#------------------------------------------------------------------------------
#$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 FeN₄ 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       'ω 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/[σ²(Fo²)+(0.0282P)²+0.3122P] where P=(Fo²+2Fc²)/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 > 2σ(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
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
