#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/38/2013841.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_2013841 loop_ _publ_author_name 'Kolitsch, Uwe' _publ_section_title ; (NH~4~)~4~Cd(HSe^IV^O~3~)~2~(Se^VI^O~4~)~2~: a new structure type with kr\"ohnkite-like chains ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i3 _journal_page_last i6 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '(N H4)4 Cd (H Se O3)2 (Se O4)2' _chemical_formula_moiety '4N H4 + , Cd 2+ , 2H Se O3 - , 2Se O4 2-' _chemical_formula_structural '(N H4)4 Cd (H Se O3)2 (Se O4)2' _chemical_formula_sum 'Cd H18 N4 O14 Se4' _chemical_formula_weight 726.42 _chemical_name_common 'ammonium cadmium selenite selenate' _chemical_name_systematic ; tetraammonium cadmium dihydrogenselenite(IV) diselenate(VI) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.05(3) _cell_angle_beta 105.02(3) _cell_angle_gamma 112.61(3) _cell_formula_units_Z 1 _cell_length_a 5.7910(10) _cell_length_b 7.4110(10) _cell_length_c 10.736(2) _cell_measurement_reflns_used 2196 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.03 _cell_measurement_theta_min 2.04 _cell_volume 408.20(17) _computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor 1997)' _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_data_reduction 'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK' _computing_molecular_graphics 'ATOMS (Dowty, 1999) and ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\y and \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 0.027 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4514 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 3.00 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 10.330 _exptl_absorpt_correction_T_max 0.747 _exptl_absorpt_correction_T_min 0.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'HKL SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.955 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 342 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.85 _refine_diff_density_min -1.22 _refine_ls_extinction_coef 0.0173(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 143 _refine_ls_number_reflns 2368 _refine_ls_number_restraints 9 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.058P)^2^+0.1P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.096 _refine_ls_wR_factor_ref 0.101 _reflns_number_gt 2003 _reflns_number_total 2368 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1663.cif _[local]_cod_data_source_block I _cod_database_code 2013841 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cd 0.0000 1.0000 1.0000 0.01992(15) Uani d S 1 . . Cd Se1 -0.30508(8) 0.66588(6) 0.70424(4) 0.01855(15) Uani d . 1 . . Se Se2 -0.44491(9) 0.95670(6) 1.17649(4) 0.01930(15) Uani d . 1 . . Se N1 0.2256(10) 0.5281(7) 0.8977(5) 0.0313(10) Uani d D 1 . . N N2 -0.1594(10) 0.2294(7) 0.5369(5) 0.0328(10) Uani d D 1 . . N O1 -0.3238(8) 0.8566(6) 0.6377(4) 0.0402(9) Uani d . 1 . . O O2 -0.5896(7) 0.4829(6) 0.6614(4) 0.0352(8) Uani d . 1 . . O O3 -0.0842(7) 0.6066(6) 0.6666(4) 0.0362(9) Uani d . 1 . . O O4 -0.2218(7) 0.7089(5) 0.8639(3) 0.0306(8) Uani d . 1 . . O O5 -0.7602(7) 0.8285(5) 1.1036(4) 0.0329(8) Uani d . 1 . . O O6 -0.3077(7) 0.8426(5) 1.1027(4) 0.0347(8) Uani d . 1 . . O O7 -0.3990(8) 0.8726(6) 1.3280(3) 0.0352(9) Uani d D 1 . . O H1 0.161(16) 0.558(13) 0.822(6) 0.08(3) Uiso d D 1 . . H H2 0.294(15) 0.635(9) 0.950(7) 0.07(2) Uiso d D 1 . . H H3 0.356(10) 0.519(10) 0.897(7) 0.04(2) Uiso d D 1 . . H H4 0.121(12) 0.424(8) 0.914(8) 0.06(2) Uiso d D 1 . . H H5 -0.125(17) 0.146(11) 0.593(7) 0.08(3) Uiso d D 1 . . H H6 -0.100(11) 0.346(7) 0.578(5) 0.031(16) Uiso d D 1 . . H H7 -0.022(10) 0.259(9) 0.511(6) 0.033(16) Uiso d D 1 . . H H8 -0.311(9) 0.210(9) 0.478(5) 0.034(16) Uiso d D 1 . . H H9 -0.418(17) 0.750(8) 1.339(8) 0.07(3) 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 Cd 0.0193(2) 0.0198(2) 0.0218(3) 0.00794(18) 0.00735(18) 0.00340(18) Se1 0.0202(2) 0.0174(2) 0.0174(2) 0.00719(17) 0.00472(17) 0.00213(17) Se2 0.0208(2) 0.0166(2) 0.0192(2) 0.00605(17) 0.00579(17) 0.00228(17) N1 0.030(3) 0.031(3) 0.033(2) 0.012(2) 0.008(2) 0.005(2) N2 0.034(3) 0.027(2) 0.030(2) 0.005(2) 0.008(2) 0.000(2) O1 0.045(2) 0.030(2) 0.043(2) 0.0144(18) 0.0067(18) 0.0139(18) O2 0.0241(18) 0.035(2) 0.041(2) 0.0084(15) 0.0049(16) 0.0041(17) O3 0.031(2) 0.048(2) 0.041(2) 0.0230(18) 0.0171(17) 0.0053(19) O4 0.041(2) 0.0282(18) 0.0184(15) 0.0094(16) 0.0090(15) -0.0003(14) O5 0.0245(18) 0.0223(17) 0.044(2) 0.0076(14) -0.0003(16) 0.0034(16) O6 0.043(2) 0.0269(18) 0.044(2) 0.0132(17) 0.0309(18) 0.0051(17) O7 0.056(3) 0.034(2) 0.0196(17) 0.0248(19) 0.0059(17) 0.0083(16) 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 Cd O6 . 2.275(3) yes Cd O6 2_577 2.275(3) ? Cd O4 . 2.309(4) yes Cd O4 2_577 2.309(4) ? Cd O5 2_477 2.311(3) ? Cd O5 1_655 2.311(3) yes Se1 O1 . 1.612(4) yes Se1 O2 . 1.629(4) yes Se1 O3 . 1.641(3) yes Se1 O4 . 1.651(3) yes Se2 O5 . 1.665(4) yes Se2 O6 . 1.678(3) yes Se2 O7 . 1.735(3) yes N1 H1 . 0.87(5) ? N1 H2 . 0.86(5) ? N1 H3 . 0.78(4) ? N1 H4 . 0.83(5) ? N2 H5 . 0.90(5) ? N2 H6 . 0.87(4) ? N2 H7 . 0.86(4) ? N2 H8 . 0.90(4) ? O7 H9 . 0.88(5) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' 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 O6 Cd O6 . 2_577 180 ? O6 Cd O4 . 2_577 99.14(13) ? O6 Cd O4 . . 80.86(13) ? O4 Cd O4 2_577 . 180 ? O6 Cd O5 . 2_477 91.15(14) ? O4 Cd O5 . 2_477 98.13(13) ? O6 Cd O5 . 1_655 88.85(14) ? O4 Cd O5 . 1_655 81.87(13) ? O5 Cd O5 2_477 1_655 180 ? O1 Se1 O2 . . 109.8(2) yes O1 Se1 O3 . . 111.2(2) yes O2 Se1 O3 . . 111.0(2) yes O1 Se1 O4 . . 110.7(2) yes O2 Se1 O4 . . 106.62(19) yes O3 Se1 O4 . . 107.38(19) yes O5 Se2 O6 . . 101.24(19) yes O5 Se2 O7 . . 103.65(19) yes O6 Se2 O7 . . 100.96(19) yes H1 N1 H2 . . 106(8) ? H1 N1 H3 . . 108(8) ? H2 N1 H3 . . 97(7) ? H1 N1 H4 . . 111(8) ? H2 N1 H4 . . 122(8) ? H3 N1 H4 . . 111(8) ? H5 N2 H6 . . 109(7) ? H5 N2 H7 . . 96(7) ? H6 N2 H7 . . 92(5) ? H5 N2 H8 . . 128(7) ? H6 N2 H8 . . 108(6) ? H7 N2 H8 . . 118(6) ? Se2 O7 H9 . . 123(6) ? 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 _geom_hbond_publ_flag N1 H1 O3 . 0.87(5) 2.03(5) 2.866(6) 163(8) yes N1 H2 O5 1_655 0.86(5) 2.34(6) 3.099(6) 147(7) yes N1 H2 O6 1_655 0.86(5) 2.38(6) 3.105(7) 142(7) yes N1 H3 O4 1_655 0.78(4) 2.43(5) 3.078(6) 141(6) yes N1 H4 O5 2_467 0.83(5) 2.17(5) 2.958(6) 160(7) yes N2 H5 O1 1_545 0.90(5) 2.13(7) 2.868(6) 138(8) yes N2 H6 O3 . 0.87(4) 2.11(4) 2.947(7) 161(5) yes N2 H7 O3 2_566 0.86(4) 2.26(5) 2.919(6) 133(5) yes N2 H8 O1 2_466 0.90(4) 2.02(4) 2.915(7) 172(5) yes O7 H9 O2 2_467 0.88(5) 1.75(5) 2.614(5) 167(8) yes _cod_database_fobs_code 2013841