#------------------------------------------------------------------------------ #$Date: 2008-03-30 13:21:05 +0300 (Sun, 30 Mar 2008) $ #$Revision: 321 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2203958.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_2203958 loop_ _publ_author_name 'Rempfer, Nora' 'Lerner, Hans-Wolfram' 'Bolte, Michael' _publ_section_title ; The ammonium chromium(III) alum NH~4~Cr(SO~4~)~2~.12H~2~O ; _journal_issue 7 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i80 _journal_page_last i81 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'N H4 Cr (S O 4)2, 12H2 O' _chemical_formula_moiety 'N H4 1+, Cr (H 2 O)6 3+, ( S O4 2-)2, 6(H2 O)' _chemical_formula_structural '(N H4) Cr (H 2 O)6 (S O 4)2 (H2 O)6' _chemical_formula_sum 'Cr H28 N O20 S2' _chemical_formula_weight 478.35 _chemical_name_systematic ; ; _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _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 12.2491(12) _cell_length_b 12.2491(12) _cell_length_c 12.2491(12) _cell_measurement_reflns_used 4846 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.6 _cell_measurement_theta_min 3.7 _cell_volume 1837.9(3) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction X-AREA _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Stoe IPDS-II two-circle' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 5024 _diffrn_reflns_theta_full 27.72 _diffrn_reflns_theta_max 27.72 _diffrn_reflns_theta_min 3.72 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_T_max 0.8487 _exptl_absorpt_correction_T_min 0.8054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(MULABS; Spek, 1990; Blessing, 1995)' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1004 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.287 _refine_diff_density_min -0.358 _refine_ls_extinction_coef 0.090(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 714 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0190 _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^)+(0.0348P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0506 _reflns_number_gt 613 _reflns_number_total 714 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm6019.cif 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_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_type_symbol Cr1 0.5000 0.5000 0.5000 0.00994(16) Uani d S 1 Cr N1 1.0000 0.5000 0.5000 0.0323(8) Uani d S 1 N H1 1.012(4) 0.544(3) 0.553(3) 0.039 Uiso d P 0.667 H S1 0.80864(2) 0.69136(2) 0.30864(2) 0.01273(17) Uani d S 1 S O1 0.81058(8) 0.73618(8) 0.41998(8) 0.0252(3) Uani d . 1 O O2 0.73931(8) 0.76069(8) 0.23931(8) 0.0340(5) Uani d S 1 O O3 0.48764(7) 0.51483(7) 0.34114(7) 0.0148(2) Uani d . 1 O H3A 0.4708(16) 0.5712(19) 0.3131(16) 0.035(5) Uiso d . 1 H H3B 0.4803(16) 0.4626(19) 0.2983(18) 0.036(5) Uiso d . 1 H O4 1.04676(9) 0.63817(8) 0.69723(8) 0.0220(2) Uani d . 1 O H4A 1.0075(16) 0.6829(17) 0.7082(16) 0.026(5) Uiso d . 1 H H4B 1.104(2) 0.6663(18) 0.7085(18) 0.039(5) Uiso 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 Cr1 0.00994(16) 0.00994(16) 0.00994(16) -0.00036(8) -0.00036(8) -0.00036(8) N1 0.0323(8) 0.0323(8) 0.0323(8) -0.0160(9) 0.0160(9) -0.0160(9) S1 0.01273(17) 0.01273(17) 0.01273(17) -0.00183(9) 0.00183(9) -0.00183(9) O1 0.0219(4) 0.0348(5) 0.0190(5) -0.0111(4) 0.0042(3) -0.0126(4) O2 0.0340(5) 0.0340(5) 0.0340(5) 0.0085(4) -0.0085(4) 0.0085(4) O3 0.0197(4) 0.0134(4) 0.0114(4) 0.0013(3) -0.0016(3) -0.0003(3) O4 0.0205(5) 0.0188(4) 0.0266(5) 0.0038(4) 0.0060(4) 0.0058(4) 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 Cr1 O3 9 1.9602(9) y Cr1 O3 21_666 1.9602(9) ? Cr1 O3 17_666 1.9602(9) ? Cr1 O3 13_666 1.9602(9) ? Cr1 O3 . 1.9602(9) ? Cr1 O3 5 1.9603(9) ? N1 H1 . 0.85(3) ? S1 O1 . 1.4704(9) y S1 O1 12_664 1.4704(9) ? S1 O1 6_566 1.4704(9) ? S1 O2 . 1.4709(18) y O3 H3A . 0.80(2) ? O3 H3B . 0.83(2) ? O4 H4A . 0.74(2) ? O4 H4B . 0.79(3) ? 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 O3 Cr1 O3 9 21_666 180.0 O3 Cr1 O3 9 17_666 88.71(4) O3 Cr1 O3 21_666 17_666 91.29(4) O3 Cr1 O3 9 13_666 88.71(4) O3 Cr1 O3 21_666 13_666 91.29(4) O3 Cr1 O3 17_666 13_666 91.29(4) O3 Cr1 O3 9 . 91.29(4) O3 Cr1 O3 21_666 . 88.71(4) O3 Cr1 O3 17_666 . 88.71(4) O3 Cr1 O3 13_666 . 180.0 O3 Cr1 O3 9 5 91.29(4) O3 Cr1 O3 21_666 5 88.71(4) O3 Cr1 O3 17_666 5 180.0 O3 Cr1 O3 13_666 5 88.71(4) O3 Cr1 O3 . 5 91.29(4) O1 S1 O1 . 12_664 109.72(5) O1 S1 O1 . 6_566 109.72(5) O1 S1 O1 12_664 6_566 109.72(5) O1 S1 O2 . . 109.22(5) O1 S1 O2 12_664 . 109.22(5) O1 S1 O2 6_566 . 109.22(5) Cr1 O3 H3A . . 121.8(14) Cr1 O3 H3B . . 124.3(14) H3A O3 H3B . . 111.5(19) H4A O4 H4B . . 103(2) 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 N1 H1 O4 . 0.85(3) 2.16(3) 3.0049(11) 173(3) O3 H3A O1 20_575 0.80(2) 1.84(2) 2.6293(13) 172(2) O3 H3B O4 2_664 0.83(2) 1.78(2) 2.6071(13) 173(2) O4 H4B O2 4_566 0.79(3) 1.99(3) 2.7752(15) 171(2) O4 H4A O1 19_657 0.74(2) 2.02(2) 2.7454(14) 169(2)