#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/31/2013138.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_2013138 loop_ _publ_author_name 'Skellern, Matthew G.' 'Howie, R. Alan' 'Lachowski, Eric E.' 'Skakle, Janet M. S.' _publ_section_title ; Barium-deficient celsian, Ba~1{-~x}Al~2{-~2x}Si~2+2x~O~8~ (x = 0.20 or 0.06) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i11 _journal_page_last i14 _journal_paper_doi 10.1107/S0108270102023053 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety 'Al1.88 Ba0.94 O8 Si2.12' _chemical_formula_sum 'Al1.88 Ba0.94 O8 Si2.12' _chemical_formula_weight 367.03 _chemical_name_common celsian _chemical_name_systematic ; Barium aluminium silicate ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 115.17(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.633(6) _cell_length_b 13.063(8) _cell_length_c 7.214(5) _cell_measurement_reflns_used 14 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 14.15 _cell_measurement_theta_min 12.25 _cell_volume 736.3(9) _computing_cell_refinement 'P3 software' _computing_data_collection 'P3 software (Nicolet, 1980)' _computing_data_reduction 'RDNIC (Howie, 1980)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.497 _diffrn_measured_fraction_theta_max 0.497 _diffrn_measurement_device_type 'Nicolet P3' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.018 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1169 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 3.04 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 50 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 5.647 _exptl_absorpt_correction_T_max 0.551 _exptl_absorpt_correction_T_min 0.127 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.311 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 682 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _refine_diff_density_max 1.31 _refine_diff_density_min -1.03 _refine_ls_extinction_coef 0.0261(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.364 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 65 _refine_ls_number_reflns 1112 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.364 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.032 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0373P)^2^+6.7094P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.095 _refine_ls_wR_factor_ref 0.095 _reflns_number_gt 1111 _reflns_number_total 1112 _reflns_threshold_expression I>2\s(I) _cod_data_source_file fg1678.cif _cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M 'C 2/m' _cod_database_code 2013138 _cod_database_fobs_code 2013138 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ba1 0.28270(5) 0.0000 0.13057(6) 0.0203(2) Uani d SP 0.938(5) . . Ba Al1 0.00832(15) 0.18272(9) 0.22450(18) 0.0167(4) Uani d P 0.469(2) . . Al Si1 0.00832(15) 0.18272(9) 0.22450(18) 0.0167(4) Uani d P 0.531(2) . . Si Al2 0.20313(15) 0.38148(10) 0.34697(18) 0.0165(3) Uani d P 0.469(2) . . Al Si2 0.20313(15) 0.38148(10) 0.34697(18) 0.0165(3) Uani d P 0.531(2) . . Si O1 0.0000 0.1381(3) 0.0000 0.0192(8) Uani d S 1 . . O O2 0.1209(6) 0.5000 0.2878(8) 0.0220(9) Uani d S 1 . . O O3 0.3266(5) 0.3626(3) 0.2241(5) 0.0259(7) Uani d . 1 . . O O4 0.0251(4) 0.3101(3) 0.2520(6) 0.0250(7) Uani d . 1 . . O O5 0.1865(4) 0.1264(3) 0.3970(5) 0.0245(7) Uani d . 1 . . O 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 Ba1 0.0171(3) 0.0182(3) 0.0232(3) 0.000 0.00635(16) 0.000 Al1 0.0166(6) 0.0131(6) 0.0185(6) -0.0017(4) 0.0056(4) -0.0002(4) Si1 0.0166(6) 0.0131(6) 0.0185(6) -0.0017(4) 0.0056(4) -0.0002(4) Al2 0.0170(6) 0.0140(6) 0.0166(6) -0.0013(4) 0.0054(4) 0.0003(4) Si2 0.0170(6) 0.0140(6) 0.0166(6) -0.0013(4) 0.0054(4) 0.0003(4) O1 0.023(2) 0.0156(19) 0.0177(18) 0.000 0.0076(16) 0.000 O2 0.020(2) 0.0100(18) 0.032(2) 0.000 0.0071(18) 0.000 O3 0.0267(16) 0.0248(17) 0.0249(16) 0.0031(13) 0.0096(13) 0.0016(13) O4 0.0231(15) 0.0182(15) 0.0337(17) -0.0008(12) 0.0120(13) 0.0031(13) O5 0.0232(15) 0.0255(16) 0.0221(15) 0.0004(13) 0.0072(12) -0.0030(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' O O 0.0106 0.0060 '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 O2 Ba1 O1 3_545 . 140.79(8) O2 Ba1 O1 3_545 5 140.79(8) O1 Ba1 O1 . 5 78.42(15) O2 Ba1 O5 3_545 2 106.85(12) O1 Ba1 O5 . 2 97.61(9) O1 Ba1 O5 5 2 54.21(8) O2 Ba1 O5 3_545 . 106.85(12) O1 Ba1 O5 . . 54.21(8) O1 Ba1 O5 5 . 97.61(9) O5 Ba1 O5 2 . 69.13(16) O2 Ba1 O3 3_545 8_545 105.13(12) O1 Ba1 O3 . 8_545 100.73(10) O1 Ba1 O3 5 8_545 54.03(8) O5 Ba1 O3 2 8_545 98.79(11) O5 Ba1 O3 . 8_545 147.89(10) O2 Ba1 O3 3_545 7 105.13(12) O1 Ba1 O3 . 7 54.03(8) O1 Ba1 O3 5 7 100.73(10) O5 Ba1 O3 2 7 147.89(10) O5 Ba1 O3 . 7 98.79(11) O3 Ba1 O3 8_545 7 75.44(15) O2 Ba1 O4 3_545 4 52.66(7) O1 Ba1 O4 . 4 88.14(11) O1 Ba1 O4 5 4 166.50(10) O5 Ba1 O4 2 4 127.67(11) O5 Ba1 O4 . 4 73.10(11) O3 Ba1 O4 8_545 4 131.27(10) O3 Ba1 O4 7 4 71.77(11) O2 Ba1 O4 3_545 3_545 52.66(7) O1 Ba1 O4 . 3_545 166.50(10) O1 Ba1 O4 5 3_545 88.14(11) O5 Ba1 O4 2 3_545 73.10(11) O5 Ba1 O4 . 3_545 127.67(11) O3 Ba1 O4 8_545 3_545 71.77(11) O3 Ba1 O4 7 3_545 131.27(10) O4 Ba1 O4 4 3_545 105.28(14) O2 Ba1 Si1 3_545 5 127.66(7) O1 Ba1 Si1 . 5 86.81(9) O1 Ba1 Si1 5 5 27.20(3) O5 Ba1 Si1 2 5 77.65(9) O5 Ba1 Si1 . 5 122.31(8) O3 Ba1 Si1 8_545 5 27.14(8) O3 Ba1 Si1 7 5 85.25(9) O4 Ba1 Si1 4 5 154.64(8) O4 Ba1 Si1 3_545 5 81.68(9) O2 Ba1 Al1 3_545 5 127.66(7) O1 Ba1 Al1 . 5 86.81(9) O1 Ba1 Al1 5 5 27.20(3) O5 Ba1 Al1 2 5 77.65(9) O5 Ba1 Al1 . 5 122.31(8) O3 Ba1 Al1 8_545 5 27.14(8) O3 Ba1 Al1 7 5 85.25(9) O4 Ba1 Al1 4 5 154.64(8) O4 Ba1 Al1 3_545 5 81.68(9) Si1 Ba1 Al1 5 5 0.00(7) O2 Ba1 Al1 3_545 6 127.66(7) O1 Ba1 Al1 . 6 27.20(3) O1 Ba1 Al1 5 6 86.82(9) O5 Ba1 Al1 2 6 122.31(8) O5 Ba1 Al1 . 6 77.65(9) O3 Ba1 Al1 8_545 6 85.25(9) O3 Ba1 Al1 7 6 27.14(8) O4 Ba1 Al1 4 6 81.68(9) O4 Ba1 Al1 3_545 6 154.64(8) Si1 Ba1 Al1 5 6 82.53(7) Al1 Ba1 Al1 5 6 82.53(7) O4 Al1 O3 . 4_455 112.64(19) O4 Al1 O5 . . 109.97(19) O3 Al1 O5 4_455 . 114.1(2) O4 Al1 O1 . . 114.9(2) O3 Al1 O1 4_455 . 102.58(16) O5 Al1 O1 . . 102.13(17) O4 Al1 Ba1 . 5 137.57(14) O3 Al1 Ba1 4_455 5 53.00(13) O5 Al1 Ba1 . 5 112.10(15) O1 Al1 Ba1 . 5 50.34(10) O4 Al1 Ba1 . . 130.25(14) O3 Al1 Ba1 4_455 . 116.93(14) O5 Al1 Ba1 . . 52.06(13) O1 Al1 Ba1 . . 50.19(10) Ba1 Al1 Ba1 5 . 75.25(6) O3 Al2 O4 . . 112.5(2) O3 Al2 O2 . . 107.3(2) O4 Al2 O2 . . 101.2(2) O3 Al2 O5 . 7_556 112.49(19) O4 Al2 O5 . 7_556 114.1(2) O2 Al2 O5 . 7_556 108.4(2) O3 Al2 Ba1 . 3_455 125.59(14) O4 Al2 Ba1 . 3_455 59.05(13) O2 Al2 Ba1 . 3_455 42.37(15) O5 Al2 Ba1 7_556 3_455 119.56(14) O3 Al2 Ba1 . 7 46.33(13) O4 Al2 Ba1 . 7 103.42(14) O2 Al2 Ba1 . 7 64.55(18) O5 Al2 Ba1 7_556 7 142.45(14) Ba1 Al2 Ba1 3_455 7 81.33(5) Al1 O1 Si1 . 6 139.7(3) Al1 O1 Al1 . 6 139.7(3) Si1 O1 Al1 6 6 0.00(13) Al1 O1 Ba1 . 5 102.46(9) Si1 O1 Ba1 6 5 102.68(9) Al1 O1 Ba1 6 5 102.68(9) Al1 O1 Ba1 . . 102.68(9) Si1 O1 Ba1 6 . 102.46(9) Al1 O1 Ba1 6 . 102.46(9) Ba1 O1 Ba1 5 . 101.58(15) Al2 O2 Si2 . 2_565 134.2(3) Al2 O2 Al2 . 2_565 134.2(3) Si2 O2 Al2 2_565 2_565 0.00(15) Al2 O2 Ba1 . 3_455 112.27(15) Si2 O2 Ba1 2_565 3_455 112.27(15) Al2 O2 Ba1 2_565 3_455 112.27(15) Al2 O3 Si1 . 4 149.3(2) Al2 O3 Al1 . 4 149.3(2) Si1 O3 Al1 4 4 0.00(13) Al2 O3 Ba1 . 7 109.37(17) Si1 O3 Ba1 4 7 99.85(16) Al1 O3 Ba1 4 7 99.85(16) Al2 O4 Al1 . . 128.3(2) Al2 O4 Ba1 . 3_455 93.54(16) Al1 O4 Ba1 . 3_455 137.96(18) Al1 O5 Si2 . 7_556 138.7(2) Al1 O5 Al2 . 7_556 138.7(2) Si2 O5 Al2 7_556 7_556 0.00(14) Al1 O5 Ba1 . . 100.82(16) Si2 O5 Ba1 7_556 . 120.20(18) Al2 O5 Ba1 7_556 . 120.20(18) 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 Ba1 O2 3_545 2.645(5) ? Ba1 O1 . 2.853(3) ? Ba1 O1 5 2.853(3) ? Ba1 O5 2 2.910(4) ? Ba1 O5 . 2.910(4) ? Ba1 O3 8_545 2.933(4) ? Ba1 O3 7 2.933(4) ? Ba1 O4 4 3.120(4) ? Ba1 O4 3_545 3.120(4) ? Ba1 Si1 5 3.619(2) ? Ba1 Al1 5 3.619(2) ? Ba1 Al1 6 3.619(2) ? Al1 O4 . 1.675(4) ? Al1 O3 4_455 1.676(4) ? Al1 O5 . 1.682(4) ? Al1 O1 . 1.694(2) ? Al1 Ba1 5 3.619(2) ? Al2 O3 . 1.669(4) ? Al2 O4 . 1.675(4) ? Al2 O2 . 1.681(2) ? Al2 O5 7_556 1.683(4) ? Al2 Ba1 3_455 3.632(3) ? Al2 Ba1 7 3.826(3) ? O1 Si1 6 1.694(2) ? O1 Al1 6 1.694(2) ? O1 Ba1 5 2.853(3) ? O2 Si2 2_565 1.681(2) ? O2 Al2 2_565 1.681(2) ? O2 Ba1 3_455 2.645(5) ? O3 Si1 4 1.676(4) ? O3 Al1 4 1.676(4) ? O3 Ba1 7 2.933(4) ? O4 Ba1 3_455 3.120(4) ? O5 Si2 7_556 1.683(4) ? O5 Al2 7_556 1.683(4) ?