#------------------------------------------------------------------------------ #$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $ #$Revision: 154542 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/32/4513294.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4513294 loop_ _publ_author_name 'Gu\'nka, Piotr A.' 'Dranka, Maciej' 'Hanfland, Michael' 'Dziubek, Kamil F.' 'Katrusiak, Andrzej' 'Zachara, Janusz' _publ_section_title ; Cascade of High-Pressure Transitions of Claudetite II and the First Polar Phase of Arsenic(III) Oxide ; _journal_issue 8 _journal_name_full 'Crystal Growth & Design' _journal_page_first 3950 _journal_paper_doi 10.1021/acs.cgd.5b00567 _journal_volume 15 _journal_year 2015 _chemical_formula_moiety '0.25(As8 O12)' _chemical_formula_sum 'As2 O3' _chemical_formula_weight 197.84 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _audit_creation_date 2015-04-13 _audit_creation_method ; Olex2 1.2-beta (compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4998) ; _cell_angle_alpha 90 _cell_angle_beta 106.53(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.2230(7) _cell_length_b 3.9071(2) _cell_length_c 7.130(3) _cell_measurement_pressure 2.116e7(11) _cell_measurement_reflns_used 357 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 19.5130 _cell_measurement_theta_min 1.5080 _cell_volume 219.61(10) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _diffrn_ambient_environment He _diffrn_ambient_pressure 2.116e7(11) _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.398 _diffrn_measured_fraction_theta_max 0.270 _diffrn_measurement_details ; 1 phi 142.00 218.00 0.5000 1.0000 omega____ theta____ kappa____ phi______ frames 0.0000 0.0000 0.0000 - 152 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'MAR-CrysAlisPro-abstract goniometer: imported MAR images' _diffrn_measurement_method '\p scans' _diffrn_orient_matrix_UB_11 -0.0603605000 _diffrn_orient_matrix_UB_12 0.0080881000 _diffrn_orient_matrix_UB_13 -0.0138250000 _diffrn_orient_matrix_UB_21 0.0030246000 _diffrn_orient_matrix_UB_22 0.0860311000 _diffrn_orient_matrix_UB_23 -0.0286562000 _diffrn_orient_matrix_UB_31 -0.0036720000 _diffrn_orient_matrix_UB_32 -0.0615637000 _diffrn_orient_matrix_UB_33 -0.0418192000 _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.41427 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_unetI/netI 0.0764 _diffrn_reflns_laue_measured_fraction_full 0.398 _diffrn_reflns_laue_measured_fraction_max 0.270 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 637 _diffrn_reflns_point_group_measured_fraction_full 0.429 _diffrn_reflns_point_group_measured_fraction_max 0.278 _diffrn_reflns_theta_full 14.392 _diffrn_reflns_theta_max 20.245 _diffrn_reflns_theta_min 1.506 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 6.914 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.37047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 5.984 _exptl_crystal_description block _exptl_crystal_F_000 360 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 2.231 _refine_diff_density_min -1.820 _refine_diff_density_rms 0.475 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 62 _refine_ls_number_reflns 499 _refine_ls_number_restraints 67 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0929 _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^)+(0.1150P)^2^+21.3530P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2382 _refine_ls_wR_factor_ref 0.2450 _reflns_Friedel_coverage 0.852 _reflns_friedel_fraction_full 0.470 _reflns_friedel_fraction_max 0.289 _reflns_number_gt 447 _reflns_number_total 499 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cg5b00567_si_002.cif _cod_data_source_block mclau2_019_pl _cod_depositor_comments 'Adding full bibliography for 4513277--4513300.cif.' _cod_database_code 4513294 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.7(6) 0.3(6) 2. Restrained distances As1-O1 \\sim As1-O2 \\sim As2-O2 \\sim As2-O3 \\sim As3-O4 \\sim As3-O5 \\sim As4-O5 \\sim As4-O6 \\sim As1- O1 \\sim As1-O1 \\sim As1-O1_$1 \\sim As2-O3_$2 \\sim As3-O4_$3 \\sim As4-O6_$4 with sigma of 0.01 ; _shelx_res_file ; mclau2_019_pl.res created by SHELXL-2014/7 TITL mclau2_019_a.res in P2(1) CELL 0.41427 8.223 3.9071 7.13 90 106.53 90 ZERR 4 0.0007 0.0002 0.003 0 0.02 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC As O DISP As 0.311 0.799 1882.762 DISP O 0.002 0.002 10.067 UNIT 8 12 EQIV $1 1-X,-0.5+Y,-Z EQIV $2 -X,-0.5+Y,-Z EQIV $3 1-X,0.5+Y,1-Z EQIV $4 -X,-0.5+Y,1-Z SADI 0.01 As1 O1 As1 O2 As2 O2 As2 O3 As3 O4 As3 O5 As4 O5 As4 O6 As1 O1 As1 = O1 AS1 O1_$1 AS2 O3_$2 AS3 O4_$3 AS4 O6_$4 L.S. 10 PLAN -20 BOND $H CONF MORE -1 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.115000 21.352999 BASF 0.29168 FVAR 1.37703 AS1 1 0.369890 0.238370 -0.117422 11.00000 0.02262 0.01948 = 0.05603 0.00579 0.01909 0.00227 AS2 1 0.120232 0.003836 0.129370 11.00000 0.02019 0.01863 = 0.05788 0.00206 0.01373 -0.00298 O1 2 0.578605 0.300470 0.046648 11.00000 0.03253 O2 2 0.260045 0.305409 0.064255 11.00000 0.01779 O3 2 -0.037790 0.330002 0.112680 11.00000 0.02256 AS3 1 0.398180 0.598836 0.347980 11.00000 0.01862 0.02141 = 0.05425 0.00235 0.01654 -0.00131 AS4 1 0.146391 0.660186 0.575830 11.00000 0.02047 0.02246 = 0.05555 -0.00267 0.01571 -0.00021 O4 2 0.530884 0.225407 0.399309 11.00000 0.01698 O5 2 0.235066 0.386922 0.427136 11.00000 0.02533 O6 2 -0.026054 0.805455 0.374563 11.00000 0.02398 HKLF 4 1 0 0 -1 0 -1 0 -1 0 0 REM mclau2_019_a.res in P2(1) REM R1 = 0.0929 for 447 Fo > 4sig(Fo) and 0.1016 for all 499 data REM 62 parameters refined using 67 restraints END WGHT 0.1164 20.4506 REM Highest difference peak 2.231, deepest hole -1.820, 1-sigma level 0.475 Q1 1 0.1232 0.4093 -0.3829 11.00000 0.05 2.23 Q2 1 0.3649 -0.1218 0.4340 11.00000 0.05 2.05 Q3 1 0.5288 0.2485 0.0150 11.00000 0.05 1.51 Q4 1 0.3358 0.0372 -0.0473 11.00000 0.05 1.47 Q5 1 0.4462 0.0984 0.0819 11.00000 0.05 1.46 Q6 1 0.5467 0.2494 -0.2285 11.00000 0.05 1.41 Q7 1 0.1407 0.4637 -0.1658 11.00000 0.05 1.39 Q8 1 0.1198 0.3312 0.1405 11.00000 0.05 1.37 Q9 1 0.4956 0.2175 0.2654 11.00000 0.05 1.35 Q10 1 0.7231 0.0921 0.0190 11.00000 0.05 1.33 Q11 1 0.0381 0.1680 -0.3447 11.00000 0.05 1.30 Q12 1 0.6569 0.2171 -0.1925 11.00000 0.05 1.30 Q13 1 0.2016 0.5000 0.4325 11.00000 0.05 1.26 Q14 1 0.1816 0.2114 0.0619 11.00000 0.05 1.24 Q15 1 0.2854 0.1177 0.4309 11.00000 0.05 1.23 Q16 1 0.5631 0.2018 0.5206 11.00000 0.05 1.22 Q17 1 0.4565 0.0077 -0.0782 11.00000 0.05 1.21 Q18 1 0.6586 0.2191 0.0760 11.00000 0.05 1.20 Q19 1 0.6768 0.4550 0.1734 11.00000 0.05 1.19 Q20 1 0.1803 0.4029 0.2879 11.00000 0.05 1.17 ; _shelx_res_checksum 24025 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _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 _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn As1 As 0.3699(7) 0.2384(11) -0.1174(19) 0.031(6) Uani 1 1 d D As2 As 0.1202(6) 0.0038(13) 0.1294(17) 0.032(6) Uani 1 1 d D O1 O 0.579(3) 0.300(5) 0.047(7) 0.033(9) Uiso 1 1 d D O2 O 0.260(4) 0.305(5) 0.064(5) 0.018(6) Uiso 1 1 d D O3 O -0.038(3) 0.330(6) 0.113(3) 0.023(7) Uiso 1 1 d D As3 As 0.3982(6) 0.5988(13) 0.3480(17) 0.030(5) Uani 1 1 d D As4 As 0.1464(7) 0.6602(12) 0.5758(19) 0.032(5) Uani 1 1 d D O4 O 0.531(3) 0.225(5) 0.399(3) 0.017(6) Uiso 1 1 d D O5 O 0.235(5) 0.387(6) 0.427(7) 0.025(7) Uiso 1 1 d D O6 O -0.026(3) 0.805(6) 0.375(4) 0.024(7) Uiso 1 1 d D loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.023(2) 0.019(2) 0.056(19) 0.006(3) 0.019(6) 0.0023(18) As2 0.020(3) 0.0186(19) 0.06(2) 0.002(3) 0.014(6) -0.0030(18) As3 0.019(2) 0.021(2) 0.054(17) 0.002(3) 0.017(5) -0.0013(19) As4 0.020(2) 0.022(2) 0.056(18) -0.003(3) 0.016(6) -0.0002(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.3110 0.7990 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0020 0.0020 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 As1 O1 80.8(6) . 2_645 O1 As1 O1 69.0(9) . 2_655 O1 As1 O1 147.6(19) 2_645 2_655 O1 As1 O2 95(2) . . O1 As1 As3 74.6(16) . 2_645 O1 As1 As3 101.4(13) 2_655 2_645 O1 As1 As3 80.8(17) 2_645 2_645 O2 As1 O1 94(2) . 2_645 O2 As1 O1 78.4(15) . 2_655 O2 As1 As3 169.1(13) . 2_645 O2 As2 O3 95.4(11) . 2_545 O2 As2 O3 91.2(13) . . O2 As2 As3 91.9(12) . 1_545 O3 As2 O3 97.8(9) 2_545 . O3 As2 As3 109.9(11) 2_545 1_545 O3 As2 As3 151.7(11) . 1_545 As1 O1 As1 147.6(19) 2_655 2_645 As1 O1 As1 114.6(13) . 2_655 As1 O1 As1 95.6(7) . 2_645 As1 O2 As2 125.5(13) . . As1 O2 As3 118.6(12) . . As2 O2 As3 106.8(12) . . As2 O3 As2 113.5(13) 2 . As2 As3 As1 98.0(4) 1_565 2_655 O2 As3 As1 80.6(4) . 2_655 O2 As3 As2 71.4(8) . 1_565 O4 As3 As1 79.0(8) . 2_655 O4 As3 As1 116.0(7) 2_656 2_655 O4 As3 As2 155.3(10) . 1_565 O4 As3 As2 112.1(9) 2_656 1_565 O4 As3 O2 161.4(7) 2_656 . O4 As3 O2 84.0(12) . . O4 As3 O4 90.8(9) . 2_656 O4 As3 O5 91.5(15) . . O5 As3 As1 159.0(10) . 2_655 O5 As3 As2 82.7(16) . 1_565 O5 As3 O2 79.8(13) . . O5 As3 O4 82.6(14) . 2_656 O6 As4 O5 89.8(12) 2_546 . O6 As4 O5 94.4(18) . . O6 As4 O6 92.7(10) 2_546 . As3 O4 As3 115.6(13) . 2_646 As3 O5 As4 112.0(12) . . As4 O6 As4 116.1(13) 2_556 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 As1 O1 1.797(14) . As1 O1 2.27(2) 2_655 As1 O1 1.800(13) 2_645 As1 O2 1.797(13) . As1 As3 2.902(11) 2_645 As2 O2 1.797(12) . As2 O3 1.798(14) 2_545 As2 O3 1.800(13) . As2 As3 2.851(10) 1_545 O1 As1 1.800(13) 2_655 O1 As1 2.27(2) 2_645 O2 As3 2.32(3) . O3 As2 1.798(14) 2 As3 As1 2.902(11) 2_655 As3 As2 2.851(10) 1_565 As3 O4 1.798(14) 2_656 As3 O4 1.796(13) . As3 O5 1.798(13) . As4 O5 1.799(13) . As4 O6 1.798(14) . As4 O6 1.796(13) 2_546 O4 As3 1.798(14) 2_646 O6 As4 1.796(13) 2_556 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 As1 As3 O4 As3 134.8(15) 2_655 2_646 As1 As3 O5 As4 -161(2) 2_655 . As2 As3 O4 As3 -139.9(14) 1_565 2_646 As2 As3 O5 As4 -67(2) 1_565 . O1 As1 O1 As1 1.6(6) 2_655 2_655 O1 As1 O1 As1 -167(5) 2_645 2_655 O1 As1 O1 As1 170(4) 2_655 2_645 O1 As1 O1 As1 1.4(5) 2_645 2_645 O1 As1 O2 As2 -122(2) . . O1 As1 O2 As2 171(3) 2_655 . O1 As1 O2 As2 -41(2) 2_645 . O1 As1 O2 As3 101.7(16) 2_645 . O1 As1 O2 As3 -46.7(13) 2_655 . O1 As1 O2 As3 20.5(16) . . O2 As1 O1 As1 94.2(18) . 2_645 O2 As1 O1 As1 -74(3) . 2_655 O2 As2 O3 As2 63(2) . 2 O2 As3 O4 As3 -143.6(15) . 2_646 O2 As3 O5 As4 -139(3) . . O3 As2 O2 As1 -34(3) 2_545 . O3 As2 O2 As1 -132(2) . . O3 As2 O2 As3 180.0(14) 2_545 . O3 As2 O2 As3 82.0(14) . . O3 As2 O3 As2 -32.2(19) 2_545 2 As3 As1 O1 As1 -81.5(14) 2_645 2_645 As3 As1 O1 As1 111(3) 2_645 2_655 As3 As1 O2 As2 -99(4) 2_645 . As3 As1 O2 As3 43(4) 2_645 . As3 As2 O2 As1 76(2) 1_545 . As3 As2 O2 As3 -69.9(11) 1_545 . As3 As2 O3 As2 159.7(6) 1_545 2 O4 As3 O4 As3 18.5(12) 2_656 2_646 O4 As3 O5 As4 46(2) 2_656 . O4 As3 O5 As4 137(3) . . O5 As3 O4 As3 -64(2) . 2_646 O5 As4 O6 As4 -169.0(18) . 2_556 O6 As4 O5 As3 94(3) . . O6 As4 O5 As3 -173(3) 2_546 . O6 As4 O6 As4 101(3) 2_546 2_556 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.7(6) 2 0.3(6)