# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Xiaoming Wang' ; College of Chemistry and Molecular Engineering Peaking University, Beijing 100871 China ; 'Chun-Hai Wang' ; College of Chemistry and Molecular Engineering Peaking University, Beijing 100871 China ; 'Meimei Wu' ; China Institute of Atomic Energy, Beijing 102413 China National Institute of Standards and Technology Gaithersburg, MD20899 USA ; 'Yingxia Wang' ; College of Chemistry and Molecular Engineering Peaking University, Beijing 100871 China ; 'Xiping Jing' ; College of Chemistry and Molecular Engineering Peaking University, Beijing 100871 China ; _publ_contact_author_address # Address of author for correspondence ; College of Chemistry and Molecular Engineering Peaking University, Beijing 100871 China ; _publ_contact_author_email xpjing@pku.edu.cn _publ_contact_author_fax '86 10 6275 1708' _publ_contact_author_phone '86 10 6275 4188' #TrackingRef '- CaSiNO.cif' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr X. P. Jing' _publ_contact_letter ; ? ; _publ_requested_category ? #============================================================================== # 2.TITLE AND AUTHOR LIST _publ_section_title ; Title (type -US>Mullite-type Ca~3~Si~2~O~4~N~2~) ; data_C _database_code_depnum_ccdc_archive 'CCDC 838658' _publ_section_title_footnote . #============================================================================== # 3.TEXT _publ_section_synopsis ; The structure of Ca~3~Si~2~O~4~N~2~is solved from powder X-ray diffraction data and refined by Rietveld analysis. ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; 6 mmol Ca~C~O~3~, 1 mmol Si~3~N~4~, and 1mmol Si~O~2 were mixed in an agate mortar and filled into a tungsten crucible, then the powder mixtures were pre-heated at 900\%C for 2 h, then the temperature was enhanced to 1450\%C for 8 h. After firing, the samples were cooled to 900\%Cand finally quenched to room temperature. ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_exptl_refinement ; ? ; _exptl_crystal_density_diffrn 3.123 # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'Ca3 N2 O4 Si2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 268.42 _chemical_formula_sum 'Ca3 N2 O4 Si2' _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2030 0.3060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # 4. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system cubic _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_int_tables_number 205 _space_group_name_Hall '-P 2ac 2ab' _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_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' _cell_length_a 15.07392 _cell_length_b 15.07392 _cell_length_c 15.07392 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3425.141 _cell_formula_units_Z 24 _cell_measurement_temperature 293 _cell_special_details ; ? ; #============================================================================== # 5. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_char_colour white _diffrn_ambient_temperature 293 _diffrn_radiation_probe ? _diffrn_radiation_type 'Cu K\a' # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 1.540596 _diffrn_source ? _diffrn_source_type ? _diffrn_source_target Cu _diffrn_measurement_device_type 'Bruker D8 Advance' _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; _diffrn_radiation_monochromator Ge # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5829 _pd_meas_2theta_range_min 5 _pd_meas_2theta_range_max 119.9876 _pd_meas_2theta_range_inc 0.0144 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function PV-TCHZ _pd_proc_ls_background_function '20 Legendre polynoms' _pd_proc_ls_prof_R_factor 0.0470 _pd_proc_ls_prof_wR_factor 0.0735 _pd_proc_ls_prof_wR_expected 0.0506 _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 1/[Y~i~] _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_number_constraints 9 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all ? _refine_ls_restrained_S_all ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? #============================================================================== # 6. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Ca1 Ca+2 4 0 0 0 0.5612916 0.011408(6) Ca2 Ca+2 8 0.2382236 0.2382236 0.2382236 0.3325827 0.011408(6) Ca3 Ca+2 8 0.07028575 0.07028575 0.07028575 0.3867715 0.011408(6) Ca4 Ca+2 8 0.3702033 0.3702033 0.3702033 1 0.011408(6) Ca5 Ca+2 8 0.1579415 0.1579415 0.1579415 1 0.011408(6) Ca6 Ca+2 24 0.3543181 0.13831 0.3720886 1 0.011408(6) Ca7 Ca+2 24 0.1177887 0.09622956 0.3867902 1 0.011408(6) Si1 Si+4 24 0.5043013 0.2273262 0.2363038 1 0.000483(4) Si2 Si+4 24 0.4861069 0.01844902 0.2556805 1 0.000483(4) O1 O 24 0.2642051 0.2700584 0.411071 1 0.01(0) O2 O 24 0.3352409 0.4709358 0.4819417 1 0.01(0) N1 N 24 0.1234548 0.2724936 0.517672 1 0.00269(0) O3 O 24 0.08690233 0.2853346 0.2276274 1 0.01(0) O4 O 24 0.01401109 0.9600786 0.1582686 1 0.01(0) N2 N 24 0.235273 0.1203689 0.5094904 1 0.00269(0) # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. 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 _atom_site_aniso_type_symbol ? ? ? ? ? ? ? ? #============================================================================== # 7. MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O4 2.47(0) ? ? ? Ca2 O3 2.39(4) . . . Ca2 O1 2.67(8) . . . Ca3 O4 2.28(9) . . . Ca3 N1 2.62(4) . . . Ca4 O1 2.28(3) . . . Ca4 O2 2.32(8) . . . Ca5 O3 2.43(7) . . . Ca5 N1 2.42(7) . . . Ca6 O1 2.47(7) . . . Ca6 O3 2.43(7) . . . Ca6 N1 2.41(7) . . . Ca7 O2 2.31(5) . . . Ca7 O3 2.25(8) . . . Ca7 N1 2.86(5) . . . Ca7 N2 2.65(9) . . . Si1 O1 1.59(5) . . . Si1 O3 1.61(6) . . . Si1 N1 1.67(0) . . . Si1 N2 1.75(3) . . . Si2 O2 1.61(3) . . . Si2 O4 1.62(3) . . . Si2 N1 1.67(2) . . . Si2 N2 1.64(0) . . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 O1 60.0 ? ? ? ? O1 Si1 N1 66.9 . . . . O1 Si1 O3 59.7 . . . . O1 Si1 N2 110.9 . . . . O2 Si2 O2 60.0 . . . . O2 Si2 N1 63.8 . . . . O2 Si2 O4 59.6 . . . . O2 Si2 N2 62.3 . . . . O3 Si1 O1 60.0 . . . . O3 Si1 N1 128.2 . . . . O3 Si1 N2 61.5 . . . . O4 Si2 O2 55.9 . . . . O4 Si2 N1 120.3 . . . . O4 Si2 O4 73.1 . . . . O4 Si2 N2 60.8 . . . . N1 Si1 O3 99.4 . . . . N1 Si1 O4 136.6 . . . . N1 Si1 N2 99.9 . . . . N1 Si1 O1 60.3 . . . . N1 Si1 O2 60.4 . . . . N1 Si2 O2 131.5 . . . . N1 Si2 O3 57.2 . . . . N1 Si2 O4 148.7 . . . . N1 Si2 N2 89.2 . . . . N1 Si2 O1 116.0 . . . . N2 Si1 O3 99.4 . . . . N2 Si1 O4 136.6 . . . . N2 Si1 N2 99.9 . . . . N2 Si1 O1 60.3 . . . . N2 Si2 O2 148.5 . . . . N2 Si2 O3 89.4 . . . . N2 Si2 O4 126.6 . . . . N2 Si2 O1 112.1 . . . . N2 Si2 N1 114.2 . . . . #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./