data_CaIrO3-300K-Pbnm _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ca Ir O3' _chemical_formula_sum 'Ca Ir O3' _chemical_formula_weight 280.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'orthorhombic' _space_group_IT_number 62 _space_group_name_H-M_alt 'P b n m' _space_group_name_Hall '-P 2c 2ab' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, y, -z+1/2' 'x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' '-x, -y, z-1/2' '-x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 5.3597(5) _cell_length_b 5.6131(4) _cell_length_c 7.6824(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 231.12(4) _cell_formula_units_Z 4 _cell_measurement_temperature 300 _cell_measurement_reflns_used 14436 _cell_measurement_theta_min 4.637 _cell_measurement_theta_max 40.984 _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 8.055 _exptl_crystal_F_000 484 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.090 _exptl_absorpt_coefficient_mu 59.687 _shelx_estimated_absorpt_T_min 0.044 _shelx_estimated_absorpt_T_max 0.075 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.01118 _exptl_absorpt_correction_T_max 0.09737 _exptl_absorpt_process_details ; Analytical Absorption Correction Program, N.W. Alcock (1970). Cryst. Computing, 271. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus rotating ande' _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD' _diffrn_measurement_method '\w-scan' _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 14436 _diffrn_reflns_av_unetI/netI 0.0467 _diffrn_reflns_av_R_equivalents 0.1558 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.637 _diffrn_reflns_theta_max 40.984 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 799 _reflns_number_gt 690 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000' _computing_structure_solution 'SHELXT-2018/2' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'SHELXLE' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.1552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 0.031(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 799 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.000000 0.000000 0.000000 0.01334(17) Uani 1 2 d S . P . . Ca Ca 0.48318(12) 0.0604(2) 0.250000 0.0173(2) Uani 1 2 d S T P . . O1 O 0.6036(5) 0.4650(5) 0.250000 0.0177(4) Uani 1 2 d S T P . . O2 O 0.1933(3) 0.3011(4) 0.0522(2) 0.0178(3) Uani 1 1 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 Ir 0.0146(3) 0.0180(3) 0.0075(3) -0.00002(3) -0.00002(2) -0.00005(3) Ca 0.0182(3) 0.0215(5) 0.0122(3) 0.000 0.000 -0.0009(2) O1 0.0193(10) 0.0250(11) 0.0088(8) 0.000 0.000 -0.0002(9) O2 0.0184(7) 0.0218(7) 0.0133(6) -0.0012(5) 0.0019(5) -0.0028(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir O1 2.0089(9) 7_656 ? Ir O1 2.0089(9) 3_454 ? Ir O2 2.0228(19) . ? Ir O2 2.0228(19) 5 ? Ir O2 2.0269(18) 8_655 ? Ir O2 2.0269(18) 4_455 ? Ir Ca 3.1283(10) 7_656 ? Ir Ca 3.1283(10) 3_454 ? Ir Ca 3.2419(6) . ? Ir Ca 3.2419(6) 5 ? Ir Ca 3.3877(6) 5_655 ? Ir Ca 3.3877(6) 1_455 ? Ca O1 2.279(3) 7_756 ? Ca O2 2.307(2) 8_655 ? Ca O2 2.307(2) 7_656 ? Ca O1 2.361(3) . ? Ca O2 2.559(2) 2 ? Ca O2 2.559(2) . ? Ca O2 2.6951(19) 3 ? Ca O2 2.6951(19) 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 _geom_angle_publ_flag O1 Ir O1 180.0 7_656 3_454 ? O1 Ir O2 91.94(9) 7_656 . ? O1 Ir O2 88.06(9) 3_454 . ? O1 Ir O2 88.06(9) 7_656 5 ? O1 Ir O2 91.94(9) 3_454 5 ? O2 Ir O2 180.0 . 5 ? O1 Ir O2 88.92(9) 7_656 8_655 ? O1 Ir O2 91.08(9) 3_454 8_655 ? O2 Ir O2 90.32(3) . 8_655 ? O2 Ir O2 89.68(3) 5 8_655 ? O1 Ir O2 91.08(9) 7_656 4_455 ? O1 Ir O2 88.92(9) 3_454 4_455 ? O2 Ir O2 89.68(3) . 4_455 ? O2 Ir O2 90.32(3) 5 4_455 ? O2 Ir O2 180.00(6) 8_655 4_455 ? O1 Ir Ca 48.99(8) 7_656 7_656 ? O1 Ir Ca 131.01(8) 3_454 7_656 ? O2 Ir Ca 121.51(5) . 7_656 ? O2 Ir Ca 58.49(5) 5 7_656 ? O2 Ir Ca 54.60(5) 8_655 7_656 ? O2 Ir Ca 125.40(5) 4_455 7_656 ? O1 Ir Ca 131.01(8) 7_656 3_454 ? O1 Ir Ca 48.99(8) 3_454 3_454 ? O2 Ir Ca 58.49(5) . 3_454 ? O2 Ir Ca 121.51(5) 5 3_454 ? O2 Ir Ca 125.40(5) 8_655 3_454 ? O2 Ir Ca 54.60(5) 4_455 3_454 ? Ca Ir Ca 180.00(4) 7_656 3_454 ? O1 Ir Ca 70.41(8) 7_656 . ? O1 Ir Ca 109.59(8) 3_454 . ? O2 Ir Ca 52.12(6) . . ? O2 Ir Ca 127.88(6) 5 . ? O2 Ir Ca 44.97(5) 8_655 . ? O2 Ir Ca 135.03(5) 4_455 . ? Ca Ir Ca 72.285(16) 7_656 . ? Ca Ir Ca 107.715(16) 3_454 . ? O1 Ir Ca 109.59(8) 7_656 5 ? O1 Ir Ca 70.41(8) 3_454 5 ? O2 Ir Ca 127.88(6) . 5 ? O2 Ir Ca 52.12(6) 5 5 ? O2 Ir Ca 135.03(5) 8_655 5 ? O2 Ir Ca 44.97(5) 4_455 5 ? Ca Ir Ca 107.715(16) 7_656 5 ? Ca Ir Ca 72.285(16) 3_454 5 ? Ca Ir Ca 180.0 . 5 ? O1 Ir Ca 139.31(8) 7_656 5_655 ? O1 Ir Ca 40.69(8) 3_454 5_655 ? O2 Ir Ca 77.12(5) . 5_655 ? O2 Ir Ca 102.88(5) 5 5_655 ? O2 Ir Ca 52.70(5) 8_655 5_655 ? O2 Ir Ca 127.30(5) 4_455 5_655 ? Ca Ir Ca 104.216(18) 7_656 5_655 ? Ca Ir Ca 75.784(18) 3_454 5_655 ? Ca Ir Ca 72.131(10) . 5_655 ? Ca Ir Ca 107.869(10) 5 5_655 ? O1 Ir Ca 40.69(8) 7_656 1_455 ? O1 Ir Ca 139.31(8) 3_454 1_455 ? O2 Ir Ca 102.88(5) . 1_455 ? O2 Ir Ca 77.12(5) 5 1_455 ? O2 Ir Ca 127.30(5) 8_655 1_455 ? O2 Ir Ca 52.70(5) 4_455 1_455 ? Ca Ir Ca 75.784(18) 7_656 1_455 ? Ca Ir Ca 104.216(18) 3_454 1_455 ? Ca Ir Ca 107.869(10) . 1_455 ? Ca Ir Ca 72.131(10) 5 1_455 ? Ca Ir Ca 180.00(4) 5_655 1_455 ? O1 Ca O2 104.50(8) 7_756 8_655 ? O1 Ca O2 104.50(8) 7_756 7_656 ? O2 Ca O2 82.40(10) 8_655 7_656 ? O1 Ca O1 87.72(8) 7_756 . ? O2 Ca O1 135.96(6) 8_655 . ? O2 Ca O1 135.96(6) 7_656 . ? O1 Ca O2 135.57(6) 7_756 2 ? O2 Ca O2 118.38(4) 8_655 2 ? O2 Ca O2 72.12(4) 7_656 2 ? O1 Ca O2 70.00(7) . 2 ? O1 Ca O2 135.57(6) 7_756 . ? O2 Ca O2 72.12(4) 8_655 . ? O2 Ca O2 118.38(4) 7_656 . ? O1 Ca O2 70.00(7) . . ? O2 Ca O2 72.85(8) 2 . ? O1 Ca O2 70.21(5) 7_756 3 ? O2 Ca O2 157.04(6) 8_655 3 ? O2 Ca O2 77.64(7) 7_656 3 ? O1 Ca O2 66.94(5) . 3 ? O2 Ca O2 65.79(3) 2 3 ? O2 Ca O2 127.80(5) . 3 ? O1 Ca O2 70.21(5) 7_756 4 ? O2 Ca O2 77.64(7) 8_655 4 ? O2 Ca O2 157.04(6) 7_656 4 ? O1 Ca O2 66.94(5) . 4 ? O2 Ca O2 127.80(5) 2 4 ? O2 Ca O2 65.79(3) . 4 ? O2 Ca O2 118.96(8) 3 4 ? O1 Ca Ir 99.05(6) 7_756 3 ? O2 Ca Ir 156.04(5) 8_655 3 ? O2 Ca Ir 96.03(5) 7_656 3 ? O1 Ca Ir 39.95(3) . 3 ? O2 Ca Ir 40.21(4) 2 3 ? O2 Ca Ir 88.02(5) . 3 ? O2 Ca Ir 39.78(4) 3 3 ? O2 Ca Ir 106.82(6) 4 3 ? O1 Ca Ir 99.05(6) 7_756 4 ? O2 Ca Ir 96.03(5) 8_655 4 ? O2 Ca Ir 156.04(5) 7_656 4 ? O1 Ca Ir 39.95(3) . 4 ? O2 Ca Ir 88.02(5) 2 4 ? O2 Ca Ir 40.21(4) . 4 ? O2 Ca Ir 106.82(6) 3 4 ? O2 Ca Ir 39.78(4) 4 4 ? Ir Ca Ir 75.75(3) 3 4 ? O1 Ca Ir 138.75(4) 7_756 . ? O2 Ca Ir 38.39(5) 8_655 . ? O2 Ca Ir 89.81(5) 7_656 . ? O1 Ca Ir 108.60(6) . . ? O2 Ca Ir 85.53(4) 2 . ? O2 Ca Ir 38.60(4) . . ? O2 Ca Ir 150.97(5) 3 . ? O2 Ca Ir 81.59(4) 4 . ? Ir Ca Ir 117.98(3) 3 . ? Ir Ca Ir 75.035(14) 4 . ? O1 Ca Ir 138.75(4) 7_756 2 ? O2 Ca Ir 89.81(5) 8_655 2 ? O2 Ca Ir 38.39(5) 7_656 2 ? O1 Ca Ir 108.60(6) . 2 ? O2 Ca Ir 38.60(4) 2 2 ? O2 Ca Ir 85.53(4) . 2 ? O2 Ca Ir 81.59(4) 3 2 ? O2 Ca Ir 150.97(5) 4 2 ? Ir Ca Ir 75.035(14) 3 2 ? Ir Ca Ir 117.98(3) 4 2 ? Ir Ca Ir 72.659(16) . 2 ? Ir O1 Ir 145.90(16) 4 3 ? Ir O1 Ca 104.22(8) 4 7_766 ? Ir O1 Ca 104.22(8) 3 7_766 ? Ir O1 Ca 91.06(8) 4 . ? Ir O1 Ca 91.06(8) 3 . ? Ca O1 Ca 119.46(13) 7_766 . ? Ir O2 Ir 146.76(10) . 4 ? Ir O2 Ca 116.59(8) . 7_666 ? Ir O2 Ca 96.63(8) 4 7_666 ? Ir O2 Ca 89.28(7) . . ? Ir O2 Ca 85.19(7) 4 . ? Ca O2 Ca 101.01(6) 7_666 . ? Ir O2 Ca 81.73(6) . 3_454 ? Ir O2 Ca 90.55(7) 4 3_454 ? Ca O2 Ca 102.36(7) 7_666 3_454 ? Ca O2 Ca 156.57(8) . 3_454 ? _refine_diff_density_max 7.930 _refine_diff_density_min -3.245 _refine_diff_density_rms 1.268 _shelx_res_file ; TITL CaIrO3 at 300 K in Pbnm CaIrO3_300K_Pbnm.res created by SHELXL-2018/3 at 16:33:04 on 13-Jun-2018 CELL 0.71073 5.3597 5.6131 7.6824 90 90 90 ZERR 4 0.0005 0.0004 0.0008 0 0 0 LATT 1 SYMM x, y, -z+1/2 SYMM x+1/2, -y+1/2, z+1/2 SYMM x+1/2, -y+1/2, -z SFAC O Ca Ir UNIT 12 4 4 L.S. 10 LIST 6 FMAP 2 PLAN 10 TEMP 27 SIZE 0.14 0.11 0.09 REM Black, Block ACTA WGHT 0.088100 0.155200 EXTI 0.031190 FVAR 0.49287 IR 3 0.000000 0.000000 0.000000 10.50000 0.01457 0.01798 = 0.00746 -0.00002 -0.00002 -0.00005 CA 2 0.483176 0.060376 0.250000 10.50000 0.01821 0.02155 = 0.01215 0.00000 0.00000 -0.00094 O1 1 0.603607 0.464994 0.250000 10.50000 0.01934 0.02501 = 0.00882 0.00000 0.00000 -0.00020 O2 1 0.193341 0.301138 0.052207 11.00000 0.01842 0.02178 = 0.01328 -0.00122 0.00188 -0.00285 HKLF 4 REM CaIrO3 at 300 K in Pbnm REM wR2 = 0.1440, GooF = S = 1.147, Restrained GooF = 1.147 for all data REM R1 = 0.0516 for 690 Fo > 4sig(Fo) and 0.0540 for all 799 data REM 29 parameters refined using 0 restraints END WGHT 0.0881 0.1552 REM Highest difference peak 7.930, deepest hole -3.245, 1-sigma level 1.268 Q1 1 0.1138 -0.1197 -0.0018 11.00000 0.05 7.93 Q2 1 0.1142 0.1203 -0.0015 11.00000 0.05 7.87 Q3 1 -0.0028 -0.0006 -0.0985 11.00000 0.05 7.45 Q4 1 0.2020 0.1956 -0.0005 11.00000 0.05 5.38 Q5 1 0.2980 0.3023 -0.0014 11.00000 0.05 5.33 Q6 1 0.1097 -0.0024 -0.0702 11.00000 0.05 4.87 Q7 1 -0.0046 0.1032 -0.0006 11.00000 0.05 4.31 Q8 1 0.1574 -0.0001 0.0160 11.00000 0.05 4.07 Q9 1 -0.0005 -0.1387 -0.0473 11.00000 0.05 3.68 Q10 1 -0.0008 0.1407 -0.0480 11.00000 0.05 3.63 ; _shelx_res_checksum 93165 _shelx_hkl_file ; 0 0 1 4.81 1.121661 0 0 1 3.75 0.981951 0 0 1 3.15 0.702256 0 0 -1 1.41 0.30 171 0 0 -1 1.65 0.44 758 0 0 -1 1.30 0.463104 0 0 210390.13 350.171667 0 0 211722.82 445.191957 0 0 212202.88 433.892263 0 0 3 3.44 2.131673 0 0 3 7.45 2.311962 0 0 3 6.70 1.512269 0 0 3 6.32 1.332544 0 0 -3 2.80 0.88 189 0 0 -3 1.18 0.92 467 0 0 -3 2.36 1.02 769 0 0 -3 4.18 1.263115 0 0 412792.39 414.851417 0 0 417043.53 686.271679 0 0 421719.69 782.332276 0 0 -411720.62 409.06 199 0 0 -412458.38 431.07 473 0 0 -415685.34 557.483121 0 0 5 0.55 1.631424 0 0 5 -0.99 2.131685 0 0 5 -2.36 1.402282 0 0 5 0.99 1.002573 0 0 -5 -0.29 0.83 210 0 0 -5 1.33 1.25 479 0 0 -5 -0.40 1.21 780 0 0 -5 -0.45 1.853127 0 0 6 3085.35 124.591429 0 0 6 4870.45 224.162289 0 0 -6 3316.60 120.57 220 0 0 -6 3359.42 135.01 485 0 0 -6 3358.13 134.12 785 0 0 -6 4455.38 174.733132 0 0 7 0.01 1.861435 0 0 7 1.67 2.781697 0 0 7 5.61 3.501984 0 0 7 2.47 1.902296 0 0 -7 -0.54 1.78 491 0 0 -7 3.13 2.28 791 0 0 -7 -0.08 2.403138 0 0 8 7465.62 308.521703 0 0 8 5386.02 234.372303 0 0 -8 6619.71 226.06 243 0 0 -8 5460.93 218.28 497 0 0 -8 6063.82 218.95 797 0 0 -8 5802.50 224.951083 0 0 -8 8245.76 308.253144 0 0 9 -0.94 3.491710 0 0 9 2.99 3.251995 0 0 9 -0.83 1.232311 0 0 -9 -0.46 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