#------------------------------------------------------------------------------ #$Date: 2014-03-11 16:03:39 +0000 (Tue, 11 Mar 2014) $ #$Revision: 104874 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239035.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2239035 loop_ _publ_author_name 'Souilem, Amira' 'Zid, Mohamed Faouzi' 'Driss, Ahmed' _publ_section_title ; \b-Li~0.37~Na~0.63~Fe(MoO~4~)~2~ ; _journal_coeditor_code VN2079 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i9 _journal_page_last i10 _journal_paper_doi 10.1107/S1600536814000646 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'Li0.37 Na0.63 Fe (Mo O4)2' _chemical_formula_moiety 'Fe Mo2 O8, 0.63(Na), 0.37(Li)' _chemical_formula_sum 'Fe Li0.37 Mo2 Na0.63 O8' _chemical_formula_weight 392.78 _chemical_name_systematic ; Lithium/sodium iron(III) bis[orthomolybdate(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_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 91.060(6) _cell_angle_beta 110.933(9) _cell_angle_gamma 105.661(9) _cell_formula_units_Z 2 _cell_length_a 6.8860(8) _cell_length_b 7.2560(9) _cell_length_c 7.3786(9) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 11 _cell_volume 328.84(7) _computing_cell_refinement 'CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'WinGX (Farrugia, 2012)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _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 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2838 _diffrn_reflns_theta_full 26.96 _diffrn_reflns_theta_max 26.96 _diffrn_reflns_theta_min 2.94 _diffrn_standards_decay_% 1.3 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 5.975 _exptl_absorpt_correction_T_max 0.4884 _exptl_absorpt_correction_T_min 0.2855 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 3.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 364 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _refine_diff_density_max 1.229 _refine_diff_density_min -0.582 _refine_ls_extinction_coef 0.0119(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 2008)' _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 1431 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.187 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0195 _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^)+(0.0210P)^2^+0.8764P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.0514 _reflns_number_gt 1380 _reflns_number_total 1431 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL zid17 in P -1 CELL 0.71073 6.8860 7.2560 7.3786 91.060 110.933 105.661 ZERR 2 0.0008 0.0009 0.0009 0.006 0.009 0.009 LATT 1 SFAC O Fe Mo Li Na UNIT 16 2 4 0.74 1.26 TEMP 25 SIZE 0.28 0.21 0.14 ACTA L.S. 10 BOND OMIT 0 8 2 OMIT 0 -1 1 FMAP 2 PLAN 20 REM EQIV $1 1-X,1-Y,-Z REM RTAB X..Y MO2 O5 REM SUMP 1.0 0.001 1. 2 1. 3 EXYZ NA1 LI1 EADP NA1 LI1 WGHT 0.021000 0.876400 EXTI 0.011891 FVAR 0.83916 0.63056 0.36944 MO1 3 0.183077 0.034175 0.283416 11.00000 0.00649 0.01197 = 0.01053 -0.00055 0.00226 0.00259 MO2 3 0.666246 0.424403 0.200099 11.00000 0.01547 0.00794 = 0.01610 -0.00076 -0.00234 0.00378 FE1 2 0.394525 0.095528 0.819986 11.00000 0.00899 0.00879 = 0.01067 0.00021 0.00243 0.00255 NA1 5 0.764807 0.449001 0.756660 21.00000 0.01961 0.01736 = 0.03379 0.00756 0.01378 0.00699 LI1 4 0.764807 0.449001 0.756660 -21.00000 0.01961 0.01736 = 0.03379 0.00756 0.01378 0.00699 O1 1 0.316287 0.875811 0.227777 11.00000 0.01075 0.01362 = 0.01921 0.00320 0.00785 0.00428 O2 1 0.894605 0.954986 0.154741 11.00000 0.00789 0.01966 = 0.01601 -0.00079 0.00457 0.00417 O3 1 0.528479 0.620010 0.147521 11.00000 0.01944 0.00908 = 0.01839 -0.00089 0.00145 0.00531 O4 1 0.753030 0.433401 0.447628 11.00000 0.02908 0.02466 = 0.01640 -0.00297 -0.00393 0.00963 O5 1 0.293672 0.266146 0.240092 11.00000 0.01905 0.01443 = 0.02532 -0.00022 0.00804 0.00215 O6 1 0.240317 0.042373 0.537343 11.00000 0.01575 0.03291 = 0.01123 -0.00084 0.00343 0.00739 O7 1 0.896339 0.514660 0.152118 11.00000 0.02384 0.02067 = 0.03341 0.00417 0.00686 0.00058 O8 1 0.582267 0.159659 0.111424 11.00000 0.01240 0.00968 = 0.01193 0.00143 0.00283 0.00341 HKLF 4 REM zid17 in P -1 REM R1 = 0.0195 for 1380 Fo > 4sig(Fo) and 0.0204 for all 1431 data REM 112 parameters refined using 0 restraints END WGHT 0.0215 0.8425 REM Highest difference peak 1.229, deepest hole -0.582, 1-sigma level 0.139 Q1 1 0.2104 0.0336 0.4151 11.00000 0.05 1.23 Q2 1 0.1816 0.0406 0.1766 11.00000 0.05 1.06 Q3 1 0.6769 0.4237 0.3118 11.00000 0.05 1.05 Q4 1 0.4046 0.0969 0.9436 11.00000 0.05 0.64 Q5 1 0.3863 0.1073 0.6962 11.00000 0.05 0.61 Q6 1 0.6465 0.4290 0.0768 11.00000 0.05 0.60 Q7 1 0.7657 0.4102 0.2260 11.00000 0.05 0.55 Q8 1 0.0554 0.0436 0.2392 11.00000 0.05 0.51 Q9 1 0.9048 0.5342 0.2411 11.00000 0.05 0.47 Q10 1 0.8075 0.9201 0.2389 11.00000 0.05 0.44 Q11 1 0.9776 0.5009 0.1509 11.00000 0.05 0.42 Q12 1 0.7983 1.0254 -0.0463 11.00000 0.05 0.42 Q13 1 0.3627 0.0622 0.5532 11.00000 0.05 0.41 Q14 1 0.7804 0.4750 0.0916 11.00000 0.05 0.39 Q15 1 0.8829 0.9485 0.0767 11.00000 0.05 0.39 Q16 1 1.0599 0.5303 0.2389 11.00000 0.05 0.38 Q17 1 0.3205 1.0010 0.2219 11.00000 0.05 0.37 Q18 1 0.2107 0.8992 0.1838 11.00000 0.05 0.35 Q19 1 0.8880 0.4368 0.1826 11.00000 0.05 0.34 Q20 1 0.3001 0.0247 0.3193 11.00000 0.05 0.34 ; _[local]_cod_data_source_file vn2079sup1.cf _[local]_cod_data_source_block I _cod_original_cell_volume 328.83(7) _cod_database_code 2239035 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Mo Mo1 0.18308(4) 0.03418(4) 0.28342(4) 0.00999(11) Uani d . 1 1 Mo Mo2 0.66625(5) 0.42440(4) 0.20010(5) 0.01552(11) Uani d . 1 1 Fe Fe1 0.39452(8) 0.09553(7) 0.81999(7) 0.00988(13) Uani d . 1 1 Na Na1 0.7648(4) 0.4490(3) 0.7567(4) 0.0221(8) Uani d P 0.631(9) 1 Li Li1 0.7648(4) 0.4490(3) 0.7567(4) 0.0221(8) Uani d P 0.369(9) 1 O O1 0.3163(4) 0.8758(3) 0.2278(4) 0.0137(5) Uani d . 1 1 O O2 0.8946(4) 0.9550(4) 0.1547(4) 0.0145(5) Uani d . 1 1 O O3 0.5285(4) 0.6200(3) 0.1475(4) 0.0171(5) Uani d . 1 1 O O4 0.7530(5) 0.4334(4) 0.4476(4) 0.0267(6) Uani d . 1 1 O O5 0.2937(4) 0.2661(4) 0.2401(4) 0.0203(6) Uani d . 1 1 O O6 0.2403(4) 0.0424(4) 0.5373(4) 0.0205(6) Uani d . 1 1 O O7 0.8963(5) 0.5147(4) 0.1521(5) 0.0284(7) Uani d . 1 1 O O8 0.5823(4) 0.1597(3) 0.1114(3) 0.0118(5) Uani 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 Mo1 0.00649(16) 0.01197(16) 0.01053(16) 0.00259(11) 0.00226(11) -0.00055(10) Mo2 0.01547(17) 0.00794(16) 0.01610(17) 0.00378(12) -0.00234(12) -0.00076(11) Fe1 0.0090(2) 0.0088(2) 0.0107(2) 0.00255(17) 0.00243(18) 0.00021(17) Na1 0.0196(12) 0.0174(12) 0.0338(14) 0.0070(9) 0.0138(10) 0.0076(9) Li1 0.0196(12) 0.0174(12) 0.0338(14) 0.0070(9) 0.0138(10) 0.0076(9) O1 0.0108(11) 0.0136(12) 0.0192(13) 0.0043(9) 0.0079(10) 0.0032(10) O2 0.0079(11) 0.0197(13) 0.0160(12) 0.0042(9) 0.0046(9) -0.0008(10) O3 0.0194(13) 0.0091(11) 0.0184(13) 0.0053(10) 0.0015(10) -0.0009(9) O4 0.0291(15) 0.0247(15) 0.0164(14) 0.0096(12) -0.0039(11) -0.0030(11) O5 0.0191(13) 0.0144(12) 0.0253(14) 0.0021(10) 0.0080(11) -0.0002(11) O6 0.0158(13) 0.0329(15) 0.0112(12) 0.0074(11) 0.0034(10) -0.0008(11) O7 0.0238(15) 0.0207(14) 0.0334(17) 0.0006(12) 0.0069(13) 0.0042(12) O8 0.0124(11) 0.0097(11) 0.0119(11) 0.0034(9) 0.0028(9) 0.0014(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 4 -2 -3 4 -2 -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 O5 Mo1 O6 . . 107.29(13) O5 Mo1 O1 . 1_545 110.16(12) O6 Mo1 O1 . 1_545 106.37(12) O5 Mo1 O2 . 1_445 110.72(12) O6 Mo1 O2 . 1_445 108.81(12) O1 Mo1 O2 1_545 1_445 113.22(11) O4 Mo2 O7 . . 105.39(15) O4 Mo2 O8 . . 103.81(12) O7 Mo2 O8 . . 103.08(13) O4 Mo2 O3 . . 103.37(13) O7 Mo2 O3 . . 103.71(13) O8 Mo2 O3 . . 134.72(11) O4 Mo2 O3 . 2_665 168.20(13) O7 Mo2 O3 . 2_665 86.38(13) O8 Mo2 O3 . 2_665 72.08(9) O3 Mo2 O3 . 2_665 73.94(11) O6 Fe1 O8 . 2_656 101.81(11) O6 Fe1 O3 . 2_666 99.65(12) O8 Fe1 O3 2_656 2_666 156.83(11) O6 Fe1 O2 . 2_666 88.11(11) O8 Fe1 O2 2_656 2_666 92.41(10) O3 Fe1 O2 2_666 2_666 96.92(11) O6 Fe1 O8 . 1_556 174.67(11) O8 Fe1 O8 2_656 1_556 78.88(11) O3 Fe1 O8 2_666 1_556 78.95(10) O2 Fe1 O8 2_666 1_556 97.16(10) O6 Fe1 O1 . 2_666 87.72(11) O8 Fe1 O1 2_656 2_666 84.61(10) O3 Fe1 O1 2_666 2_666 87.65(10) O2 Fe1 O1 2_666 2_666 174.27(10) O8 Fe1 O1 1_556 2_666 87.08(10) 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 Mo1 O5 . 1.737(3) y Mo1 O6 . 1.768(3) y Mo1 O1 1_545 1.775(2) y Mo1 O2 1_445 1.787(2) y Mo2 O4 . 1.701(3) y Mo2 O7 . 1.707(3) y Mo2 O8 . 1.880(2) y Mo2 O3 . 1.884(2) y Mo2 O3 2_665 2.400(3) y Mo2 O5 . 2.636(3) y Fe1 O6 . 1.947(3) y Fe1 O8 2_656 1.961(2) y Fe1 O3 2_666 1.975(2) y Fe1 O2 2_666 2.002(2) y Fe1 O8 1_556 2.041(2) y Fe1 O1 2_666 2.101(2) y Na1 O7 2_766 2.123(4) y Na1 O5 2_666 2.211(3) y Na1 O4 . 2.252(4) y Na1 O1 2_666 2.286(3) y Na1 O3 2_666 2.306(3) y Na1 O7 1_556 2.718(4) y _cod_database_fobs_code 2239035