#------------------------------------------------------------------------------ #$Date: 2023-09-20 04:48:56 +0300 (Wed, 20 Sep 2023) $ #$Revision: 286429 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022864.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_2022864 loop_ _publ_author_name 'Jurzick, Pascal L.' 'Krach, Georg' 'Br\"uning, Lukas' 'Schnick, Wolfgang' 'Bykov, Maxim' _publ_section_title ; Synthesis and crystal structure of silicon pernitride SiN2 at 140 GPa ; _journal_coeditor_code WM5694 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989023008058 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'Si N2' _chemical_formula_moiety 'N2 Si' _chemical_formula_sum 'N2 Si' _chemical_formula_weight 56.11 _chemical_name_systematic 'Silicon pernitride' _space_group_crystal_system cubic _space_group_IT_number 205 _space_group_name_Hall '-P 2ac 2ab 3' _space_group_name_H-M_alt 'P a -3' _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.1205(5) _cell_length_b 4.1205(5) _cell_length_c 4.1205(5) _cell_measurement_reflns_used 79 _cell_measurement_temperature 293 _cell_measurement_theta_max 16.4030 _cell_measurement_theta_min 3.4280 _cell_volume 69.960(15) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2023) ; _computing_molecular_graphics ; VESTA (Momma & Izumi, 2011) ; _computing_publication_material ; Olex2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 5.0 _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.732 _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'customized \w-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.28457 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_unetI/netI 0.0531 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 269 _diffrn_reflns_theta_full 9.831 _diffrn_reflns_theta_max 18.450 _diffrn_reflns_theta_min 3.429 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 5.327 _exptl_crystal_description irregular _exptl_crystal_F_000 112 _exptl_crystal_size_max 0.001 _exptl_crystal_size_mid 0.001 _exptl_crystal_size_min 0.001 _refine_diff_density_max 1.079 _refine_diff_density_min -1.146 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 6 _refine_ls_number_reflns 101 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.1285 _refine_ls_R_factor_gt 0.0706 _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^)+(0.1090P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1601 _refine_ls_wR_factor_ref 0.1907 _reflns_number_gt 60 _reflns_number_total 101 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5694sup1.cif _cod_data_source_block I _cod_original_cell_volume 69.96(3) _cod_database_code 2022864 _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 1.000 _shelx_estimated_absorpt_t_max 1.000 _shelx_hkl_file ; 0 0 -1 4.18 4.79 0 1 -1 0.37 6.14 0 -1 1 -1.65 6.68 -1 -1 1 1871.53 17.13 1 1 -1 1871.34 16.37 0 0 2 9927.42 37.67 0 0 -2 9999.00 34.70 0 1 2 2.71 12.53 0 -1 2 -7.23 14.25 0 1 -2 3.10 13.93 0 -1 -2 4.83 9.95 -1 0 2 1522.70 20.57 1 0 -2 1539.43 19.23 0 -2 1 1552.51 16.14 -1 1 2 889.51 17.80 1 2 -1 964.93 14.76 1 -1 -2 875.60 16.84 -1 -2 1 975.11 16.34 -1 -1 2 945.79 22.06 0 -2 2 4809.14 32.19 0 2 -2 4782.63 33.42 -1 -2 2 104.06 20.90 1 2 -2 82.25 16.47 -1 2 2 106.23 14.61 1 -2 -2 103.51 14.24 -2 -1 2 83.70 16.69 -2 -2 2 4107.14 37.49 2 2 -2 4121.01 35.99 0 0 -3 8.67 18.58 0 3 0 -4.43 7.42 0 0 3 9.26 21.79 0 -1 -3 8.04 18.15 0 -1 3 13.03 23.68 -1 -3 0 10.47 10.89 0 -2 3 1027.12 30.04 0 2 -3 1012.83 28.52 1 0 -3 17.79 19.63 -1 0 3 28.23 24.70 0 3 -1 7.64 15.25 -1 -3 1 5578.61 32.25 -1 -1 3 5618.96 51.83 -1 1 3 5384.80 41.40 1 3 -1 5520.31 27.79 1 -1 -3 5406.48 41.52 -1 -2 3 21.94 24.12 -1 2 3 19.93 18.29 1 -2 -3 3.62 18.73 1 2 -3 1.55 22.23 0 -3 2 23.56 20.21 0 3 -2 -7.01 23.57 2 0 -3 5.67 22.06 0 -3 -2 -7.19 11.86 -2 0 3 4.86 28.63 -2 1 3 727.04 32.08 -2 -1 3 730.85 29.22 -1 3 2 796.63 16.19 1 3 -2 869.76 22.76 -1 -3 2 841.40 28.00 2 -1 -3 671.55 30.35 2 3 -2 128.65 23.38 2 2 -3 89.74 23.21 -2 -3 2 113.49 28.66 -2 2 3 78.79 24.61 -2 -2 3 69.18 28.35 0 3 -3 -20.60 29.98 -1 -3 3 1865.80 33.75 -1 3 3 2028.37 23.67 2 3 -3 54.97 23.72 -2 -3 3 35.96 32.59 -2 3 3 72.67 19.70 -3 -3 3 1675.35 38.02 0 4 0 690.48 10.09 0 0 -4 595.36 29.74 0 1 -4 -25.97 27.25 0 -1 -4 -1.21 25.37 0 -2 -4 1259.26 28.67 0 2 -4 1190.03 34.32 0 -3 -4 8.51 25.47 0 3 -4 -2.49 36.47 -1 0 4 180.98 27.67 1 0 -4 128.90 30.60 0 4 -1 148.53 17.37 -1 1 4 79.40 26.49 1 -1 -4 102.43 28.76 1 1 -4 138.06 29.05 1 -2 -4 -11.35 28.86 1 2 -4 5.26 32.38 -1 -2 4 72.79 27.71 -1 2 4 21.98 22.46 -2 -4 1 3.18 19.49 1 -3 -4 136.99 24.13 1 3 -4 144.53 33.51 -1 3 4 124.55 24.65 -1 -3 4 121.14 32.70 2 0 -4 1606.67 35.64 -2 0 4 1618.71 40.54 2 1 -4 150.71 30.25 -2 1 4 121.04 31.70 2 -1 -4 142.49 26.82 -1 4 2 129.56 11.24 -1 -4 2 129.74 23.38 -2 2 4 1539.09 36.08 2 -2 -4 1543.85 32.51 2 3 -4 280.64 31.51 2 -3 -4 362.05 31.68 -2 -3 4 318.84 40.79 -3 0 4 271.67 38.98 3 0 -4 240.68 36.22 0 -4 -3 312.66 17.85 -1 4 3 23.14 15.53 -1 -4 3 18.16 23.92 1 4 -3 -7.57 29.57 3 1 -4 57.46 35.88 -3 1 4 12.47 34.05 -2 -4 3 8.31 33.16 -3 2 4 21.07 32.62 2 4 -3 73.47 25.55 3 2 -4 68.28 36.75 -2 4 3 59.30 20.60 -3 -2 4 65.52 41.32 3 3 -4 -15.84 36.78 -3 -3 4 60.13 39.21 -3 -4 3 19.89 31.57 0 -4 -4 1864.21 29.30 1 -4 -4 8.82 20.49 -1 4 4 55.53 23.99 1 4 -4 95.65 31.52 -1 -4 4 33.71 34.84 2 4 -4 1320.24 36.14 -2 4 4 1406.48 32.60 -3 -4 4 148.49 44.75 3 4 -4 148.07 37.51 -3 4 4 72.24 23.77 -1 -5 0 -2.07 17.13 0 -2 -5 41.93 34.52 0 -4 -5 28.83 28.29 1 0 -5 61.02 33.19 -1 0 5 0.41 33.39 0 5 -1 23.59 18.39 1 -1 -5 3024.31 48.89 -1 -1 5 2952.84 48.51 -1 1 5 2989.73 46.67 1 1 -5 2986.18 49.21 -1 -5 1 3127.09 27.57 1 -2 -5 271.06 31.16 1 2 -5 161.10 36.66 -1 -2 5 120.95 39.07 -2 -5 1 217.39 26.91 1 -3 -5 670.58 31.28 -1 3 5 560.47 31.29 -1 -3 5 574.93 39.42 1 3 -5 593.95 44.14 -1 -4 5 51.39 40.49 1 4 -5 128.01 38.63 1 -4 -5 36.98 26.33 0 5 -2 57.22 23.87 2 0 -5 25.11 33.49 -2 0 5 -31.86 41.59 2 1 -5 14.80 34.36 -1 -5 2 29.90 23.14 2 -1 -5 -2.83 33.32 -2 -1 5 -13.84 35.99 -2 1 5 8.56 40.16 -2 -5 2 29.19 29.52 2 2 -5 -9.60 35.65 -2 -2 5 5.66 37.89 -2 2 5 -14.52 30.21 2 -2 -5 38.76 30.94 2 -3 -5 9.50 29.88 2 3 -5 32.17 35.52 -2 3 5 -19.68 29.96 -2 -3 5 -9.69 41.26 2 4 -5 1.30 39.12 -2 4 5 -12.92 24.19 -2 -4 5 47.15 40.32 -3 0 5 23.25 42.11 3 0 -5 -15.83 36.99 0 -5 -3 -6.34 10.95 -3 -1 5 771.46 47.81 -3 1 5 752.21 43.39 3 2 -5 378.18 37.32 -2 -5 3 423.27 39.12 -2 5 3 355.61 19.00 -3 -2 5 377.67 48.67 -3 2 5 345.66 38.65 3 3 -5 689.48 41.76 -3 -3 5 888.26 52.81 -3 3 5 767.15 38.24 -3 -5 3 911.26 42.40 -3 4 5 98.16 31.67 -3 -4 5 87.20 51.41 0 5 -4 -2.69 36.12 0 -5 -4 4.98 17.39 1 5 -4 -39.19 37.53 2 5 -4 56.23 30.85 -2 5 4 3.08 20.57 -3 5 4 49.62 23.20 3 5 -4 58.36 36.37 0 -5 -5 -31.56 21.82 1 5 -5 25.62 43.30 1 -5 -5 -34.84 22.72 -2 5 5 50.23 27.06 2 5 -5 56.88 38.22 3 5 -5 498.53 43.64 -3 5 5 465.47 33.65 -1 6 0 -1.28 13.66 -1 -6 0 7.30 12.87 -2 -6 0 471.43 23.22 0 -5 -6 -15.79 25.24 1 0 -6 95.99 41.45 -1 0 6 3.68 36.65 0 6 -1 35.96 16.37 1 1 -6 17.11 40.73 -1 1 6 52.26 38.61 -1 -6 1 26.21 18.17 -1 -1 6 10.82 38.54 1 -1 -6 32.23 42.58 -2 -6 1 -7.38 25.02 -1 2 6 -18.79 38.78 -1 -2 6 14.91 43.08 -1 -3 6 49.37 45.65 1 3 -6 97.46 50.24 1 -3 -6 38.66 38.37 1 -4 -6 19.56 29.90 1 4 -6 1.00 49.10 1 5 -6 106.21 41.65 1 -5 -6 18.89 25.77 0 6 -2 434.26 23.09 -2 0 6 326.93 41.38 2 1 -6 69.77 51.31 -1 -6 2 57.95 23.97 2 -1 -6 46.45 36.58 1 6 -2 87.98 20.05 -2 1 6 93.96 38.31 -2 -1 6 120.17 50.52 -2 2 6 419.39 34.35 -2 -2 6 437.83 42.12 -2 -6 2 541.52 29.00 2 -3 -6 164.52 32.97 2 3 -6 116.65 43.58 -2 3 6 185.10 35.34 -2 -3 6 160.14 40.84 -3 -6 2 183.45 31.85 2 4 -6 516.02 47.85 2 -4 -6 497.31 35.62 -2 4 6 426.61 35.45 -2 5 6 33.98 32.03 0 6 -3 52.52 27.62 3 0 -6 41.90 39.73 -3 0 6 118.11 48.25 -1 -6 -3 10.89 10.04 3 -1 -6 -0.64 40.15 -1 -6 3 -29.89 30.10 3 1 -6 12.60 39.48 1 6 -3 0.14 26.19 -3 -1 6 -10.37 50.76 -3 1 6 11.97 47.00 -2 -6 3 17.36 30.61 -3 2 6 -19.73 45.13 2 6 -3 -9.52 29.54 -3 -6 3 -58.83 38.79 3 3 -6 59.08 40.38 -3 3 6 2.56 41.79 -3 4 6 57.14 33.59 -3 5 6 -11.81 28.63 0 6 -4 972.94 38.52 1 6 -4 45.10 31.95 4 1 -6 2.60 49.23 -4 1 6 40.00 44.40 -1 -6 4 31.13 37.20 2 6 -4 396.03 32.31 -2 -6 4 504.28 40.18 -4 2 6 470.81 43.88 -3 -6 4 64.39 49.09 1 6 -5 28.23 37.27 -2 -6 5 68.18 42.91 2 6 -5 31.06 35.27 3 6 -5 -32.63 45.01 -2 -7 0 288.71 22.21 -1 0 7 41.20 47.78 1 0 -7 34.28 48.30 0 7 -1 10.08 15.06 -1 1 7 428.43 49.97 -2 -7 -1 17.31 14.92 1 -2 -7 19.35 39.07 -2 -7 1 -1.93 22.38 1 -3 -7 262.92 44.65 1 -4 -7 -8.09 33.89 0 7 -2 2.67 21.53 2 -1 -7 92.88 44.12 -2 1 7 184.43 47.77 -2 -7 2 43.18 23.68 2 -2 -7 -19.74 42.83 -3 -7 2 36.95 32.22 -2 3 7 2.92 36.73 2 -3 -7 -12.45 35.91 -2 4 7 10.72 38.26 2 -4 -7 11.96 34.06 0 7 -3 16.69 31.75 1 7 -3 203.22 25.84 3 -1 -7 136.20 41.91 3 -2 -7 14.67 42.57 -2 -7 3 7.76 32.63 3 -3 -7 171.93 45.62 -3 3 7 187.67 39.87 -3 -7 3 240.56 35.49 -3 4 7 -14.66 31.92 1 7 -4 8.76 32.24 -2 -7 4 38.47 35.08 2 7 -4 122.53 32.76 -3 -7 4 68.50 38.53 1 7 -5 103.52 37.67 2 7 -5 6.30 35.17 1 -3 -8 14.35 37.42 2 -4 -8 75.05 36.76 1 8 -3 -35.87 26.09 1 8 -4 6.60 29.04 2 8 -4 142.25 34.21 0 0 0 0.00 0.00 _shelx_res_file ; _shelx_hkl_checksum 28902 _shelx_res_file {26c6c36b-09aa-4389-a52a-17eac477c28c _shelx_res_checksum 52692 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-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 Si Si1 0.5000 0.5000 0.5000 0.0084(5) Uani d 1 . . N N1 0.5982(5) 0.4018(5) 0.9018(5) 0.0076(6) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si1 0.0084(5) 0.0084(5) 0.0084(5) -0.0005(3) -0.0005(3) -0.0005(3) N1 0.0076(6) 0.0076(6) 0.0076(6) 0.0012(8) 0.0012(8) -0.0012(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N -0.0013 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0075 0.0103 '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 Si1 N1 . 15_565 86.94(4) ? N1 Si1 N1 13_666 14_557 93.06(4) ? N1 Si1 N1 2_664 3_656 93.06(4) ? N1 Si1 N1 . 13_666 180.0 ? N1 Si1 N1 15_565 3_656 180.00(14) ? N1 Si1 N1 15_565 13_666 93.06(4) ? N1 Si1 N1 15_565 14_557 93.06(4) ? N1 Si1 N1 . 2_664 93.06(4) ? N1 Si1 N1 2_664 14_557 180.0 ? N1 Si1 N1 15_565 2_664 86.94(4) ? N1 Si1 N1 13_666 3_656 86.94(4) ? N1 Si1 N1 13_666 2_664 86.94(4) ? N1 Si1 N1 14_557 3_656 86.94(4) ? N1 Si1 N1 . 14_557 86.94(4) ? N1 Si1 N1 . 3_656 93.06(4) ? Si1 N1 Si1 . 3_646 112.54(10) ? Si1 N1 Si1 2_665 3_646 112.54(10) ? Si1 N1 Si1 2_665 . 112.54(10) ? N1 N1 Si1 13_667 3_646 106.20(12) ? N1 N1 Si1 13_667 2_665 106.20(12) ? N1 N1 Si1 13_667 . 106.20(12) ? 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 Si1 N1 . 1.7517(11) ? Si1 N1 3_656 1.7517(11) ? Si1 N1 2_664 1.7517(11) ? Si1 N1 15_565 1.7517(11) ? Si1 N1 13_666 1.7517(11) ? Si1 N1 14_557 1.7517(11) ? N1 Si1 3_646 1.7517(11) ? N1 Si1 2_665 1.7517(11) ? N1 N1 13_667 1.402(8) ? 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 N1 Si1 N1 Si1 15_565 . . 2_665 94.59(6) ? N1 Si1 N1 Si1 15_565 . . 3_646 -33.8(3) ? N1 Si1 N1 Si1 14_557 . . 3_646 59.4(2) ? N1 Si1 N1 Si1 3_656 . . 3_646 146.2(3) ? N1 Si1 N1 Si1 2_664 . . 3_646 -120.6(2) ? N1 Si1 N1 Si1 14_557 . . 2_665 -172.18(11) ? N1 Si1 N1 Si1 3_656 . . 2_665 -85.41(6) ? N1 Si1 N1 Si1 2_664 . . 2_665 7.82(11) ? N1 Si1 N1 N1 15_565 . . 13_667 -149.62(10) ? N1 Si1 N1 N1 14_557 . . 13_667 -56.39(6) ? N1 Si1 N1 N1 3_656 . . 13_667 30.38(10) ? N1 Si1 N1 N1 2_664 . . 13_667 123.61(6) ? _cod_database_fobs_code 2022864