#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/25/2102555.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_2102555 loop_ _publ_author_name 'du Boulay, D.' 'Ishizawa, N.' 'Atake, T.' 'Streltsov, V.' 'Furuya, K.' 'Munakata, F.' _publ_section_title ; Synchrotron X-ray and ab initio studies of \b-Si~3~N~4~ ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 388 _journal_page_last 405 _journal_volume 60 _journal_year 2004 _chemical_formula_moiety 'N4 Si3' _chemical_formula_sum 'N4 Si3' _chemical_formula_weight 140.31 _chemical_name_common '%b silicon nitride' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall p_6c _symmetry_space_group_name_H-M P_63 _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 120.0000 _cell_formula_units_Z 1.5 _cell_length_a 7.6020(2) _cell_length_b 7.6020(2) _cell_length_c 2.90600(10) _cell_measurement_reflns_used 12 _cell_measurement_temperature 150 _cell_measurement_theta_max 56.03 _cell_measurement_theta_min 52.34 _cell_volume 145.439(9) _computing_cell_refinement 'xtal3.7 LATCON' _computing_data_collection 'Diff14A, Vaalsta & Hester 1997' _computing_data_reduction 'xtal DIFDAT SORTRF ABSORB ADDREF' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' _computing_structure_refinement 'xtal CRYLSQ' _computing_structure_solution 'already known structure' _diffrn_ambient_temperature 295 _diffrn_measured_fraction_theta_full 1.0 _diffrn_measurement_device_type PF-BL14A_Rigaku_4circle _diffrn_measurement_method %w/2%q _diffrn_radiation_monochromator 'Double Si ' _diffrn_radiation_source Synchrotron _diffrn_radiation_type 'syn x' _diffrn_radiation_wavelength .75037 _diffrn_reflns_av_R_equivalents .027 _diffrn_reflns_av_sigmaI/netI .012 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 8549 _diffrn_reflns_reduction_process 'equatorial monochr Lp' _diffrn_reflns_theta_full 60 _diffrn_reflns_theta_max 65.05 _diffrn_reflns_theta_min 3.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 6 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_T_max .9719 _exptl_absorpt_correction_T_min .9319 _exptl_absorpt_correction_type analytical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.204 _exptl_crystal_description irregular _exptl_crystal_F_000 140 _exptl_crystal_size_max .0352 _exptl_crystal_size_mid .0250 _exptl_crystal_size_min .0185 _refine_diff_density_max .442 _refine_diff_density_min -.435 _refine_ls_abs_structure_details 'see text' _refine_ls_extinction_coef 4E2(5) _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_extinction_method Zachariasen _refine_ls_goodness_of_fit_all 1.841 _refine_ls_goodness_of_fit_ref 1.841 _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 22 _refine_ls_number_reflns 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .0149 _refine_ls_R_factor_gt .0149 _refine_ls_shift/su_max .00059 _refine_ls_shift/su_mean .00006 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all .0136 _refine_ls_wR_factor_ref .0136 _reflns_number_gt 787 _reflns_number_total 800 _reflns_threshold_expression 'F > .00 sig(F )' _[local]_cod_data_source_file av5009.cif loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,1/2+z -y,+x-y,+z +y,-x+y,1/2+z -x+y,-x,+z +x-y,+x,1/2+z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si .079775 .078978 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N .005011 .003704 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _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_occupancy Si .76847(2) .17453(2) .25000 .00246(4) Uani 1.00000 N1 .03054(5) .33023(6) .2459(6) .00343(7) Uani 1.00000 N2 .66666 .33333 .2502(17) .00338(10) Uani 1.00000 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 Si .00268(4) .00254(4) .00209(4) .00126(3) .0001(2) -.0002(2) N1 .00287(8) .00428(9) .00252(9) .00133(7) .0000(4) .0009(4) N2 .00304(8) .00304(8) .00406(14) .00152(4) .00000 .00000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Si N2 . 1.72936(14) Si N1 '1 655' 1.7355(4) Si N1 '6 654' 1.7451(15) Si N1 '6 655' 1.7252(15) 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 N2 Si N1 . '1 655' 106.602(18) N2 Si N1 . '6 654' 110.00(15) N2 Si N1 . '6 655' 110.20(15) N1 Si N1 '1 655' '6 654' 107.56(6) N1 Si N1 '1 655' '6 655' 108.46(6) N1 Si N1 '6 654' '6 655' 113.73(5) Si N1 Si '1 455' '4 564' 123.63(9) Si N1 Si '1 455' '4 565' 122.42(9) Si N1 Si '4 564' '4 565' 113.73(2) Si N2 Si . '3 655' 119.997(7) Si N2 Si . '5 665' 120.002(6) Si N2 Si '3 655' '5 665' 120.001(8) _cod_database_code 2102555 _journal_paper_doi 10.1107/S010876810401393X