#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/10/2011082.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_2011082 loop_ _publ_author_name 'Figgis, Brian N.' 'Reynolds, Philip A.' 'Sobolev, Alexandre N.' _publ_section_title ; The structures of the \a-alums RbCr(SO~4~)~2~·12H~2~O and CsCr(SeO~4~)~2~·12H~2~O at 293 and 12K ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 731 _journal_page_last 734 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'Cs Cr (Se O4)2, 12H2 O' _chemical_formula_sum 'Cr Cs H24 O20 Se2' _chemical_formula_weight 687.02 _chemical_name_common 'Caesium chromium bis(selenate) dodecahydrate' _chemical_name_systematic ; Chromium alpha-Alums ; _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.522(3) _cell_length_b 12.522(3) _cell_length_c 12.522(3) _cell_measurement_reflns_used 14 _cell_measurement_temperature 12(2) _cell_measurement_theta_max 17.15 _cell_measurement_theta_min 16.47 _cell_volume 1963.5(8) _computing_cell_refinement 'Local diffractometer control software' _computing_data_collection 'Local diffractometer control software' _computing_data_reduction 'PROFIT (Streltsov & Zavodnik, 1989)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1983)' _computing_publication_material 'SHELXTL (Sheldrick, 1983)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 12(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Huber 512 goniometer' _diffrn_measurement_method '\w-2\q scan' _diffrn_radiation_monochromator none _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0326 _diffrn_reflns_av_sigmaI/netI .0151 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 4443 _diffrn_reflns_theta_full 29.98 _diffrn_reflns_theta_max 29.98 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% .5 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.202 _exptl_absorpt_correction_T_max .1879 _exptl_absorpt_correction_T_min .1315 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'XTAL 3.4 (Hall, King & Stewart, 1994)' _exptl_crystal_colour 'Dark Violet' _exptl_crystal_density_diffrn 2.324 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 1324 _exptl_crystal_size_max .65 _exptl_crystal_size_mid .64 _exptl_crystal_size_min .63 _refine_diff_density_max .463 _refine_diff_density_min -.454 _refine_ls_extinction_coef .0092(3) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.309 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 963 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.307 _refine_ls_R_factor_all .0203 _refine_ls_R_factor_gt .0186 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+2.1334P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0417 _reflns_number_gt 916 _reflns_number_total 963 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file br1280.cif _[local]_cod_data_source_block IIb _[local]_cod_chemical_formula_sum_orig 'H24 Cr Cs O20 Se2' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011082 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' 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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cs .0000 .0000 .0000 .00401(8) Uani d S 1 . . Cs Cr .5000 .5000 .5000 .00283(13) Uani d S 1 . . Cr Se .182558(13) .182558(13) .182558(13) .00297(9) Uani d S 1 . . Se O1 .25820(10) .25820(10) .25820(10) .0077(4) Uani d S 1 . . O O2 .06066(10) .17818(11) .23076(10) .0066(2) Uani d . 1 . . O O11 -.14282(11) .20648(11) .04845(11) .0074(2) Uani d D 1 . . O O12 .34334(11) .49408(11) .50842(11) .0060(2) Uani d D 1 . . O H1 -.164(3) .208(4) .1128(14) .069(15) Uiso d D 1 . . H H2 -.1937(18) .221(3) .007(2) .024(8) Uiso d D 1 . . H H3 .313(2) .478(3) .5664(15) .033(9) Uiso d D 1 . . H H4 .299(2) .483(3) .458(2) .033(9) Uiso d D 1 . . H 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 Cs .00401(8) .00401(8) .00401(8) .00036(5) .00036(5) .00036(5) Cr .00283(13) .00283(13) .00283(13) -.00016(13) -.00016(13) -.00016(13) Se .00297(9) .00297(9) .00297(9) .00020(6) .00020(6) .00020(6) O1 .0077(4) .0077(4) .0077(4) -.0016(4) -.0016(4) -.0016(4) O2 .0042(5) .0070(5) .0087(6) .0007(5) .0034(5) .0015(5) O11 .0060(5) .0090(6) .0073(6) -.0001(5) -.0002(5) .0010(5) O12 .0041(6) .0089(6) .0049(6) -.0009(4) -.0002(4) .0002(5) 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 Cs O11 9 3.202(2) no Cs O11 5 3.202(2) no Cs O11 21 3.202(2) no Cs O11 . 3.202(2) yes Cs O11 17 3.202(2) no Cs O11 13 3.202(2) no Cs O2 21 3.729(2) no Cs O2 17 3.729(2) no Cs O2 13 3.729(2) no Cs O2 . 3.729(2) yes Cs O2 9 3.729(2) no Cs O2 5 3.729(2) no Cr O12 . 1.9660(10) yes Cr O12 5 1.9660(10) no Cr O12 21_666 1.9660(10) no Cr O12 13_666 1.9660(10) no Cr O12 17_666 1.9660(10) no Cr O12 9 1.9660(10) no Se O1 . 1.641(2) yes Se O2 . 1.6420(10) yes Se O2 9 1.6420(10) no Se O2 5 1.6420(10) no O11 H1 . .849(10) no O11 H2 . .844(10) no O12 H3 . .844(10) no O12 H4 . .849(10) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -.3680 2.1192 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 Cs O11 . 17 66.18(2) yes O11 Cs O11 . 5 113.82(2) yes O11 Cs O11 9 5 113.82(2) no O11 Cs O11 9 21 180.00(5) no O11 Cs O11 5 21 66.18(2) no O11 Cs O11 9 . 113.82(2) no O11 Cs O11 21 . 66.18(2) no O11 Cs O11 9 17 66.18(2) no O11 Cs O11 5 17 180.00(4) no O11 Cs O11 21 17 113.82(2) no O11 Cs O11 9 13 66.18(2) no O11 Cs O11 5 13 66.18(2) no O11 Cs O11 21 13 113.82(2) no O11 Cs O11 . 13 180.00(4) no O11 Cs O11 17 13 113.82(2) no O11 Cs O2 . . 58.92(3) yes O11 Cs O2 9 21 121.08(3) no O11 Cs O2 5 21 81.08(3) no O11 Cs O2 21 21 58.92(3) no O11 Cs O2 . 21 109.28(3) no O11 Cs O2 17 21 98.92(3) no O11 Cs O2 13 21 70.72(3) no O11 Cs O2 9 17 109.28(3) no O11 Cs O2 5 17 121.08(3) no O11 Cs O2 21 17 70.72(3) no O11 Cs O2 . 17 81.08(3) no O11 Cs O2 17 17 58.92(3) no O11 Cs O2 13 17 98.92(3) no O11 Cs O2 9 13 81.08(3) no O11 Cs O2 5 13 109.28(3) no O11 Cs O2 21 13 98.92(3) no O11 Cs O2 . 13 121.08(3) no O11 Cs O2 17 13 70.72(3) no O11 Cs O2 13 13 58.92(3) no O11 Cs O2 9 . 98.92(3) no O11 Cs O2 5 . 70.72(3) no O11 Cs O2 21 . 81.08(3) no O11 Cs O2 17 . 109.28(3) no O11 Cs O2 13 . 121.08(3) no O11 Cs O2 9 9 58.92(3) no O11 Cs O2 5 9 98.92(3) no O11 Cs O2 21 9 121.08(3) no O11 Cs O2 . 9 70.72(3) no O11 Cs O2 17 9 81.08(3) no O11 Cs O2 13 9 109.28(3) no O11 Cs O2 9 5 70.72(3) no O11 Cs O2 5 5 58.92(3) no O11 Cs O2 21 5 109.28(3) no O11 Cs O2 . 5 98.92(3) no O11 Cs O2 17 5 121.08(3) no O11 Cs O2 13 5 81.08(3) no O2 Cs O2 . 5 41.98(3) yes O2 Cs O2 21 13 41.98(3) no O2 Cs O2 17 13 41.98(3) no O2 Cs O2 9 5 41.98(3) no O2 Cs O2 21 17 41.98(3) no O2 Cs O2 21 5 138.02(3) no O2 Cs O2 17 5 180.00(4) no O2 Cs O2 13 5 138.02(3) no O2 Cs O2 21 9 180.00(3) no O2 Cs O2 17 9 138.02(3) no O2 Cs O2 13 9 138.02(3) no O2 Cs O2 . 9 41.98(3) no O2 Cs O2 21 . 138.02(3) no O2 Cs O2 17 . 138.02(3) no O2 Cs O2 13 . 180.0 no O12 Cr O12 . 17_666 88.97(5) yes O12 Cr O12 . 5 91.03(5) yes O12 Cr O12 . 21_666 88.97(5) no O12 Cr O12 5 21_666 88.97(5) no O12 Cr O12 . 13_666 180.0 no O12 Cr O12 5 13_666 88.97(5) no O12 Cr O12 21_666 13_666 91.03(5) no O12 Cr O12 5 17_666 180.0 no O12 Cr O12 21_666 17_666 91.03(5) no O12 Cr O12 13_666 17_666 91.03(5) no O12 Cr O12 . 9 91.03(5) no O12 Cr O12 5 9 91.03(5) no O12 Cr O12 21_666 9 180.0 no O12 Cr O12 13_666 9 88.97(5) no O12 Cr O12 17_666 9 88.97(5) no O1 Se O2 . . 110.10(5) yes O1 Se O2 . 5 110.10(5) yes O1 Se O2 . 9 110.10(5) no O2 Se O2 . 9 108.83(5) no O2 Se O2 . 5 108.83(5) no O2 Se O2 9 5 108.83(5) no O1 Se Cs . . 180.00(4) no O2 Se Cs . . 69.90(5) no O2 Se Cs 9 . 69.90(5) no O2 Se Cs 5 . 69.90(5) no Se O2 Cs . . 85.67(5) no Cs O11 H1 . . 112(3) no Cs O11 H2 . . 119(2) no H1 O11 H2 . . 110(4) no Cr O12 H3 . . 120(2) no Cr O12 H4 . . 128(2) no H3 O12 H4 . . 108(3) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O11 H1 O1 14_556 .849(10) 1.99(2) 2.796(2) 158(4) O11 H2 O2 11_455 .844(10) 1.910(12) 2.740(2) 167(3) O12 H3 O2 20_566 .844(10) 1.804(11) 2.641(2) 171(3) O12 H4 O11 22_566 .849(10) 1.761(10) 2.609(2) 176(3)