#------------------------------------------------------------------------------ #$Date: 2015-06-25 01:13:37 +0300 (Thu, 25 Jun 2015) $ #$Revision: 139558 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/32/4513295.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_4513295 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_name_full 'Crystal Growth & Design' _journal_page_first 150624123626000 _journal_paper_doi 10.1021/acs.cgd.5b00567 _journal_year 2015 _chemical_formula_moiety '0.5(As4 O6)' _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 107.03(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.3873(8) _cell_length_b 4.1360(2) _cell_length_c 7.490(4) _cell_measurement_pressure 9.54e6(11) _cell_measurement_reflns_used 455 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.3580 _cell_measurement_theta_min 1.4740 _cell_volume 248.43(14) _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 9.54e6(11) _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.405 _diffrn_measured_fraction_theta_max 0.264 _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 0.0575631000 _diffrn_orient_matrix_UB_12 0.0084531000 _diffrn_orient_matrix_UB_13 0.0134811000 _diffrn_orient_matrix_UB_21 -0.0026391000 _diffrn_orient_matrix_UB_22 0.0773243000 _diffrn_orient_matrix_UB_23 0.0306807000 _diffrn_orient_matrix_UB_31 0.0044391000 _diffrn_orient_matrix_UB_32 -0.0631870000 _diffrn_orient_matrix_UB_33 0.0393064000 _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.41427 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_unetI/netI 0.0495 _diffrn_reflns_laue_measured_fraction_full 0.405 _diffrn_reflns_laue_measured_fraction_max 0.264 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 681 _diffrn_reflns_point_group_measured_fraction_full 0.428 _diffrn_reflns_point_group_measured_fraction_max 0.269 _diffrn_reflns_theta_full 14.392 _diffrn_reflns_theta_max 20.359 _diffrn_reflns_theta_min 1.480 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 6.111 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79052 _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 5.289 _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 1.496 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.343 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 62 _refine_ls_number_reflns 551 _refine_ls_number_restraints 67 _refine_ls_restrained_S_all 1.140 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0694 _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^)+(0.1320P)^2^+1.4650P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1846 _refine_ls_wR_factor_ref 0.1919 _reflns_Friedel_coverage 0.838 _reflns_friedel_fraction_full 0.459 _reflns_friedel_fraction_max 0.275 _reflns_number_gt 495 _reflns_number_total 551 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cg5b00567_si_002.cif _cod_data_source_block mclau2_020_pl _cod_database_code 4513295 _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: 0.3(4) 0.7(4) 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_020_pl.res created by SHELXL-2014/7 TITL mclau2_020_a.res in P2(1) CELL 0.41427 8.3873 4.136 7.49 90 107.03 90 ZERR 4 0.0008 0.0002 0.004 0 0.03 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 OMIT 8 -3 1 OMIT -8 4 4 OMIT -13 1 6 OMIT 4 -2 0 OMIT -2 -1 2 REM REM REM WGHT 0.132000 1.465000 BASF 0.73296 FVAR 1.14002 AS1 1 0.372130 0.218879 -0.110502 11.00000 0.02191 0.01827 = 0.06000 0.00559 0.01900 0.00346 AS2 1 0.117084 0.029206 0.122663 11.00000 0.02106 0.01745 = 0.04934 0.00448 0.01267 -0.00001 O1 2 0.576593 0.309664 0.038522 11.00000 0.01683 O2 2 0.255448 0.291291 0.050301 11.00000 0.02292 O3 2 -0.038782 0.336135 0.099351 11.00000 0.02182 AS3 1 0.399161 0.605651 0.357535 11.00000 0.02196 0.02010 = 0.07151 0.00481 0.02265 0.00148 AS4 1 0.141347 0.653355 0.574028 11.00000 0.01925 0.01948 = 0.07951 0.00130 0.02050 0.00077 O4 2 0.527272 0.253566 0.408773 11.00000 0.01983 O5 2 0.231008 0.424695 0.424245 11.00000 0.02177 O6 2 -0.026188 0.812861 0.388159 11.00000 0.02115 HKLF 4 1 0 0 -1 0 -1 0 -1 0 0 REM mclau2_020_a.res in P2(1) REM R1 = 0.0694 for 495 Fo > 4sig(Fo) and 0.0754 for all 551 data REM 62 parameters refined using 67 restraints END WGHT 0.1342 2.2764 REM Highest difference peak 1.496, deepest hole -1.359, 1-sigma level 0.343 Q1 1 0.0573 0.0165 -0.1596 11.00000 0.05 1.50 Q2 1 0.1189 0.4521 -0.4137 11.00000 0.05 1.37 Q3 1 0.4350 0.6990 -0.5319 11.00000 0.05 1.35 Q4 1 0.5784 1.1855 -0.4233 11.00000 0.05 1.33 Q5 1 0.1584 0.6211 -0.3833 11.00000 0.05 1.30 Q6 1 0.6217 0.1897 -0.2988 11.00000 0.05 1.29 Q7 1 0.1621 0.0000 0.3594 11.00000 0.05 1.25 Q8 1 0.6338 0.2011 -0.2548 11.00000 0.05 1.25 Q9 1 0.3594 -0.1914 0.4581 11.00000 0.05 1.25 Q10 1 0.4437 0.2428 0.1757 11.00000 0.05 1.24 Q11 1 0.3635 0.0642 -0.1015 11.00000 0.05 1.21 Q12 1 0.3147 0.2309 -0.3525 11.00000 0.05 1.21 Q13 1 0.1766 0.5639 -0.3092 11.00000 0.05 1.17 Q14 1 0.1003 -0.3449 0.3121 11.00000 0.05 1.16 Q15 1 0.2437 0.6645 0.5760 11.00000 0.05 1.12 Q16 1 -0.0844 0.3511 0.3894 11.00000 0.05 1.07 Q17 1 0.2802 -0.3916 0.3925 11.00000 0.05 1.04 Q18 1 0.4753 0.2031 0.4420 11.00000 0.05 1.04 Q19 1 0.2408 0.4138 -0.3798 11.00000 0.05 0.98 Q20 1 0.3024 0.3365 0.2672 11.00000 0.05 0.97 ; _shelx_res_checksum 9316 _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 0.3721(4) 0.2189(6) -0.1105(10) 0.032(3) Uani 1 1 d D As2 As 0.1171(4) 0.0292(6) 0.1227(10) 0.029(4) Uani 1 1 d D O1 O 0.5766(15) 0.310(3) 0.039(4) 0.017(4) Uiso 1 1 d D O2 O 0.255(3) 0.291(4) 0.050(3) 0.023(4) Uiso 1 1 d D O3 O -0.0388(18) 0.336(4) 0.099(2) 0.022(4) Uiso 1 1 d D As3 As 0.3992(4) 0.6057(7) 0.3575(10) 0.036(3) Uani 1 1 d D As4 As 0.1413(4) 0.6534(7) 0.5740(11) 0.038(3) Uani 1 1 d D O4 O 0.527(2) 0.254(3) 0.409(2) 0.020(4) Uiso 1 1 d D O5 O 0.231(2) 0.425(4) 0.424(4) 0.022(4) Uiso 1 1 d D O6 O -0.0262(18) 0.813(4) 0.388(3) 0.021(4) 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 0.0219(12) 0.0183(17) 0.060(11) 0.0056(19) 0.019(3) 0.0035(11) As2 0.0211(14) 0.0174(13) 0.049(11) 0.004(2) 0.013(3) 0.0000(11) As3 0.0220(13) 0.0201(15) 0.072(11) 0.005(2) 0.023(3) 0.0015(13) As4 0.0193(13) 0.0195(16) 0.080(11) 0.001(2) 0.021(3) 0.0008(12) 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 O1 As1 O1 84.8(4) 2_645 O1 As1 O2 94.9(12) 2_645 O2 As1 O1 99.1(12) . O2 As2 O3 93.5(9) . O3 As2 O2 94.8(8) 2_545 O3 As2 O3 99.6(6) 2_545 As1 O1 As1 119.2(8) 2_655 As2 O2 As1 129.5(10) . As2 O3 As2 117.7(9) 2 O4 As3 O4 93.2(6) 2_656 O4 As3 O5 94.2(9) . O4 As3 O5 86.8(9) 2_656 O6 As4 O5 94.9(11) . O6 As4 O5 91.7(8) 2_546 O6 As4 O6 94.4(6) 2_546 As3 O4 As3 120.3(10) 2_646 As3 O5 As4 117.6(8) . As4 O6 As4 120.5(10) 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 1.790(10) 2_645 As1 O1 1.791(10) . As1 O2 1.786(11) . As2 O2 1.784(10) . As2 O3 1.794(10) . As2 O3 1.787(11) 2_545 O1 As1 1.790(10) 2_655 O3 As2 1.787(11) 2 As3 O4 1.785(11) 2_656 As3 O4 1.784(10) . As3 O5 1.792(10) . As4 O5 1.792(11) . As4 O6 1.789(11) . As4 O6 1.777(11) 2_546 O4 As3 1.785(11) 2_646 O6 As4 1.777(11) 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 O1 As1 O1 As1 -163(3) 2_645 2_655 O1 As1 O2 As2 -39(2) 2_645 . O1 As1 O2 As2 -124.1(18) . . O2 As1 O1 As1 -69.1(18) . 2_655 O2 As2 O3 As2 56.5(13) . 2 O3 As2 O2 As1 -134.8(19) . . O3 As2 O2 As1 -35(2) 2_545 . O3 As2 O3 As2 -39.0(13) 2_545 2 O4 As3 O4 As3 23.1(10) 2_656 2_646 O4 As3 O5 As4 132.7(16) . . O4 As3 O5 As4 39.7(16) 2_656 . O5 As3 O4 As3 -63.9(14) . 2_646 O5 As4 O6 As4 -163.3(12) . 2_556 O6 As4 O5 As3 -169.4(16) 2_546 . O6 As4 O5 As3 96.0(17) . . O6 As4 O6 As4 104.7(18) 2_546 2_556 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.3(4) 2 0.7(4)