#------------------------------------------------------------------------------ #$Date: 2014-11-26 15:25:09 +0200 (Wed, 26 Nov 2014) $ #$Revision: 127915 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/02/4030260.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_4030260 loop_ _publ_author_name 'Hiltunen, L.' 'Holsa, J.' _publ_section_title ; Structural study of praseodynium oxalate halide trihydrates ; _journal_name_full 'European Journal of Solid State and Inorganic Chemistry' _journal_page_first 401 _journal_page_last 410 _journal_volume 27 _journal_year 1990 _chemical_formula_sum 'C2 H6 Br O7 Pr' _chemical_formula_weight 362.83 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 104.28(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.941(1) _cell_length_b 16.260(7) _cell_length_c 8.494(4) _cell_volume 795.2(5) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 10.75 _exptl_crystal_density_diffrn 3.031 _exptl_crystal_F_000 648 _refine_ls_number_parameters 100 _refine_ls_number_reflns 1974 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_gt 0.0383 _[local]_cod_data_source_file EJSSIC-1990-27-401-410-2.cif _[local]_cod_data_source_block PcC2O4Br-3H2O _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 4030260 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Pr Pr Uiso 0.02450(5) 0.10142(2) 0.32819(4) 1.000 0.0127(2) Br Br Uiso 0.22680(10) 0.26926(4) 0.28139(8) 1.000 0.0213(3) O1 O Uiso -0.2192(7) 0.0228(3) 0.4846(5) 1.000 0.0195(19) O2 O Uiso 0.1287(9) 0.0951(3) 0.0599(6) 1.000 0.020(2) O3 O Uiso 0.4422(8) 0.0765(3) 0.3527(6) 1.000 0.033(2) O4 O Uiso -0.0818(9) -0.0290(3) 0.1766(5) 1.000 0.023(2) O11 O Uiso 0.1998(8) 0.1450(3) 0.6181(6) 1.000 0.021(2) O12 O Uiso -0.2147(8) 0.2112(3) 0.4148(6) 1.000 0.025(2) O13 O Uiso -0.3371(9) 0.1337(4) 0.1066(6) 1.000 0.034(3) C1 C Uiso -0.4387(10) 0.0292(4) 0.4514(8) 1.000 0.020(3) C2 C Uiso 0.0613(11) 0.0361(4) -0.0333(7) 1.000 0.018(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 ' 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' Pr Pr -0.2180 2.8214 ' 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 _geom_angle_publ_flag Br Pr O1 144.44(11) . . yes Br Pr O2 74.00(12) . . yes Br Pr O3 74.80(12) . . yes Br Pr O4 139.12(11) . . yes Br Pr O11 78.17(12) . . yes Br Pr O12 70.76(12) . . yes Br Pr O13 90.40(15) . . yes Br Pr O1 129.22(10) . 3_556 yes O1 Pr O2 139.09(16) . . yes O1 Pr O3 124.31(16) . . yes O1 Pr O4 74.70(16) . . yes O1 Pr O11 77.43(15) . . yes O1 Pr O12 76.52(16) . . yes O1 Pr O13 90.26(16) . . yes O1 Pr O1 61.55(14) . 3_556 yes O2 Pr O3 66.54(17) . . yes O2 Pr O4 65.25(16) . . yes O2 Pr O11 139.70(17) . . yes O2 Pr O12 125.59(16) . . yes O2 Pr O13 71.81(17) . . yes O1 Pr O2 110.17(15) 3_556 . yes O3 Pr O4 91.45(17) . . yes O3 Pr O11 78.46(16) . . yes O3 Pr O12 136.32(16) . . yes O3 Pr O13 138.16(17) . . yes O1 Pr O3 62.91(15) 3_556 . yes O4 Pr O11 137.44(15) . . yes O4 Pr O12 132.23(17) . . yes O4 Pr O13 74.41(19) . . yes O1 Pr O4 71.20(15) 3_556 . yes O11 Pr O12 68.96(16) . . yes O11 Pr O13 137.30(17) . . yes O1 Pr O11 67.38(15) 3_556 . yes O12 Pr O13 68.42(18) . . yes O1 Pr O12 124.20(15) 3_556 . yes O1 Pr O13 140.02(18) 3_556 . yes Pr O1 C1 122.0(4) . . yes Pr O1 Pr 118.45(17) . 3_556 yes Pr O1 C1 117.9(4) 3_556 . yes Pr O2 C2 119.8(4) . . yes Pr O3 C1 124.0(4) . 1_655 yes Pr O4 C2 120.5(4) . 3_555 yes O1 C1 O3 126.3(6) . 1_455 yes O1 C1 C1 115.0(5) . 3_456 yes O3 C1 C1 118.7(6) 1_455 3_456 yes O2 C2 O4 126.4(6) . 3_555 yes O2 C2 C2 117.1(5) . 3_555 yes O4 C2 C2 116.6(5) 3_555 3_555 yes 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 Pr Br 3.0473(16) . yes Pr O1 2.539(5) . yes Pr O2 2.507(5) . yes Pr O3 2.472(5) . yes Pr O4 2.481(5) . yes Pr O11 2.527(5) . yes Pr O12 2.503(5) . yes Pr O13 2.537(5) . yes Pr O1 2.653(5) 3_556 yes O1 C1 1.269(8) . yes O2 C2 1.245(8) . yes O3 C1 1.226(8) 1_655 yes O4 C2 1.258(7) 3_555 yes C1 C1 1.553(9) 3_456 no C2 C2 1.560(9) 3_555 no 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_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br Pr O1 C1 76.3(5) . . . no Br Pr O1 Pr -118.60(17) . . 3_556 no O2 Pr O1 C1 -76.6(5) . . . no O2 Pr O1 Pr 88.5(3) . . 3_556 no O3 Pr O1 C1 -169.6(4) . . . no O3 Pr O1 Pr -4.5(3) . . 3_556 no O4 Pr O1 C1 -88.5(5) . . . no O4 Pr O1 Pr 76.6(2) . . 3_556 no O11 Pr O1 C1 124.0(5) . . . no O11 Pr O1 Pr -70.90(19) . . 3_556 no O12 Pr O1 C1 53.0(5) . . . no O12 Pr O1 Pr -141.9(2) . . 3_556 no O13 Pr O1 C1 -14.8(5) . . . no O13 Pr O1 Pr 150.4(2) . . 3_556 no O1 Pr O1 C1 -165.1(5) 3_556 . . no O1 Pr O1 Pr -0.02(14) 3_556 . 3_556 no Br Pr O2 C2 -169.1(5) . . . no O1 Pr O2 C2 -5.1(6) . . . no O3 Pr O2 C2 110.9(5) . . . no O4 Pr O2 C2 7.6(5) . . . no O11 Pr O2 C2 142.8(5) . . . no O12 Pr O2 C2 -117.9(5) . . . no O13 Pr O2 C2 -73.2(5) . . . no O1 Pr O2 C2 64.4(5) 3_556 . . no Br Pr O3 C1 140.5(5) . . 1_655 no O1 Pr O3 C1 -6.1(6) . . 1_655 no O2 Pr O3 C1 -140.6(6) . . 1_655 no O4 Pr O3 C1 -78.5(5) . . 1_655 no O11 Pr O3 C1 59.8(5) . . 1_655 no O12 Pr O3 C1 101.7(5) . . 1_655 no O13 Pr O3 C1 -146.5(5) . . 1_655 no O1 Pr O3 C1 -10.5(5) 3_556 . 1_655 no Br Pr O4 C2 -2.8(6) . . 3_555 no O1 Pr O4 C2 163.8(5) . . 3_555 no O2 Pr O4 C2 -7.7(5) . . 3_555 no O3 Pr O4 C2 -71.0(5) . . 3_555 no O11 Pr O4 C2 -145.4(5) . . 3_555 no O12 Pr O4 C2 108.9(5) . . 3_555 no O13 Pr O4 C2 69.1(5) . . 3_555 no O1 Pr O4 C2 -131.6(5) 3_556 . 3_555 no Br Pr O1 Pr 138.76(13) . 3_556 3_556 no Br Pr O1 C1 -27.0(5) . 3_556 3_556 no O1 Pr O1 Pr 0.02(15) . 3_556 3_556 no O1 Pr O1 C1 -165.7(5) . 3_556 3_556 no O2 Pr O1 Pr -135.79(19) . 3_556 3_556 no O2 Pr O1 C1 58.5(5) . 3_556 3_556 no O3 Pr O1 Pr 175.8(3) . 3_556 3_556 no O3 Pr O1 C1 10.1(4) . 3_556 3_556 no O4 Pr O1 Pr -82.4(2) . 3_556 3_556 no O4 Pr O1 C1 111.9(5) . 3_556 3_556 no O11 Pr O1 Pr 87.6(2) . 3_556 3_556 no O11 Pr O1 C1 -78.1(4) . 3_556 3_556 no O12 Pr O1 Pr 46.5(3) . 3_556 3_556 no O12 Pr O1 C1 -119.3(4) . 3_556 3_556 no O13 Pr O1 Pr -50.4(3) . 3_556 3_556 no O13 Pr O1 C1 143.9(4) . 3_556 3_556 no Pr O1 C1 O3 -5.8(9) . . 1_455 no Pr O1 C1 C1 174.6(4) . . 3_456 no Pr O1 C1 O3 -170.9(5) 3_556 . 1_455 no Pr O1 C1 C1 9.5(7) 3_556 . 3_456 no Pr O2 C2 O4 172.8(5) . . 3_555 no Pr O2 C2 C2 -7.0(8) . . 3_555 no Pr O3 C1 O1 -169.3(5) . 1_655 1_655 no Pr O3 C1 C1 10.2(8) . 1_655 3_556 no Pr O4 C2 C2 7.4(8) . 3_555 . no Pr O4 C2 O2 -172.8(5) . 3_555 3_555 no O1 C1 C1 O1 -180.0(6) . 3_456 3_456 no O1 C1 C1 O3 -0.4(9) . 3_456 3_556 no O2 C2 C2 O4 -0.2(9) . 3_555 . no O2 C2 C2 O2 180.0(6) . 3_555 3_555 no O4 C2 C2 O4 180.0(6) 3_555 3_555 . no