# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? loop_ _publ_author_name _publ_author_address 'A. Shahul Hameed' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; 'Mangayarkarasi Nagarathinam' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; 'M.V. Reddy' ; Department of Physics, National University of Singapore Singapore 117542 ; 'B.V.R. Chowdari' ; Department of Physics National University of Singapore Singapore 117542 ; 'Jagadese J. Vittal' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; #TrackingRef '- ShahulEES.cif' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Jagadese J. Vittal Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; _publ_contact_author_email chmjjv@nus.edu.sg _publ_contact_author_fax '(65) 6779 1691' _publ_contact_author_phone '(65) 6516 2677' _publ_contact_letter ; '' ; _publ_requested_coeditor_name ' ' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and electrochemical studies of layer-structured tetragonal aI-LiVOPO4 ; data_ShahulEES _database_code_depnum_ccdc_archive 'CCDC 855311' _iucr_compatibility_tag ACTA95 #============================================================================== # Compounds 1 and 3 have been previously reported _data_compound LiVOPO4.2H2O # data_b252 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H4 Li O7 P V' _chemical_formula_weight 204.88 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' H H 0.0000 0.0000 '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' V V 0.3005 0.5294 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 8.9454(7) _cell_length_b 9.0406(7) _cell_length_c 12.7473(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1030.90(14) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2489 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 27.44 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 2.206 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4724 _exptl_absorpt_correction_T_max 0.7192 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3374 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 633 _reflns_number_gt 625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+2.7579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 633 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.5000 0.62335(4) 0.79062(3) 0.00458(17) Uani 1 2 d S . . Li1 Li 0.5000 0.8776(5) 0.9344(4) 0.0178(10) Uani 1 2 d S . . P1 P 0.2500 0.87610(6) 0.7500 0.00421(19) Uani 1 2 d S . . O1 O 0.65668(13) 0.47274(13) 0.82570(10) 0.0080(3) Uani 1 1 d . . . O2 O 0.5000 0.6125(2) 0.66636(16) 0.0120(4) Uani 1 2 d S . . O3 O 0.35070(13) 0.78219(13) 0.82088(10) 0.0077(3) Uani 1 1 d . . . O1W O 0.3359(2) 1.0000 1.0000 0.0130(4) Uani 1 2 d S . . H1 H 0.279(3) 0.986(3) 1.050(2) 0.031(7) Uiso 1 1 d . . . O2W O 0.5000 0.6676(2) 0.98991(16) 0.0135(4) Uani 1 2 d S . . H2 H 0.436(4) 0.654(4) 1.029(3) 0.052(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0032(2) 0.0040(3) 0.0066(3) -0.00024(13) 0.000 0.000 Li1 0.020(2) 0.014(2) 0.019(3) -0.0051(18) 0.000 0.000 P1 0.0025(3) 0.0034(3) 0.0067(4) 0.000 0.0000(2) 0.000 O1 0.0064(5) 0.0077(6) 0.0100(6) -0.0017(5) 0.0000(5) 0.0036(5) O2 0.0115(9) 0.0146(9) 0.0100(10) -0.0012(7) 0.000 0.000 O3 0.0068(5) 0.0071(5) 0.0093(6) 0.0000(4) -0.0015(5) 0.0032(4) O1W 0.0107(9) 0.0205(10) 0.0077(8) -0.0011(7) 0.000 0.000 O2W 0.0153(10) 0.0139(9) 0.0112(9) 0.0020(8) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O2 1.587(2) . ? V1 O3 1.9987(12) 12_655 ? V1 O3 1.9987(12) . ? V1 O1 2.0045(12) 12_655 ? V1 O1 2.0045(12) . ? V1 Li1 2.940(5) . ? Li1 O1W 2.020(4) 9_677 ? Li1 O1W 2.020(4) . ? Li1 O2W 2.026(5) . ? Li1 O3 2.150(4) . ? Li1 O3 2.150(4) 12_655 ? Li1 O2 2.482(5) 10_567 ? Li1 Li1 2.774(10) 9_677 ? P1 O3 1.5325(12) 7_546 ? P1 O3 1.5325(12) . ? P1 O1 1.5464(12) 5_455 ? P1 O1 1.5464(12) 3_656 ? O1 P1 1.5464(12) 5_545 ? O2 Li1 2.482(5) 10_557 ? O1W Li1 2.020(4) 9_677 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 V1 O3 103.70(6) . 12_655 ? O2 V1 O3 103.70(6) . . ? O3 V1 O3 83.86(7) 12_655 . ? O2 V1 O1 100.42(6) . 12_655 ? O3 V1 O1 155.81(6) 12_655 12_655 ? O3 V1 O1 88.73(5) . 12_655 ? O2 V1 O1 100.42(6) . . ? O3 V1 O1 88.73(5) 12_655 . ? O3 V1 O1 155.81(6) . . ? O1 V1 O1 88.72(7) 12_655 . ? O2 V1 Li1 132.09(13) . . ? O3 V1 Li1 46.99(6) 12_655 . ? O3 V1 Li1 46.99(6) . . ? O1 V1 Li1 113.09(8) 12_655 . ? O1 V1 Li1 113.09(8) . . ? O1W Li1 O1W 93.3(2) 9_677 . ? O1W Li1 O2W 111.6(2) 9_677 . ? O1W Li1 O2W 111.6(2) . . ? O1W Li1 O3 161.8(3) 9_677 . ? O1W Li1 O3 92.69(7) . . ? O2W Li1 O3 81.90(16) . . ? O1W Li1 O3 92.69(7) 9_677 12_655 ? O1W Li1 O3 161.8(3) . 12_655 ? O2W Li1 O3 81.90(16) . 12_655 ? O3 Li1 O3 76.82(18) . 12_655 ? O1W Li1 O2 75.26(14) 9_677 10_567 ? O1W Li1 O2 75.26(14) . 10_567 ? O2W Li1 O2 169.3(3) . 10_567 ? O3 Li1 O2 89.73(19) . 10_567 ? O3 Li1 O2 89.73(19) 12_655 10_567 ? O1W Li1 Li1 46.63(10) 9_677 9_677 ? O1W Li1 Li1 46.63(11) . 9_677 ? O2W Li1 Li1 122.5(4) . 9_677 ? O3 Li1 Li1 136.56(16) . 9_677 ? O3 Li1 Li1 136.56(16) 12_655 9_677 ? O2 Li1 Li1 68.25(19) 10_567 9_677 ? O1W Li1 V1 133.35(11) 9_677 . ? O1W Li1 V1 133.35(11) . . ? O2W Li1 V1 59.01(13) . . ? O3 Li1 V1 42.83(9) . . ? O3 Li1 V1 42.83(9) 12_655 . ? O2 Li1 V1 110.3(2) 10_567 . ? Li1 Li1 V1 178.5(3) 9_677 . ? O3 P1 O3 112.72(10) 7_546 . ? O3 P1 O1 111.32(7) 7_546 5_455 ? O3 P1 O1 105.21(7) . 5_455 ? O3 P1 O1 105.21(7) 7_546 3_656 ? O3 P1 O1 111.32(7) . 3_656 ? O1 P1 O1 111.20(10) 5_455 3_656 ? P1 O1 V1 128.46(8) 5_545 . ? V1 O2 Li1 124.68(16) . 10_557 ? P1 O3 V1 132.61(8) . . ? P1 O3 Li1 122.66(14) . . ? V1 O3 Li1 90.18(10) . . ? Li1 O1W Li1 86.7(2) 9_677 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2 O1 0.76(4) 2.34(4) 3.017(2) 149(3) 9_667 O1W H1 O1 0.82(3) 1.96(3) 2.7508(17) 160(3) 8_467 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.261 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.132 #===#END