#------------------------------------------------------------------------------ #$Date: 2012-02-08 22:24:44 +0200 (Wed, 08 Feb 2012) $ #$Revision: 32193 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/23/31/2233136.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_2233136 loop_ _publ_author_name 'Liu, Biao' 'Zhang, Xin' 'Wen, Lei' 'Sun, Wei' 'Huang, Ya-Xi' _publ_section_title ; An ammonium iron(II) pyrophosphate, (NH~4~)~2~[Fe~3~(P~2~O~7~)~2~(H~2~O)~2~], with a layered structure ; _journal_coeditor_code FI2119 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i5 _journal_page_last i6 _journal_volume 68 _journal_year 2012 _chemical_formula_iupac '(N H4)2 [Fe3 (H2 O)2 (P2 O7)2]' _chemical_formula_moiety '2(H4 N +), Fe3 H4 O16 P4 2-' _chemical_formula_sum 'Fe3 H12 N2 O16 P4' _chemical_formula_weight 587.55 _chemical_name_systematic ; Diammonium diaquabis(phosphato)triferrate(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 99.651(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.4131(17) _cell_length_b 8.1940(15) _cell_length_c 9.3987(17) _cell_measurement_reflns_used 4127 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.26 _cell_measurement_theta_min 2.20 _cell_volume 714.7(2) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2005) and ATOMS (Dowty, 2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 1.0 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device_type 'Bruker Smart APEXI diffractometer equipped with CCD area-detector' _diffrn_measurement_method '1265 images,\f=0, 90, 180\%, and \D\w=0.3\%, \c= 54.74\%' _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 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4127 _diffrn_reflns_theta_full 28.26 _diffrn_reflns_theta_max 28.26 _diffrn_reflns_theta_min 2.19 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(SMART; Bruker, 2001)' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 2.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.551 _refine_diff_density_min -0.548 _refine_ls_extinction_coef 0 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 135 _refine_ls_number_reflns 1652 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0399 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.7041P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0850 _reflns_number_gt 1417 _reflns_number_total 1652 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL P21/c CELL 0.71073 9.4131 8.19400 9.3987 90.000 99.651 90.000 ZERR 2 0.0017 0.0015 0.0017 0.000 0.003 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC Fe H N O P UNIT 6 24 4 32 8 L.S. 8 TEMP -100 FMAP 2 PLAN 20 ACTA BOND $H EQIV $1 x, y+1, z EQIV $2 -x+1, y+1/2, -z+1/2 EQIV $3 -x+1, y-1/2, -z+1/2 EQIV $4 x, -y+1/2, z+1/2 EQIV $5 x, y-1, z EQIV $6 -x+1, -y+1, -z+1 HTAB O8 O3_$1 HTAB O8 O7_$2 HTAB N1 O1_$3 HTAB N1 O2_$4 HTAB N1 O8_$5 HTAB N1 O7_$6 HTAB N1 O7 WGHT 0.033100 1.704100 FVAR 0.61286 0.03291 0.05016 FE1 1 0.868466 0.860145 0.501615 11.00000 0.00906 0.00869 = 0.00783 0.00060 0.00123 0.00074 FE2 1 1.000000 0.500000 0.500000 10.50000 0.00949 0.00792 = 0.00736 -0.00010 0.00079 0.00026 P1 5 0.905784 0.298654 0.209255 11.00000 0.00819 0.00816 = 0.00653 -0.00011 0.00096 0.00008 P2 5 0.704375 0.555318 0.263438 11.00000 0.00838 0.00946 = 0.00749 0.00027 0.00047 0.00104 O1 4 0.706010 0.645558 0.122866 11.00000 0.01449 0.01317 = 0.01090 0.00066 0.00445 0.00289 O2 4 0.750857 0.367880 0.234978 11.00000 0.00849 0.00951 = 0.00994 -0.00222 0.00226 -0.00146 O3 4 0.873968 0.133067 0.139817 11.00000 0.01572 0.00857 = 0.00703 -0.00100 0.00152 0.00020 O4 4 0.997096 0.295119 0.359196 11.00000 0.01164 0.01178 = 0.00685 -0.00026 0.00033 0.00194 O5 4 0.813233 0.619190 0.388658 11.00000 0.01121 0.00848 = 0.00844 -0.00224 -0.00320 0.00178 O6 4 0.962492 0.419903 0.110391 11.00000 0.01407 0.00570 = 0.01079 0.00025 0.00485 0.00111 O7 4 0.553799 0.538514 0.297164 11.00000 0.00874 0.01704 = 0.01236 -0.00061 0.00261 0.00101 O8 4 0.730130 0.990552 0.337075 11.00000 0.01117 0.02407 = 0.01397 0.00916 -0.00159 -0.00173 H1 2 0.776929 1.015945 0.264772 11.00000 21.00000 H2 2 0.646612 0.978504 0.296413 11.00000 21.00000 N1 3 0.554781 0.276111 0.486713 11.00000 0.01741 0.02075 = 0.02053 0.00119 -0.00297 -0.00587 H3 2 0.479874 0.206469 0.460801 11.00000 31.00000 H4 2 0.631869 0.213328 0.485299 11.00000 31.00000 H5 2 0.549576 0.323164 0.579168 11.00000 31.00000 H6 2 0.550160 0.362604 0.430238 11.00000 31.00000 HKLF 4 1 REM test in P 21/a New: P21/c REM R1 = 0.0399 for 1417 Fo > 4sig(Fo) and 0.0485 for all 1652 data REM 135 parameters refined using 0 restraints END WGHT 0.0331 1.7041 REM Highest difference peak 0.551, deepest hole -0.548, 1-sigma level 0.145 Q1 1 0.7874 0.7990 0.4900 11.00000 0.05 0.55 Q2 1 0.5632 0.4942 0.3558 11.00000 0.05 0.53 Q3 1 0.9219 0.9360 0.4616 11.00000 0.05 0.52 Q4 1 0.8965 0.8515 0.4061 11.00000 0.05 0.52 Q5 1 0.6872 0.9511 0.4138 11.00000 0.05 0.50 Q6 1 0.4859 0.5715 0.2661 11.00000 0.05 0.48 Q7 1 0.9416 0.3685 0.1594 11.00000 0.05 0.48 Q8 1 0.7857 0.5863 0.3081 11.00000 0.05 0.46 Q9 1 0.4931 0.5529 0.2373 11.00000 0.05 0.46 Q10 1 0.9777 0.2318 0.2993 11.00000 0.05 0.44 Q11 1 0.4301 0.3536 0.4413 11.00000 0.05 0.43 Q12 1 0.9983 0.0453 0.2110 11.00000 0.05 0.43 Q13 1 0.5196 0.5990 0.3747 11.00000 0.05 0.43 Q14 1 0.6580 0.2993 0.2153 11.00000 0.05 0.43 Q15 1 0.8126 0.5888 0.4786 11.00000 0.05 0.42 Q16 1 0.6137 0.5196 0.2594 11.00000 0.05 0.42 Q17 1 0.8801 0.1014 0.0732 11.00000 0.05 0.42 Q18 1 0.7478 0.6321 0.1945 11.00000 0.05 0.42 Q19 1 0.9184 0.5681 0.4791 11.00000 0.05 0.42 Q20 1 0.7546 0.7102 0.4627 11.00000 0.05 0.41 ; _[local]_cod_data_source_file fi2119.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2233136 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _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_symmetry_multiplicity Fe Fe1 0.86847(6) 0.86015(7) 0.50162(6) 0.00855(16) Uani d . 1 1 Fe Fe2 1.0000 0.5000 0.5000 0.00833(19) Uani d S 1 2 P P1 0.90578(11) 0.29865(13) 0.20925(10) 0.0077(2) Uani d . 1 1 P P2 0.70438(11) 0.55532(13) 0.26344(11) 0.0085(2) Uani d . 1 1 O O1 0.7060(3) 0.6456(4) 0.1229(3) 0.0126(6) Uani d . 1 1 O O2 0.7509(3) 0.3679(3) 0.2350(3) 0.0092(6) Uani d . 1 1 O O3 0.8740(3) 0.1331(3) 0.1398(3) 0.0105(6) Uani d . 1 1 O O4 0.9971(3) 0.2951(3) 0.3592(3) 0.0102(6) Uani d . 1 1 O O5 0.8132(3) 0.6192(3) 0.3887(3) 0.0099(6) Uani d . 1 1 O O6 0.9625(3) 0.4199(3) 0.1104(3) 0.0099(6) Uani d . 1 1 O O7 0.5538(3) 0.5385(4) 0.2972(3) 0.0126(6) Uani d . 1 1 O O8 0.7301(3) 0.9906(4) 0.3371(3) 0.0168(7) Uani d . 1 1 H H1 0.777(6) 1.016(7) 0.265(6) 0.033(11) Uiso d . 1 1 H H2 0.647(6) 0.979(7) 0.296(6) 0.033(11) Uiso d . 1 1 N N1 0.5548(5) 0.2761(5) 0.4867(5) 0.0203(9) Uani d . 1 1 H H3 0.480(7) 0.206(8) 0.461(7) 0.050(10) Uiso d . 1 1 H H4 0.632(7) 0.213(8) 0.485(7) 0.050(10) Uiso d . 1 1 H H5 0.550(7) 0.323(8) 0.579(7) 0.050(10) Uiso d . 1 1 H H6 0.550(7) 0.363(8) 0.430(7) 0.050(10) Uiso d . 1 1 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 Fe1 0.0091(3) 0.0087(3) 0.0078(3) 0.0007(2) 0.0012(2) 0.0006(2) Fe2 0.0095(4) 0.0079(4) 0.0074(4) 0.0003(3) 0.0008(3) -0.0001(3) P1 0.0082(5) 0.0082(5) 0.0065(5) 0.0001(4) 0.0010(4) -0.0001(4) P2 0.0084(5) 0.0095(5) 0.0075(5) 0.0010(4) 0.0005(4) 0.0003(4) O1 0.0145(14) 0.0132(15) 0.0109(14) 0.0029(12) 0.0045(11) 0.0007(12) O2 0.0085(13) 0.0095(14) 0.0099(13) -0.0015(11) 0.0023(11) -0.0022(11) O3 0.0157(14) 0.0086(14) 0.0070(13) 0.0002(12) 0.0015(11) -0.0010(11) O4 0.0116(14) 0.0118(15) 0.0069(13) 0.0019(12) 0.0003(11) -0.0003(11) O5 0.0112(14) 0.0085(14) 0.0084(13) 0.0018(11) -0.0032(11) -0.0022(11) O6 0.0141(14) 0.0057(14) 0.0108(14) 0.0011(11) 0.0048(11) 0.0003(11) O7 0.0087(13) 0.0170(16) 0.0124(14) 0.0010(12) 0.0026(11) -0.0006(12) O8 0.0112(15) 0.0241(19) 0.0140(15) -0.0017(14) -0.0016(12) 0.0092(13) N1 0.017(2) 0.021(2) 0.021(2) -0.0059(17) -0.0030(17) 0.0012(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 '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' P P 0.1023 0.0942 '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 O1 Fe1 O4 4_576 3_766 93.89(11) no O1 Fe1 O6 4_576 2_755 167.57(12) no O4 Fe1 O6 3_766 2_755 91.46(11) no O1 Fe1 O8 4_576 . 89.59(12) no O4 Fe1 O8 3_766 . 171.64(12) no O6 Fe1 O8 2_755 . 86.66(12) no O1 Fe1 O6 4_576 4_576 92.29(11) no O4 Fe1 O6 3_766 4_576 93.09(11) no O6 Fe1 O6 2_755 4_576 76.20(11) no O8 Fe1 O6 . 4_576 94.37(12) no O1 Fe1 O5 4_576 . 96.12(11) no O4 Fe1 O5 3_766 . 80.21(10) no O6 Fe1 O5 2_755 . 95.84(10) no O8 Fe1 O5 . . 91.87(12) no O6 Fe1 O5 4_576 . 169.56(10) no O5 Fe2 O5 . 3_766 180.0 no O5 Fe2 O4 . . 97.61(10) no O5 Fe2 O4 3_766 . 82.39(10) no O5 Fe2 O4 . 3_766 82.39(10) no O5 Fe2 O4 3_766 3_766 97.61(10) no O4 Fe2 O4 . 3_766 180.0 no O5 Fe2 O3 . 4_566 92.14(11) no O5 Fe2 O3 3_766 4_566 87.86(10) no O4 Fe2 O3 . 4_566 91.63(10) no O4 Fe2 O3 3_766 4_566 88.37(10) no O5 Fe2 O3 . 2_755 87.86(10) no O5 Fe2 O3 3_766 2_755 92.14(11) no O4 Fe2 O3 . 2_755 88.37(10) no O4 Fe2 O3 3_766 2_755 91.63(10) no O3 Fe2 O3 4_566 2_755 180.0 no O3 P1 O6 . . 112.80(16) no O3 P1 O4 . . 114.97(16) no O6 P1 O4 . . 112.16(16) no O3 P1 O2 . . 105.08(15) no O6 P1 O2 . . 106.26(16) no O4 P1 O2 . . 104.54(15) no O7 P2 O1 . . 111.99(16) no O7 P2 O5 . . 113.84(16) no O1 P2 O5 . . 113.78(17) no O7 P2 O2 . . 103.63(16) no O1 P2 O2 . . 105.91(15) no O5 P2 O2 . . 106.68(15) no P2 O1 Fe1 . 4_575 126.10(17) no P1 O2 P2 . . 128.83(18) yes P1 O3 Fe2 . 2_745 127.87(17) no P1 O4 Fe1 . 3_766 141.13(18) no P1 O4 Fe2 . . 120.34(16) no Fe1 O4 Fe2 3_766 . 98.46(11) yes P2 O5 Fe2 . . 128.17(16) no P2 O5 Fe1 . . 137.51(16) no Fe2 O5 Fe1 . . 93.67(10) yes P1 O6 Fe1 . 2_745 121.76(16) no P1 O6 Fe1 . 4_575 132.09(16) no Fe1 O6 Fe1 2_745 4_575 103.80(11) no Fe1 O8 H1 . . 110(4) no Fe1 O8 H2 . . 134(4) no H1 O8 H2 . . 103(5) no H3 N1 H4 . . 103(5) no H3 N1 H5 . . 110(5) no H4 N1 H5 . . 114(5) no H3 N1 H6 . . 113(5) no H4 N1 H6 . . 114(6) no H5 N1 H6 . . 103(5) no 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 Fe1 O1 4_576 2.055(3) yes Fe1 O4 3_766 2.092(3) yes Fe1 O6 2_755 2.108(3) yes Fe1 O8 . 2.134(3) yes Fe1 O6 4_576 2.185(3) yes Fe1 O5 . 2.261(3) yes Fe2 O5 . 2.127(3) yes Fe2 O5 3_766 2.127(3) yes Fe2 O4 . 2.135(3) yes Fe2 O4 3_766 2.135(3) yes Fe2 O3 4_566 2.201(3) yes Fe2 O3 2_755 2.201(3) yes P1 O3 . 1.514(3) yes P1 O6 . 1.517(3) yes P1 O4 . 1.523(3) yes P1 O2 . 1.620(3) yes P2 O7 . 1.510(3) yes P2 O1 . 1.516(3) yes P2 O5 . 1.518(3) yes P2 O2 . 1.631(3) yes O8 H1 . 0.89(6) yes O8 H2 . 0.82(6) yes N1 H3 . 0.91(7) yes N1 H4 . 0.89(6) yes N1 H5 . 0.96(7) yes N1 H6 . 0.88(7) yes 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 O8 H1 O3 1_565 0.89(6) 1.87(6) 2.734(4) 162(5) y O8 H2 O7 2_655 0.82(6) 2.00(6) 2.785(4) 159(5) y N1 H3 O1 2_645 0.91(7) 1.86(7) 2.717(5) 156(6) y N1 H4 O2 4_566 0.89(6) 2.51(6) 2.966(5) 112(5) no N1 H4 O8 1_545 0.89(6) 2.56(7) 3.310(6) 142(5) y N1 H5 O7 3_666 0.96(7) 1.99(7) 2.859(5) 150(5) y N1 H6 O7 . 0.88(7) 1.91(7) 2.791(5) 174(6) y