#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/27/2012742.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_2012742 loop_ _publ_author_name 'Assaaoudi, Hassane' 'Ennaciri, Abdelaziz' 'Harcharras, Mohamed' 'El Bali, Brahim' 'Reinauer, Felix' 'Glaum, Robert' 'Rulmont, Andr\'e' 'Spirlet, Marie-Rose' _publ_section_title ; KZn(HP~2~O~7~)·2H~2~O and KMn(HP~2~O~7~)·2H~2~O: acid pyrophosphate metallates(II) with layer structures ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i79 _journal_page_last i81 _journal_paper_doi 10.1107/S0108270102007394 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac 'K Mn (H P2 O7) (H2 O)2' _chemical_formula_structural 'K Mn (H P2 O7) (H2 O)2' _chemical_formula_sum 'H5 K Mn O9 P2' _chemical_formula_weight 305.02 _chemical_name_systematic ; potassium manganese(II) hydrogenpyrophosphate dihydrate ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens difmap _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 15.7186(5) _cell_length_b 7.8706(5) _cell_length_c 6.5297(5) _cell_measurement_reflns_used 21 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 5.0 _cell_volume 807.82(8) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'ATOMS (Dowty, 1998)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD-4' _diffrn_measurement_method 'non-profiled \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 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 17404 _diffrn_reflns_theta_full 39.95 _diffrn_reflns_theta_max 39.95 _diffrn_reflns_theta_min 2.59 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.568 _exptl_absorpt_correction_T_max 0.6018 _exptl_absorpt_correction_T_min 0.5316 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details ; Number of psi-scan sets used was 9. Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied 'North & al. (1968)' ; _exptl_crystal_colour pink _exptl_crystal_density_diffrn 2.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 604 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.725 _refine_diff_density_min -0.463 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 2633 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0241 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.2440P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.0613 _reflns_number_gt 2278 _reflns_number_total 2633 _reflns_threshold_expression I>2\s(I) _cod_data_source_file br1366.cif _cod_data_source_block II _cod_database_code 2012742 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-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 K 0.96310(2) 0.2500 -0.11760(5) 0.02138(6) Uani d S 1 . . K Mn 0.694614(11) 0.2500 0.55922(3) 0.01119(4) Uani d S 1 . . Mn P 0.866688(13) 0.06286(3) 0.36102(3) 0.01013(5) Uani d . 1 . . P O1 0.88963(6) 0.2500 0.27658(14) 0.01411(15) Uani d S 1 . . O O2 0.92618(5) 0.03270(10) 0.54532(10) 0.01680(12) Uani d . 1 . . O H2 0.968(2) 0.008(6) 0.509(6) 0.032(9) Uiso d P 0.50 . . H O3 0.88784(5) -0.05244(9) 0.18429(11) 0.01651(12) Uani d . 1 . . O O4 0.77556(4) 0.06125(8) 0.42890(11) 0.01586(12) Uani d . 1 . . O O5W 0.89678(8) -0.2500 0.80036(17) 0.02169(19) Uani d S 1 . . O H5W 0.8989(13) -0.174(2) 0.721(3) 0.038(5) Uiso d . 1 . . H O6W 0.71626(7) -0.2500 0.33230(17) 0.01878(17) Uani d S 1 . . O H6W 0.7320(13) -0.167(2) 0.390(3) 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 K 0.01792(12) 0.02820(14) 0.01803(11) 0.000 0.00050(9) 0.000 Mn 0.00991(7) 0.01041(7) 0.01323(7) 0.000 0.00147(5) 0.000 P 0.00958(8) 0.00877(8) 0.01204(8) 0.00040(6) 0.00046(6) -0.00204(6) O1 0.0171(4) 0.0103(3) 0.0149(4) 0.000 0.0045(3) 0.000 O2 0.0159(3) 0.0210(3) 0.0135(2) 0.0030(2) -0.0022(2) 0.0016(2) O3 0.0142(2) 0.0155(3) 0.0198(3) 0.0003(2) 0.0011(2) -0.0091(2) O4 0.0114(2) 0.0127(2) 0.0234(3) -0.00065(19) 0.0044(2) -0.0040(2) O5W 0.0293(5) 0.0195(4) 0.0162(4) 0.000 0.0069(4) 0.000 O6W 0.0208(4) 0.0138(4) 0.0217(4) 0.000 0.0031(4) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 '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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 6 -2 -3 2 3 -3 -1 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 K O6W . 2_654 72.45(3) ? O1 K O3 . 3_755 118.47(2) ? O6W K O3 2_654 3_755 143.156(18) ? O1 K O3 . 5_755 118.47(2) ? O6W K O3 2_654 5_755 143.156(18) ? O3 K O3 3_755 5_755 66.25(3) ? O1 K O2 . 1_554 128.45(2) ? O6W K O2 2_654 1_554 73.05(2) ? O3 K O2 3_755 1_554 112.20(2) ? O3 K O2 5_755 1_554 73.82(2) ? O1 K O2 . 7_564 128.45(2) ? O6W K O2 2_654 7_564 73.05(2) ? O3 K O2 3_755 7_564 73.82(2) ? O3 K O2 5_755 7_564 112.20(2) ? O2 K O2 1_554 7_564 73.84(3) ? O1 K O5W . 5_756 70.92(3) ? O6W K O5W 2_654 5_756 143.38(3) ? O3 K O5W 3_755 5_756 60.33(2) ? O3 K O5W 5_755 5_756 60.33(2) ? O2 K O5W 1_554 5_756 132.70(2) ? O2 K O5W 7_564 5_756 132.70(2) ? O6W K O3 2_654 7_565 73.36(2) ? O3 K O3 3_755 7_565 89.57(2) ? O3 K O3 5_755 7_565 141.128(14) ? O2 K O3 1_554 7_565 145.06(2) ? O2 K O3 7_564 7_565 87.45(2) ? O5W K O3 5_756 7_565 81.51(2) ? O6W K O3 2_654 . 73.36(2) ? O3 K O3 3_755 . 141.128(14) ? O3 K O3 5_755 . 89.57(2) ? O2 K O3 1_554 . 87.45(2) ? O2 K O3 7_564 . 145.06(2) ? O5W K O3 5_756 . 81.51(2) ? O3 K O3 7_565 . 91.99(2) ? O1 K Mn . 6_656 108.18(2) ? O6W K Mn 2_654 6_656 179.36(3) ? O2 K Mn 1_554 6_656 106.455(17) ? O2 K Mn 7_564 6_656 106.455(17) ? O3 K Mn 7_565 6_656 107.066(14) ? O3 K Mn . 6_656 107.066(14) ? O6W K P 2_654 7_565 72.33(2) ? O3 K P 3_755 7_565 104.133(17) ? O3 K P 5_755 7_565 132.133(18) ? O2 K P 1_554 7_565 142.470(19) ? O2 K P 7_564 7_565 108.904(17) ? O5W K P 5_756 7_565 74.04(2) ? O3 K P 7_565 7_565 23.384(12) ? O3 K P . 7_565 69.133(13) ? Mn K P 6_656 7_565 108.252(9) ? O6W K P 2_654 . 72.33(2) ? O3 K P 3_755 . 132.133(18) ? O3 K P 5_755 . 104.133(17) ? O2 K P 1_554 . 108.904(17) ? O2 K P 7_564 . 142.470(19) ? O5W K P 5_756 . 74.04(2) ? O3 K P 7_565 . 69.133(13) ? Mn K P 6_656 . 108.252(9) ? O4 Mn O4 7_565 . 88.29(4) ? O4 Mn O3 7_565 2_655 178.31(3) ? O4 Mn O3 . 2_655 90.42(3) ? O4 Mn O3 7_565 8_766 90.42(3) ? O4 Mn O3 . 8_766 178.31(3) ? O3 Mn O3 2_655 8_766 90.86(4) ? O4 Mn O5W 7_565 2_654 94.72(3) ? O4 Mn O5W . 2_654 94.72(3) ? O3 Mn O5W 2_655 2_654 84.29(3) ? O3 Mn O5W 8_766 2_654 84.29(3) ? O4 Mn O6W 7_565 2_655 86.86(3) ? O4 Mn O6W . 2_655 86.86(3) ? O3 Mn O6W 2_655 2_655 94.16(3) ? O3 Mn O6W 8_766 2_655 94.16(3) ? O5W Mn O6W 2_654 2_655 177.79(4) ? O4 Mn K 7_565 6_556 129.404(19) ? O4 Mn K . 6_556 129.404(19) ? O3 Mn K 2_655 6_556 50.986(18) ? O3 Mn K 8_766 6_556 50.986(18) ? O5W Mn K 2_654 6_556 55.62(3) ? O6W Mn K 2_655 6_556 122.17(3) ? O4 P O3 . . 115.63(4) yes O4 P O2 . . 110.32(4) yes O3 P O2 . . 111.81(4) yes O4 P O1 . . 108.80(4) yes O3 P O1 . . 103.82(4) yes O2 P O1 . . 105.76(5) yes O4 P K . . 129.19(3) ? O3 P K . . 60.76(3) ? O2 P K . . 117.57(3) ? P O1 P 7_565 . 131.80(6) yes P O1 K 7_565 . 113.78(3) ? P O1 K . . 113.78(3) ? P O2 K . 1_556 129.37(4) ? P O3 Mn . 2_654 125.81(4) ? P O3 K . 5_755 128.95(4) ? Mn O3 K 2_654 5_755 92.43(2) ? P O3 K . . 95.86(3) ? Mn O3 K 2_654 . 120.12(3) ? K O3 K 5_755 . 90.43(2) ? P O4 Mn . . 132.99(4) ? Mn O5W K 2_655 5_756 87.12(4) ? Mn O6W K 2_654 2_655 134.77(5) ? Mn O6W H6W 2_654 . 100.5(15) ? 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 K O1 . 2.8211(10) ? K O6W 2_654 2.8382(12) ? K O3 3_755 2.8456(7) ? K O3 5_755 2.8456(7) ? K O2 1_554 2.8472(8) ? K O2 7_564 2.8472(8) ? K O5W 5_756 3.0236(13) ? K O3 7_565 3.3093(8) ? K O3 . 3.3093(8) ? K Mn 6_656 3.6590(4) ? K P 7_565 3.7727(4) ? K P . 3.7727(4) ? Mn O4 7_565 2.1330(7) ? Mn O4 . 2.1330(7) yes Mn O3 2_655 2.1828(7) yes Mn O3 8_766 2.1828(7) ? Mn O5W 2_654 2.2183(11) yes Mn O6W 2_655 2.2676(11) yes Mn K 6_556 3.6590(4) ? P O4 . 1.4995(7) yes P O3 . 1.5052(7) yes P O2 . 1.5424(7) yes P O1 . 1.6136(4) yes P H2 . 1.91(4) ? O1 P 7_565 1.6136(4) ? O2 K 1_556 2.8472(8) ? O2 H2 . 0.72(4) ? O3 Mn 2_654 2.1828(7) ? O3 K 5_755 2.8456(7) ? O5W Mn 2_655 2.2183(11) ? O5W K 5_756 3.0236(13) ? O6W Mn 2_654 2.2676(11) ? O6W K 2_655 2.8382(12) ?