#------------------------------------------------------------------------------
#$Date: 2018-09-08 05:01:15 +0300 (Sat, 08 Sep 2018) $
#$Revision: 210555 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/26/2242624.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_2242624
loop_
_publ_author_name
'Bykov, Maxim'
'Khandarkhaeva, Saiana'
'Fedotenko, Timofey'
'Sedmak, Pavel'
'Dubrovinskaia, Natalia'
'Dubrovinsky, Leonid'
_publ_section_title
;
Synthesis of FeN~4~ at 180GPa and its crystal structure from a
submicron-sized grain
;
_journal_coeditor_code WM5459
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1392
_journal_page_last 1395
_journal_paper_doi 10.1107/S2056989018012161
_journal_volume 74
_journal_year 2018
_chemical_formula_iupac 'Fe N4'
_chemical_formula_moiety 'Fe N4'
_chemical_formula_sum 'Fe N4'
_chemical_formula_weight 111.89
_chemical_name_systematic 'Iron tetranitride'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 105.22(4)
_cell_angle_beta 110.60(4)
_cell_angle_gamma 91.39(3)
_cell_formula_units_Z 1
_cell_length_a 2.4473(10)
_cell_length_b 3.4688(14)
_cell_length_c 3.5144(13)
_cell_measurement_reflns_used 68
_cell_measurement_temperature 293
_cell_measurement_theta_max 16.0560
_cell_measurement_theta_min 2.8210
_cell_volume 26.72(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.341
_diffrn_measured_fraction_theta_max 0.212
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type 'ID11 @ ESRF'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator synchrotron
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.30996
_diffrn_reflns_av_R_equivalents 0.0201
_diffrn_reflns_limit_h_max 3
_diffrn_reflns_limit_h_min -3
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_number 117
_diffrn_reflns_theta_full 10.718
_diffrn_reflns_theta_max 16.226
_diffrn_reflns_theta_min 2.821
_exptl_absorpt_coefficient_mu 1.332
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96678
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSPACK; Oxford Diffraction, 2005)
;
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 6.953
_exptl_crystal_description irregular
_exptl_crystal_F_000 54
_exptl_crystal_size_max 0.0005
_exptl_crystal_size_mid 0.0005
_exptl_crystal_size_min 0.0005
_refine_diff_density_max 0.757
_refine_diff_density_min -0.557
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.183
_refine_ls_hydrogen_treatment undef
_refine_ls_matrix_type full
_refine_ls_number_parameters 10
_refine_ls_number_reflns 71
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.183
_refine_ls_R_factor_all 0.0413
_refine_ls_R_factor_gt 0.0403
_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^)+(0.0282P)^2^+0.3122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0813
_refine_ls_wR_factor_ref 0.0815
_reflns_number_gt 70
_reflns_number_total 71
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5459sup1.cif
_cod_data_source_block I
_cod_database_code 2242624
_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 0.999
_shelx_estimated_absorpt_t_max 0.999
_shelx_hkl_file
;
0 0 -118982.80 55.28 1
0 0 118990.10 51.21 1
0 0 224721.60 113.75 1
0 0 -224741.00 111.57 1
0 0 -3 753.26 157.61 1
0 0 3 1239.28 160.48 1
0 0 -4 3353.63 191.61 1
0 0 4 3942.28 199.40 1
0 1 -4 3171.09 197.91 1
0 -1 4 2955.25 198.12 1
0 -1 311242.60 151.39 1
0 1 -311162.30 160.19 1
0 1 -2 1995.20 95.79 1
0 -1 2 1927.82 91.93 1
0 1 -118481.30 59.10 1
0 -1 118472.50 56.64 1
0 -2 4 5452.57 190.83 1
0 2 -4 4872.97 198.39 1
0 2 -311744.40 152.61 1
0 -2 311815.90 157.51 1
0 2 -215353.80 130.62 1
0 -2 215340.30 107.78 1
0 -3 4 2383.74 208.99 1
0 3 -4 2704.96 221.23 1
0 -3 3 1390.78 160.86 1
-1 2 -3 4041.08 214.59 1
1 -2 3 4312.65 187.81 1
1 -2 4 478.47 206.48 1
-1 2 -4 724.63 222.47 1
-1 1 -219245.40 153.23 1
1 -1 219175.30 152.99 1
-1 1 -3 1703.55 173.56 1
1 -1 3 1187.46 174.10 1
1 -1 4 1849.58 216.11 1
-1 1 -4 1687.52 217.29 1
-1 0 -116176.70 94.48 1
1 0 116157.00 97.22 1
1 0 2 8778.58 142.15 1
-1 0 -2 8730.49 155.15 1
1 0 3 8819.88 195.53 1
-1 0 -3 8640.17 206.26 1
1 1 -4 3868.20 158.45 1
-1 -1 312557.20 136.68 1
1 1 -312620.10 127.73 1
1 1 -222314.10 76.85 1
1 1 010393.10 57.12 1
-1 -1 010404.20 56.22 1
1 1 1 8286.35 109.53 1
-1 -1 -1 8266.74 102.92 1
1 1 2 1385.87 161.19 1
-1 -1 -2 1484.65 140.60 1
-1 -1 -3 3729.82 197.94 1
1 2 -5 868.86 256.44 1
-1 -2 5 3366.88 266.95 1
-1 -2 4 4780.27 174.78 1
1 2 -4 4912.60 163.82 1
-1 -2 3 1083.77 124.56 1
1 2 -3 1098.12 122.55 1
1 2 -214444.10 91.37 1
-1 -3 5 5258.94 217.24 1
1 3 -5 5695.45 212.14 1
1 3 -4 3410.71 184.28 1
-1 -3 4 3447.61 163.79 1
-1 -3 3 9900.94 143.17 1
-1 -4 5 885.55 228.94 1
1 4 -5 292.96 248.00 1
-1 -4 4 2732.20 198.34 1
-1 -5 5 229.05 252.75 1
2 -1 2 2444.65 198.26 1
-2 1 -2 2860.13 226.94 1
-2 1 -3 3281.31 246.52 1
2 -1 3 3761.21 210.09 1
2 0 1 6810.64 155.68 1
-2 0 -1 6620.08 176.78 1
2 0 2 797.63 170.57 1
-2 0 -2 547.27 181.38 1
2 0 3 1343.11 227.35 1
-2 0 -3 1375.33 207.89 1
2 1 -1 2431.16 70.48 1
-2 -1 014779.90 135.44 1
2 1 014766.70 113.62 1
2 1 1 4460.44 157.93 1
-2 -1 -1 4860.83 152.45 1
2 1 2 8302.76 194.13 1
-2 -1 -2 8240.54 197.91 1
2 1 3 783.79 232.71 1
-2 -1 -3 415.12 240.90 1
2 2 -5 5103.39 198.05 1
2 2 -4 3671.24 146.23 1
2 2 -312508.50 104.64 1
-2 -2 0 1113.77 119.77 1
-2 -2 -1 3820.58 168.19 1
-2 -2 -2 1907.72 214.34 1
2 3 -6 1020.29 237.00 1
-2 -3 5 561.52 201.58 1
2 3 -5 551.14 184.73 1
2 3 -4 1280.87 158.28 1
-2 -3 4 1243.06 154.09 1
-2 -3 1 7361.08 88.64 1
-2 -3 0 3780.33 136.61 1
2 4 -5 908.43 227.97 1
3 -1 2 575.02 227.34 1
3 0 1 1372.33 213.79 1
3 0 2 4035.68 241.97 1
-3 0 -2 3880.46 283.24 1
3 1 -1 5133.13 125.12 1
3 1 0 697.12 167.50 1
3 1 1 1711.29 188.11 1
-3 -1 -1 1377.83 237.24 1
3 1 2 309.07 255.27 1
-3 -1 -2 707.62 306.97 1
3 2 -3 1609.91 84.99 1
3 2 -1 4701.17 114.50 1
3 2 0 3149.38 168.13 1
-3 -2 0 2909.66 189.82 1
3 2 1 2067.00 217.68 1
-3 -2 -1 2294.56 216.07 1
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 44141
_shelx_res_file
;
fen2_s5_1.res created by SHELXL-2014/7
TITL FeN2_s5_1
CELL 0.30996 2.4473 3.4688 3.5144 105.224 110.601 91.389
ZERR 1 0.001042 0.001418 0.001334 0.0358 0.038 0.0339
LATT 1
SFAC Fe N
DISP Fe 0.1197 0.1747 334.09
DISP N -0.001 0.0005 5.44
UNIT 1 4
L.S. 4 0 0
PLAN 20
SIZE 0.0005 0.0005 0.0005
TEMP 19.85
fmap 2 53
acta
REM
REM
REM
WGHT 0.028200 0.312200
FVAR 7.74906
FE 1 0.500000 0.000000 0.000000 10.50000 0.00715
N1 2 0.162800 -0.345749 -0.485063 11.00000 0.00655
N2 2 0.065462 -0.309431 -0.860854 11.00000 0.00676
HKLF 4
REM FeN2_s5_1
REM R1 = 0.0403 for 70 Fo > 4sig(Fo) and 0.0413 for all 71 data
REM 10 parameters refined using 0 restraints
END
WGHT 0.0267 0.3423
REM Highest difference peak 0.757, deepest hole -0.557, 1-sigma level 0.174
Q1 1 0.2353 -0.2024 -0.9206 11.00000 0.05 0.76
Q2 1 0.6611 -0.1308 0.0128 11.00000 0.05 0.56
Q3 1 0.2155 -0.1088 -0.3186 11.00000 0.05 0.47
Q4 1 0.1951 0.0572 -0.2812 11.00000 0.05 0.42
Q5 1 -0.0579 -0.5811 -0.7992 11.00000 0.05 0.40
Q6 1 0.3625 -0.2532 -0.1673 11.00000 0.05 0.38
Q7 1 -0.0813 -0.0199 -0.4410 11.00000 0.05 0.36
Q8 1 0.0749 -0.0437 -0.0977 11.00000 0.05 0.32
Q9 1 0.5329 -0.3647 -0.3377 11.00000 0.05 0.29
Q10 1 0.5759 -0.1226 -0.4171 11.00000 0.05 0.29
Q11 1 0.5211 -0.1875 0.1640 11.00000 0.05 0.26
Q12 1 -0.0083 -0.2389 -0.5368 11.00000 0.05 0.25
Q13 1 0.2563 -0.4610 -0.8208 11.00000 0.05 0.22
Q14 1 -0.1651 -0.1574 -0.3001 11.00000 0.05 0.20
Q15 1 -0.0646 -0.3248 -0.3973 11.00000 0.05 0.18
Q16 1 0.4427 -0.3443 -0.6965 11.00000 0.05 0.16
Q17 1 0.7143 -0.1685 -0.2151 11.00000 0.05 0.11
;
_shelx_res_checksum 24567
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Fe Fe 0.5000 0.0000 0.0000 0.0072(4) Uiso d 1
N N1 0.163(4) -0.346(4) -0.485(2) 0.0066(10) Uiso d 1
N N2 0.065(3) -0.309(4) -0.861(2) 0.0068(10) Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.1197 0.1747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0010 0.0005 '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
Fe Fe Fe 1_655 1_455 180.0
N1 Fe Fe . 1_655 96.6(4)
N1 Fe Fe 2_655 1_455 96.6(4)
N1 Fe Fe . 1_455 83.4(4)
N1 Fe Fe 2_655 1_655 83.4(4)
N1 Fe N1 2_655 . 180.0
N1 Fe N2 . 1_556 81.3(4)
N1 Fe N2 2_655 1_556 98.7(4)
N1 Fe N2 2_655 2_654 81.3(4)
N1 Fe N2 . 2_654 98.7(4)
N1 Fe N2 . 1_656 90.5(5)
N1 Fe N2 . 2_554 89.5(5)
N1 Fe N2 2_655 2_554 90.5(5)
N1 Fe N2 2_655 1_656 89.5(5)
N2 Fe Fe 2_654 1_655 46.7(5)
N2 Fe Fe 2_654 1_455 133.3(5)
N2 Fe Fe 1_556 1_655 133.3(5)
N2 Fe Fe 2_554 1_455 46.02(18)
N2 Fe Fe 2_554 1_655 133.98(18)
N2 Fe Fe 1_556 1_455 46.7(5)
N2 Fe Fe 1_656 1_455 133.98(18)
N2 Fe Fe 1_656 1_655 46.02(18)
N2 Fe N2 1_556 2_554 92.7(5)
N2 Fe N2 2_654 2_554 87.3(5)
N2 Fe N2 2_554 1_656 180.0(7)
N2 Fe N2 1_556 1_656 87.3(5)
N2 Fe N2 2_654 1_656 92.7(5)
N2 Fe N2 2_654 1_556 180.0
N1 N1 Fe 2_544 . 118.9(9)
N1 N1 N2 2_544 . 109.6(9)
N2 N1 Fe . . 129.4(9)
Fe N2 Fe 1_554 1_454 87.3(5)
N1 N2 Fe . 1_454 110.9(12)
N1 N2 Fe . 1_554 126.9(5)
N1 N2 N2 . 2_543 107.6(12)
N2 N2 Fe 2_543 1_454 113.1(6)
N2 N2 Fe 2_543 1_554 109.9(9)
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
Fe Fe 1_655 2.4473(10) no
Fe Fe 1_455 2.4473(10) ?
Fe N1 . 1.707(10) yes
Fe N1 2_655 1.707(10) yes
Fe N2 1_656 1.783(14) yes
Fe N2 2_554 1.783(14) yes
Fe N2 2_654 1.763(6) yes
Fe N2 1_556 1.763(6) yes
N1 N1 2_544 1.277(14) yes
N1 N2 . 1.298(8) yes
N2 Fe 1_554 1.763(6) ?
N2 Fe 1_454 1.783(14) ?
N2 N2 2_543 1.37(3) yes
_cod_database_fobs_code 2242624