#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2011731.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_2011731 loop_ _publ_author_name 'Kashino, Setsuo' 'Ishida, Hiroyuki' 'Fukunaga, Takeo' 'Oishi, Shuji' _publ_section_title ; A new polymorph of barium chloroanilate trihydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 18 _journal_page_last 19 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ba (C6 Cl2 O4)] , 3H2 O' _chemical_formula_moiety 'Ba 2+ , C6 Cl2 O4 2- , 3H2 O' _chemical_formula_sum 'C6 H6 Ba Cl2 O7' _chemical_formula_weight 398.35 _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_type_scat_source IntTabC _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.258(4) _cell_length_b 17.614(4) _cell_length_c 6.925(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 11.0 _cell_measurement_theta_min 10.2 _cell_volume 2105.1(9) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1990) ; _computing_data_reduction 'TEXSAN for Windows (Molecular Structure corporation, 1997-1999)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_refinement 'TEXSAN for Windows' _computing_structure_solution 'DIRDIF92 (Beurskens et al., 1992)' _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Rigaku AFC-5R' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .023 _diffrn_reflns_av_sigmaI/netI .036 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 3563 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 4.0 _diffrn_standards_decay_% none _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.29 _exptl_absorpt_correction_T_max .680 _exptl_absorpt_correction_T_min .351 _exptl_absorpt_correction_type '\y scans' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.514 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 1504 _exptl_crystal_size_max .46 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .09 _refine_diff_density_max 2.60 _refine_diff_density_min -1.78 _refine_ls_extinction_coef '2.14(7) \\times 10^-6^' _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_goodness_of_fit_all 1.608 _refine_ls_goodness_of_fit_ref 1.670 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 146 _refine_ls_number_reflns 2110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .071 _refine_ls_R_factor_gt .060 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all .067 _refine_ls_wR_factor_ref .065 _reflns_number_gt 2110 _reflns_number_total 2415 _reflns_threshold_expression I>0.5\s(I) _[local]_cod_data_source_file oa1107.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'C6 H6 Ba Cl2 O7 ' _cod_original_cell_volume 2105.1(8) _cod_database_code 2011731 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +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_occupancy Ba1 .424214(18) .543160(16) .25324(5) .01760(10) Uani d 1.000 Cl1 .24079(8) .27894(8) .2144(2) .0227(3) Uani d 1.000 Cl2 .58369(8) .28470(8) .5382(2) .0226(4) Uani d 1.000 O1 .4889(3) .1502(2) .4384(6) .0240(11) Uani d 1.000 O2 .3428(3) .1458(2) .3072(7) .0264(11) Uani d 1.000 O3 .3411(3) .4124(2) .2794(6) .0236(11) Uani d 1.000 O4 .4814(2) .4171(2) .4422(6) .0210(10) Uani d 1.000 O5 .2829(3) .5933(3) .1033(7) .0344(13) Uani d 1.000 O6 .3102(3) .5448(2) .5604(8) .0365(14) Uani d 1.000 O7 .5831(3) .5065(2) .1349(7) .0251(11) Uani d 1.000 C1 .4562(3) .2122(3) .4117(8) .0174(13) Uani d 1.000 C2 .3717(3) .2095(3) .3346(8) .0165(13) Uani d 1.000 C3 .3351(3) .2795(3) .2986(7) .0150(12) Uani d 1.000 C4 .3706(3) .3503(3) .3196(8) .0162(13) Uani d 1.000 C5 .4535(3) .3520(3) .4099(8) .0169(13) Uani d 1.000 C6 .4897(3) .2838(3) .4477(8) .0173(13) Uani d 1.000 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 .0124(2) .0195(2) .0208(2) -.00157(11) -.00172(16) .00032(13) Cl1 .0099(6) .0292(6) .0292(7) -.0012(5) -.0046(6) .0001(6) Cl2 .0086(6) .0309(7) .0284(8) .0012(6) -.0032(6) -.0031(6) O1 .019(2) .0230(19) .030(2) .0059(17) .002(2) -.0022(17) O2 .020(2) .021(2) .039(3) -.0007(17) -.005(2) -.0038(18) O3 .016(2) .0201(19) .034(3) .0000(15) -.0049(19) .0028(17) O4 .014(2) .0221(19) .027(2) -.0021(16) -.0109(19) -.0007(16) O5 .022(3) .049(3) .032(3) .013(2) -.002(2) .001(2) O6 .028(3) .037(3) .045(3) .004(2) .006(3) -.004(2) O7 .020(2) .025(2) .031(2) -.0024(17) .002(2) -.0002(18) C1 .019(3) .021(3) .012(3) .001(2) .008(2) -.0019(19) C2 .013(3) .021(3) .015(3) .000(2) .003(2) -.001(2) C3 .011(3) .021(2) .013(2) -.001(2) .000(2) -.003(2) C4 .009(3) .021(3) .018(3) .004(2) .001(2) -.004(2) C5 .009(3) .023(3) .018(3) -.001(2) .006(2) .003(2) C6 .011(3) .027(3) .014(3) .000(2) -.003(2) .000(2) 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 _geom_angle_publ_flag O1 Ba1 O3 3_655 . 154.20(17) no O1 Ba1 O4 3_655 . 125.82(16) no O1 Ba1 O4 3_655 5_666 82.69(16) no O1 Ba1 O5 3_655 . 94.56(17) no O1 Ba1 O6 3_655 . 135.85(16) no O1 Ba1 O7 3_655 . 60.42(15) no O1 Ba1 O7 3_655 5_665 77.18(16) no O3 Ba1 O4 . . 58.39(15) no O3 Ba1 O4 . 5_666 118.44(15) no O3 Ba1 O5 . . 80.34(17) no O3 Ba1 O6 . . 66.51(16) no O3 Ba1 O7 . . 109.00(15) no O3 Ba1 O7 . 5_665 77.15(16) no O4 Ba1 O4 . 5_666 68.30(16) no O4 Ba1 O5 . . 137.99(17) no O4 Ba1 O6 . . 84.43(16) no O4 Ba1 O7 . . 67.74(15) no O4 Ba1 O7 . 5_665 102.55(15) no O4 Ba1 O5 5_666 . 136.05(16) no O4 Ba1 O6 5_666 . 80.60(18) no O4 Ba1 O7 5_666 . 73.58(16) no O4 Ba1 O7 5_666 5_665 146.33(16) no O5 Ba1 O6 . . 71.16(18) no O5 Ba1 O7 . . 141.40(17) no O5 Ba1 O7 . 5_665 72.89(17) no O6 Ba1 O7 . . 147.34(18) no O6 Ba1 O7 . 5_665 132.07(18) no O7 Ba1 O7 . 5_665 73.05(18) no Ba1 O4 Ba1 . 5_666 111.70(16) yes Ba1 O7 Ba1 . 5_665 106.95(18) yes O5 O2 O7 6_545 3_645 98.0(2) no O5 O6 O7 4_565 5_666 90.9(2) no O2 O5 O6 6_555 4_564 84.1(2) no O2 O7 O6 3_655 5_666 83.1(2) no O1 O7 O2 3_655 3_655 56.5(2) no O1 C1 C2 . . 116.8(6) yes O1 C1 C6 . . 125.0(7) yes C2 C1 C6 . . 118.3(6) yes O2 C2 C1 . . 117.2(6) yes O2 C2 C3 . . 125.7(7) yes C1 C2 C3 . . 117.1(6) yes Cl1 C3 C2 . . 118.6(5) yes Cl1 C3 C4 . . 116.9(6) yes C2 C3 C4 . . 124.5(6) yes O3 C4 C3 . . 125.7(7) yes O3 C4 C5 . . 116.7(6) yes C3 C4 C5 . . 117.5(6) yes O4 C5 C4 . . 116.0(6) yes O4 C5 C6 . . 125.7(7) yes C4 C5 C6 . . 118.3(6) yes Cl2 C6 C1 . . 117.1(5) yes Cl2 C6 C5 . . 118.9(6) yes C1 C6 C5 . . 124.0(7) yes 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 O1 3_655 2.750(5) yes Ba1 O3 . 2.719(5) yes Ba1 O4 . 2.760(5) yes Ba1 O4 5_666 2.755(5) yes Ba1 O5 . 2.794(6) yes Ba1 O6 . 2.898(7) yes Ba1 O7 . 2.934(6) yes Ba1 O7 5_665 2.829(6) yes Cl1 C3 . 1.729(7) yes Cl2 C6 . 1.738(7) yes O1 C1 . 1.244(8) yes O2 C2 . 1.242(8) yes O3 C4 . 1.239(8) yes O4 C5 . 1.263(8) yes C1 C2 . 1.553(10) yes C1 C6 . 1.410(10) yes C2 C3 . 1.407(10) yes C3 C4 . 1.397(10) yes C4 C5 . 1.561(10) yes C5 C6 . 1.379(9) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O2 O5 2.750(8) 6_545 yes O2 O7 2.795(7) 3_645 yes O1 O7 2.865(7) 3_645 yes O6 O5 2.931(9) 4_565 yes O6 O7 2.943(9) 5_666 yes O1 C5 3.322(9) 7 yes C5 O2 3.349(9) 7 yes C6 C1 3.266(10) 7 yes C6 C2 3.368(10) 7 yes C2 C3 3.280(10) 7 yes Cl2 Cl1 3.228(3) 8 yes Cl2 Cl1 3.398(3) 2_556 yes 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_publ_flag Cl1 C3 C2 O2 1.7(10) no Cl1 C3 C2 C1 -179.5(5) no Cl1 C3 C4 O3 -1.6(10) no Cl1 C3 C4 C5 175.6(5) no Cl2 C6 C1 O1 -.6(10) no Cl2 C6 C1 C2 178.8(5) no Cl2 C6 C5 O4 -2.9(10) no Cl2 C6 C5 C4 177.2(5) no O1 C1 C2 O2 .7(10) no O1 C1 C2 C3 -178.2(6) no O1 C1 C6 C5 177.3(7) no O2 C2 C1 C6 -178.8(7) no O2 C2 C3 C4 -175.9(8) no O3 C4 C3 C2 176.0(7) no O3 C4 C5 O4 3.2(10) no O3 C4 C5 C6 -176.8(7) no O4 C5 C4 C3 -174.2(6) no O4 C5 C6 C1 179.2(7) no C1 C2 C3 C4 2.9(10) no C1 C6 C5 C4 -.7(10) no C2 C1 C6 C5 -3.2(10) no C2 C3 C4 C5 -6.8(10) no C3 C2 C1 C6 2.3(9) no C3 C4 C5 C6 5.7(10) no