5 C13 . . 121.5(4) ?
C6 C5 H5A . . 119.2 ?
C13 C5 H5A . . 119.2 ?
C5 C6 C7 . . 119.9(4) ?
C5 C6 H6A . . 120.0 ?
C7 C6 H6A . . 120.0 ?
C8 C7 C6 . . 120.1(4) ?
C8 C7 H7A . . 119.9 ?
C6 C7 H7A . . 119.9 ?
C7 C8 C14 . . 121.8(4) ?
C7 C8 H8A . . 119.1 ?
C14 C8 H8A . . 119.1 ?
C11 C9 C14 . . 121.3(3) ?
C11 C9 H9A . . 119.3 ?
C14 C9 H9A . . 119.3 ?
C12 C10 C13 . . 121.0(3) ?
C12 C10 H10A . . 119.5 ?
C13 C10 H10A . . 119.5 ?
C9 C11 C12 . . 119.6(3) ?
C9 C11 C1 . . 126.6(3) ?
C12 C11 C1 . . 113.8(3) ?
C10 C12 C11 . . 120.3(3) ?
C10 C12 C4 . . 125.0(3) ?
C11 C12 C4 . . 114.6(3) ?
C5 C13 C10 . . 122.5(3) ?
C5 C13 C14 . . 118.4(3) ?
C10 C13 C14 . . 119.1(3) ?
C8 C14 C9 . . 123.2(4) ?
C8 C14 C13 . . 118.2(4) ?
C9 C14 C13 . . 118.6(3) ?
N1 C15 Fe1 . . 178.8(3) ?
C15 N1 C16 . . 177.5(4) y
C21 C16 C17 . . 122.9(3) ?
C21 C16 N1 . . 118.3(3) ?
C17 C16 N1 . . 118.9(3) ?
C18 C17 C16 . . 117.1(3) ?
C18 C17 C22 . . 122.1(3) ?
C16 C17 C22 . . 120.8(3) ?
C17 C18 C19 . . 121.5(3) ?
C17 C18 H18A . . 119.3 ?
C19 C18 H18A . . 119.3 ?
C20 C19 C18 . . 120.3(3) ?
C20 C19 H19A . . 119.9 ?
C18 C19 H19A . . 119.9 ?
C19 C20 C21 . . 120.9(3) ?
C19 C20 H20A . . 119.5 ?
C21 C20 H20A . . 119.5 ?
C16 C21 C20 . . 117.4(3) ?
C16 C21 C23 . . 121.4(3) ?
C20 C21 C23 . . 121.2(3) ?
C17 C22 H22A . . 109.5 ?
C17 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C17 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C21 C23 H23A . . 109.5 ?
C21 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C21 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
N2 C24 Fe1 . . 174.7(3) ?
C24 N2 C25 . . 174.1(3) y
C30 C25 C26 . . 122.9(3) ?
C30 C25 N2 . . 119.0(3) ?
C26 C25 N2 . . 118.1(3) ?
C27 C26 C25 . . 117.4(3) ?
C27 C26 C31 . . 122.4(3) ?
C25 C26 C31 . . 120.3(3) ?
C28 C27 C26 . . 121.3(3) ?
C28 C27 H27A . . 119.3 ?
C26 C27 H27A . . 119.3 ?
C27 C28 C29 . . 120.0(3) ?
C27 C28 H28A . . 120.0 ?
C29 C28 H28A . . 120.0 ?
C28 C29 C30 . . 121.5(3) ?
C28 C29 H29A . . 119.3 ?
C30 C29 H29A . . 119.3 ?
C29 C30 C25 . . 117.0(3) ?
C29 C30 C32 . . 121.7(3) ?
C25 C30 C32 . . 121.3(3) ?
C26 C31 H31A . . 109.5 ?
C26 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C26 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
N3 C33 Fe1 . . 174.9(3) ?
C33 N3 C34 . . 166.5(3) y
N3 C34 C35 . . 118.1(3) ?
N3 C34 C39 . . 118.9(3) ?
C35 C34 C39 . . 122.9(3) ?
C36 C35 C34 . . 117.2(4) ?
C36 C35 C40 . . 122.7(4) ?
C34 C35 C40 . . 120.1(4) ?
C37 C36 C35 . . 121.4(4) ?
C37 C36 H36A . . 119.3 ?
C35 C36 H36A . . 119.3 ?
C36 C37 C38 . . 120.4(4) ?
C36 C37 H37A . . 119.8 ?
C38 C37 H37A . . 119.8 ?
C39 C38 C37 . . 120.4(4) ?
C39 C38 H38A . . 119.8 ?
C37 C38 H38A . . 119.8 ?
C38 C39 C34 . . 117.5(3) ?
C38 C39 C41 . . 122.2(4) ?
C34 C39 C41 . . 120.3(3) ?
C35 C40 H40B . . 109.5 ?
C35 C40 H40C . . 109.5 ?
H40B C40 H40C . . 109.5 ?
C35 C40 H40D . . 109.5 ?
H40B C40 H40D . . 109.5 ?
H40C C40 H40D . . 109.5 ?
C39 C41 H41B . . 109.5 ?
C39 C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
C39 C41 H41D . . 109.5 ?
H41B C41 H41D . . 109.5 ?
H41C C41 H41D . . 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
Fe1 C33 . 1.800(4) y
Fe1 C24 . 1.840(3) y
Fe1 C15 . 1.847(3) y
Fe1 C3 . 2.034(3) y
Fe1 C2 . 2.044(3) y
Fe1 C4 . 2.125(3) y
Fe1 C1 . 2.172(4) y
C1 C2 . 1.415(5) y
C1 C11 . 1.473(5) ?
C1 H1A . 0.96(4) ?
C2 C3 . 1.399(5) y
C2 H2A . 0.93(3) ?
C3 C4 . 1.421(5) y
C3 H3A . 0.94(4) ?
C4 C12 . 1.465(5) ?
C4 H4A . 0.91(3) ?
C5 C6 . 1.375(5) ?
C5 C13 . 1.411(5) ?
C5 H5A . 0.9500 ?
C6 C7 . 1.395(6) ?
C6 H6A . 0.9500 ?
C7 C8 . 1.363(6) ?
C7 H7A . 0.9500 ?
C8 C14 . 1.414(5) ?
C8 H8A . 0.9500 ?
C9 C11 . 1.367(5) ?
C9 C14 . 1.424(5) ?
C9 H9A . 0.9500 ?
C10 C12 . 1.371(4) ?
C10 C13 . 1.413(5) ?
C10 H10A . 0.9500 ?
C11 C12 . 1.425(4) ?
C13 C14 . 1.425(5) ?
C15 N1 . 1.167(4) y
N1 C16 . 1.403(4) ?
C16 C21 . 1.392(4) ?
C16 C17 . 1.398(5) ?
C17 C18 . 1.378(5) ?
C17 C22 . 1.507(4) ?
C18 C19 . 1.384(5) ?
C18 H18A . 0.9500 ?
C19 C20 . 1.367(5) ?
C19 H19A . 0.9500 ?
C20 C21 . 1.393(4) ?
C20 H20A . 0.9500 ?
C21 C23 . 1.504(5) ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C24 N2 . 1.165(4) y
N2 C25 . 1.398(4) ?
C25 C30 . 1.389(4) ?
C25 C26 . 1.396(4) ?
C26 C27 . 1.384(5) ?
C26 C31 . 1.499(5) ?
C27 C28 . 1.371(5) ?
C27 H27A . 0.9500 ?
C28 C29 . 1.379(5) ?
C28 H28A . 0.9500 ?
C29 C30 . 1.386(5) ?
C29 H29A . 0.9500 ?
C30 C32 . 1.496(5) ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 0.9800 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
C33 N3 . 1.181(4) y
N3 C34 . 1.382(4) ?
C34 C35 . 1.393(5) ?
C34 C39 . 1.395(5) ?
C35 C36 . 1.386(6) ?
C35 C40 . 1.494(6) ?
C36 C37 . 1.369(6) ?
C36 H36A . 0.9500 ?
C37 C38 . 1.393(6) ?
C37 H37A . 0.9500 ?
C38 C39 . 1.386(5) ?
C38 H38A . 0.9500 ?
C39 C41 . 1.505(5) ?
C40 H40B . 0.9800 ?
C40 H40C . 0.9800 ?
C40 H40D . 0.9800 ?
C41 H41B . 0.9800 ?
C41 H41C . 0.9800 ?
C41 H41D . 0.9800 ?
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
C11 C1 C2 C3 . . . . -35.8(5) ?
Fe1 C1 C2 C3 . . . . 58.2(3) ?
C11 C1 C2 Fe1 . . . . -93.9(3) ?
C1 C2 C3 C4 . . . . -1.7(4) ?
Fe1 C2 C3 C4 . . . . 59.6(3) ?
C1 C2 C3 Fe1 . . . . -61.3(3) ?
C2 C3 C4 C12 . . . . 37.7(4) ?
Fe1 C3 C4 C12 . . . . 95.6(3) ?
C2 C3 C4 Fe1 . . . . -57.9(3) ?
C13 C5 C6 C7 . . . . -0.2(5) ?
C5 C6 C7 C8 . . . . -0.3(5) ?
C6 C7 C8 C14 . . . . -0.2(5) ?
C14 C9 C11 C12 . . . . 4.3(5) ?
C14 C9 C11 C1 . . . . -174.6(3) ?
C2 C1 C11 C9 . . . . -144.3(4) ?
Fe1 C1 C11 C9 . . . . 145.5(3) ?
C2 C1 C11 C12 . . . . 36.8(4) ?
Fe1 C1 C11 C12 . . . . -33.4(3) ?
C13 C10 C12 C11 . . . . 0.7(4) ?
C13 C10 C12 C4 . . . . 176.3(3) ?
C9 C11 C12 C10 . . . . -4.2(4) ?
C1 C11 C12 C10 . . . . 174.8(3) ?
C9 C11 C12 C4 . . . . 179.8(3) ?
C1 C11 C12 C4 . . . . -1.2(4) ?
C3 C4 C12 C10 . . . . 148.6(3) ?
Fe1 C4 C12 C10 . . . . -139.5(3) ?
C3 C4 C12 C11 . . . . -35.6(4) ?
Fe1 C4 C12 C11 . . . . 36.2(3) ?
C6 C5 C13 C10 . . . . 179.4(3) ?
C6 C5 C13 C14 . . . . 1.2(5) ?
C12 C10 C13 C5 . . . . -175.7(3) ?
C12 C10 C13 C14 . . . . 2.6(4) ?
C7 C8 C14 C9 . . . . -176.2(3) ?
C7 C8 C14 C13 . . . . 1.2(5) ?
C11 C9 C14 C8 . . . . 176.3(3) ?
C11 C9 C14 C13 . . . . -1.0(5) ?
C5 C13 C14 C8 . . . . -1.6(4) ?
C10 C13 C14 C8 . . . . -179.9(3) ?
C5 C13 C14 C9 . . . . 175.8(3) ?
C10 C13 C14 C9 . . . . -2.4(4) ?
C21 C16 C17 C18 . . . . 0.8(5) ?
N1 C16 C17 C18 . . . . -179.6(3) ?
C21 C16 C17 C22 . . . . -180.0(3) ?
N1 C16 C17 C22 . . . . -0.4(5) ?
C16 C17 C18 C19 . . . . 0.0(5) ?
C22 C17 C18 C19 . . . . -179.2(3) ?
C17 C18 C19 C20 . . . . -0.3(5) ?
C18 C19 C20 C21 . . . . -0.2(5) ?
C17 C16 C21 C20 . . . . -1.3(5) ?
N1 C16 C21 C20 . . . . 179.1(3) ?
C17 C16 C21 C23 . . . . 179.2(3) ?
N1 C16 C21 C23 . . . . -0.4(5) ?
C19 C20 C21 C16 . . . . 0.9(5) ?
C19 C20 C21 C23 . . . . -179.5(3) ?
C30 C25 C26 C27 . . . . -0.2(5) ?
N2 C25 C26 C27 . . . . 178.6(3) ?
C30 C25 C26 C31 . . . . 178.4(3) ?
N2 C25 C26 C31 . . . . -2.8(5) ?
C25 C26 C27 C28 . . . . 0.6(5) ?
C31 C26 C27 C28 . . . . -177.9(4) ?
C26 C27 C28 C29 . . . . -0.6(6) ?
C27 C28 C29 C30 . . . . 0.2(6) ?
C28 C29 C30 C25 . . . . 0.1(5) ?
C28 C29 C30 C32 . . . . 179.8(3) ?
C26 C25 C30 C29 . . . . -0.2(5) ?
N2 C25 C30 C29 . . . . -179.0(3) ?
C26 C25 C30 C32 . . . . -179.8(3) ?
N2 C25 C30 C32 . . . . 1.4(5) ?
C33 N3 C34 C35 . . . . 2.0(15) ?
C33 N3 C34 C39 . . . . -177.6(13) ?
N3 C34 C35 C36 . . . . -176.0(3) ?
C39 C34 C35 C36 . . . . 3.6(5) ?
N3 C34 C35 C40 . . . . 4.2(5) ?
C39 C34 C35 C40 . . . . -176.2(3) ?
C34 C35 C36 C37 . . . . -0.1(5) ?
C40 C35 C36 C37 . . . . 179.7(4) ?
C35 C36 C37 C38 . . . . -2.2(6) ?
C36 C37 C38 C39 . . . . 1.1(6) ?
C37 C38 C39 C34 . . . . 2.2(5) ?
C37 C38 C39 C41 . . . . -176.7(3) ?
N3 C34 C39 C38 . . . . 175.0(3) ?
C35 C34 C39 C38 . . . . -4.6(5) ?
N3 C34 C39 C41 . . . . -6.2(5) ?
C35 C34 C39 C41 . . . . 174.2(3) ?
_cod_database_fobs_code 2243951