 
data_sad1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 Lithium Iron Phosphate Hydroxide 
; 
_chemical_name_common             'Lithium Iron Phosphate Hydroxide'  
_chemical_melting_point           'N/A' 
_chemical_formula_moiety          'Fe H O5 P, Li'  
_chemical_formula_sum 
 'Fe H Li O5 P' 
_chemical_formula_weight          174.77 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Li'  'Li'  -0.0003   0.0001 
 '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' 
 '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' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'Triclinic' 
_symmetry_space_group_name_H-M    'P-1   '
_symmetry_space_group_name_Hall   '-P 1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    5.3506(10) 
_cell_length_b                    7.2877(14) 
_cell_length_c                    5.1174(10) 
_cell_angle_alpha                 109.237(2) 
_cell_angle_beta                  97.878(2) 
_cell_angle_gamma                 106.397(2) 
_cell_volume                      174.81(6) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     893
_cell_measurement_theta_min        3.16
_cell_measurement_theta_max       28.28
 
_exptl_crystal_description       'octahedral'
_exptl_crystal_colour            'green' 
_exptl_crystal_size_max           0.26 
_exptl_crystal_size_mid           0.07 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       'none' 
_exptl_crystal_density_diffrn     3.320 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              170 
_exptl_absorpt_coefficient_mu     4.651 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.3777 
_exptl_absorpt_correction_T_max   0.7677 
_exptl_absorpt_process_details    '(SADABS; Bruker, 2008)'  
 
_exptl_special_details 
; 
 
; 
 
_diffrn_ambient_temperature       293(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  'Bruker Smart-Apex CCD area detector'
_diffrn_measurement_method       'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             2148 
_diffrn_reflns_av_R_equivalents   0.0258 
_diffrn_reflns_av_sigmaI/netI     0.0333 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        6 
_diffrn_reflns_theta_min          3.16 
_diffrn_reflns_theta_max          28.28 
_reflns_number_total              850 
_reflns_number_gt                 760 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker SMART V5.631 (Bruker, 2002)'
_computing_cell_refinement        'Bruker SAINT V7.60A (Bruker, 2008)' 
_computing_data_reduction         'Bruker SAINT V7.60A (Bruker, 2008)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)' 
_computing_publication_material   'SHELXTL (Sheldrick, 2008)'
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0408P)²+1.3734P] where P=(Fo²+2Fc²)/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          850 
_refine_ls_number_parameters      80 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0437 
_refine_ls_R_factor_gt            0.0393 
_refine_ls_wR_factor_ref          0.1145 
_refine_ls_wR_factor_gt           0.1126 
_refine_ls_goodness_of_fit_ref    1.265 
_refine_ls_restrained_S_all       1.265 
_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 
Fe1 Fe 0.0000 0.5000 0.0000 0.0064(3) Uani 1 2 d S . . 
Fe2 Fe 0.0000 0.0000 0.0000 0.0062(3) Uani 1 2 d S . . 
P1 P 0.6373(3) 0.7688(2) 0.3245(3) 0.0055(3) Uani 1 1 d . . . 
O1 O 0.6588(7) 0.8802(6) 0.1146(8) 0.0081(7) Uani 1 1 d . . . 
O2 O 0.3397(7) 0.6626(6) 0.3103(8) 0.0086(7) Uani 1 1 d . . . 
O3 O 0.9529(8) 0.2774(6) 0.1579(8) 0.0077(7) Uani 1 1 d . . . 
O4 O 0.7869(8) 0.6160(6) 0.2682(8) 0.0088(7) Uani 1 1 d . . . 
O5 O 0.2456(7) 0.0689(6) 0.3670(7) 0.0076(7) Uani 1 1 d . . . 
Li1 Li 0.613(2) 0.1826(19) 0.254(2) 0.024(2) Uani 1 1 d . . . 
H1 H 1.027(14) 0.326(10) 0.319(16) 0.007(16) Uiso 1 1 d . . . 
 
 
_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 
Fe1 O2 1.995(4) 2_565 ? 
Fe1 O2 1.995(4) . ? 
Fe1 O3 2.010(4) 2_665 ? 
Fe1 O3 2.010(4) 1_455 ? 
Fe1 O4 2.027(4) 2_665 ? 
Fe1 O4 2.027(4) 1_455 ? 
Fe2 O5 1.958(4) 2 ? 
Fe2 O5 1.958(4) . ? 
Fe2 O3 2.017(4) 2_655 ? 
Fe2 O3 2.017(4) 1_455 ? 
Fe2 O1 2.042(4) 1_445 ? 
Fe2 O1 2.042(4) 2_665 ? 
Fe2 Li1 2.982(12) 2_655 ? 
Fe2 Li1 2.982(12) 1_455 ? 
Fe2 Li1 3.074(12) . ? 
Fe2 Li1 3.074(12) 2 ? 
P1 O4 1.523(4) . ? 
P1 O5 1.538(4) 2_666 ? 
P1 O2 1.541(4) . ? 
P1 O1 1.543(4) . ? 
P1 Li1 2.671(11) 2_666 ? 
O1 Fe2 2.042(4) 1_665 ? 
O1 Li1 2.045(12) 2_665 ? 
O1 Li1 2.177(13) 1_565 ? 
O2 Li1 2.083(12) 2_666 ? 
O3 Li1 1.944(12) . ? 
O3 Fe1 2.010(4) 1_655 ? 
O3 Fe2 2.017(4) 1_655 ? 
O3 H1 0.78(7) . ? 
O4 Fe1 2.027(4) 1_655 ? 
O5 P1 1.538(4) 2_666 ? 
O5 Li1 2.145(12) . ? 
Li1 O1 2.045(12) 2_665 ? 
Li1 O2 2.083(12) 2_666 ? 
Li1 O1 2.177(13) 1_545 ? 
Li1 P1 2.671(11) 2_666 ? 
Li1 Li1 2.84(2) 2_655 ? 
Li1 Fe2 2.982(12) 1_655 ? 
Li1 H1 2.09(7) . ? 
 
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 Fe1 O2 180.0(2) 2_565 . ? 
O2 Fe1 O3 87.05(15) 2_565 2_665 ? 
O2 Fe1 O3 92.95(15) . 2_665 ? 
O2 Fe1 O3 92.95(15) 2_565 1_455 ? 
O2 Fe1 O3 87.05(15) . 1_455 ? 
O3 Fe1 O3 180.0 2_665 1_455 ? 
O2 Fe1 O4 90.22(15) 2_565 2_665 ? 
O2 Fe1 O4 89.78(15) . 2_665 ? 
O3 Fe1 O4 86.55(15) 2_665 2_665 ? 
O3 Fe1 O4 93.45(15) 1_455 2_665 ? 
O2 Fe1 O4 89.78(15) 2_565 1_455 ? 
O2 Fe1 O4 90.22(15) . 1_455 ? 
O3 Fe1 O4 93.45(15) 2_665 1_455 ? 
O3 Fe1 O4 86.55(15) 1_455 1_455 ? 
O4 Fe1 O4 180.0(3) 2_665 1_455 ? 
O5 Fe2 O5 180.0(2) 2 . ? 
O5 Fe2 O3 89.68(15) 2 2_655 ? 
O5 Fe2 O3 90.32(15) . 2_655 ? 
O5 Fe2 O3 90.32(15) 2 1_455 ? 
O5 Fe2 O3 89.68(15) . 1_455 ? 
O3 Fe2 O3 180.0(3) 2_655 1_455 ? 
O5 Fe2 O1 85.04(15) 2 1_445 ? 
O5 Fe2 O1 94.96(15) . 1_445 ? 
O3 Fe2 O1 92.97(15) 2_655 1_445 ? 
O3 Fe2 O1 87.03(15) 1_455 1_445 ? 
O5 Fe2 O1 94.96(15) 2 2_665 ? 
O5 Fe2 O1 85.04(15) . 2_665 ? 
O3 Fe2 O1 87.03(15) 2_655 2_665 ? 
O3 Fe2 O1 92.97(15) 1_455 2_665 ? 
O1 Fe2 O1 180.0(2) 1_445 2_665 ? 
O5 Fe2 Li1 95.4(2) 2 2_655 ? 
O5 Fe2 Li1 84.6(2) . 2_655 ? 
O3 Fe2 Li1 40.2(3) 2_655 2_655 ? 
O3 Fe2 Li1 139.8(3) 1_455 2_655 ? 
O1 Fe2 Li1 133.1(3) 1_445 2_655 ? 
O1 Fe2 Li1 46.9(3) 2_665 2_655 ? 
O5 Fe2 Li1 84.6(2) 2 1_455 ? 
O5 Fe2 Li1 95.4(2) . 1_455 ? 
O3 Fe2 Li1 139.8(3) 2_655 1_455 ? 
O3 Fe2 Li1 40.2(3) 1_455 1_455 ? 
O1 Fe2 Li1 46.9(3) 1_445 1_455 ? 
O1 Fe2 Li1 133.1(3) 2_665 1_455 ? 
Li1 Fe2 Li1 180.0(4) 2_655 1_455 ? 
O5 Fe2 Li1 136.2(2) 2 . ? 
O5 Fe2 Li1 43.8(2) . . ? 
O3 Fe2 Li1 86.3(3) 2_655 . ? 
O3 Fe2 Li1 93.7(3) 1_455 . ? 
O1 Fe2 Li1 138.7(2) 1_445 . ? 
O1 Fe2 Li1 41.3(2) 2_665 . ? 
Li1 Fe2 Li1 55.9(4) 2_655 . ? 
Li1 Fe2 Li1 124.1(4) 1_455 . ? 
O5 Fe2 Li1 43.8(2) 2 2 ? 
O5 Fe2 Li1 136.2(2) . 2 ? 
O3 Fe2 Li1 93.7(3) 2_655 2 ? 
O3 Fe2 Li1 86.3(3) 1_455 2 ? 
O1 Fe2 Li1 41.3(2) 1_445 2 ? 
O1 Fe2 Li1 138.7(2) 2_665 2 ? 
Li1 Fe2 Li1 124.1(4) 2_655 2 ? 
Li1 Fe2 Li1 55.9(4) 1_455 2 ? 
Li1 Fe2 Li1 180.0(6) . 2 ? 
O4 P1 O5 109.9(2) . 2_666 ? 
O4 P1 O2 111.8(2) . . ? 
O5 P1 O2 104.1(2) 2_666 . ? 
O4 P1 O1 111.1(2) . . ? 
O5 P1 O1 109.2(2) 2_666 . ? 
O2 P1 O1 110.5(2) . . ? 
O4 P1 Li1 120.3(3) . 2_666 ? 
O5 P1 Li1 53.4(3) 2_666 2_666 ? 
O2 P1 Li1 51.1(3) . 2_666 ? 
O1 P1 Li1 128.6(3) . 2_666 ? 
P1 O1 Fe2 125.9(2) . 1_665 ? 
P1 O1 Li1 129.1(4) . 2_665 ? 
Fe2 O1 Li1 97.5(4) 1_665 2_665 ? 
P1 O1 Li1 117.0(4) . 1_565 ? 
Fe2 O1 Li1 89.9(3) 1_665 1_565 ? 
Li1 O1 Li1 84.4(5) 2_665 1_565 ? 
P1 O2 Fe1 135.6(2) . . ? 
P1 O2 Li1 93.8(4) . 2_666 ? 
Fe1 O2 Li1 128.8(4) . 2_666 ? 
Li1 O3 Fe1 116.7(4) . 1_655 ? 
Li1 O3 Fe2 97.7(4) . 1_655 ? 
Fe1 O3 Fe2 129.62(19) 1_655 1_655 ? 
Li1 O3 H1 90(5) . . ? 
Fe1 O3 H1 110(5) 1_655 . ? 
Fe2 O3 H1 105(5) 1_655 . ? 
P1 O4 Fe1 141.4(2) . 1_655 ? 
P1 O5 Fe2 143.4(2) 2_666 . ? 
P1 O5 Li1 91.5(3) 2_666 . ? 
Fe2 O5 Li1 96.9(3) . . ? 
O3 Li1 O1 101.5(5) . 2_665 ? 
O3 Li1 O2 109.4(6) . 2_666 ? 
O1 Li1 O2 135.6(6) 2_665 2_666 ? 
O3 Li1 O5 177.3(7) . . ? 
O1 Li1 O5 80.4(4) 2_665 . ? 
O2 Li1 O5 70.1(4) 2_666 . ? 
O3 Li1 O1 85.2(5) . 1_545 ? 
O1 Li1 O1 95.6(5) 2_665 1_545 ? 
O2 Li1 O1 117.6(6) 2_666 1_545 ? 
O5 Li1 O1 92.7(5) . 1_545 ? 
O3 Li1 P1 144.6(6) . 2_666 ? 
O1 Li1 P1 107.9(5) 2_665 2_666 ? 
O2 Li1 P1 35.1(2) 2_666 2_666 ? 
O5 Li1 P1 35.13(19) . 2_666 ? 
O1 Li1 P1 110.7(5) 1_545 2_666 ? 
O3 Li1 Li1 94.5(6) . 2_655 ? 
O1 Li1 Li1 49.8(4) 2_665 2_655 ? 
O2 Li1 Li1 150.5(8) 2_666 2_655 ? 
O5 Li1 Li1 85.1(6) . 2_655 ? 
O1 Li1 Li1 45.8(4) 1_545 2_655 ? 
P1 Li1 Li1 119.5(6) 2_666 2_655 ? 
O3 Li1 Fe2 42.1(3) . 1_655 ? 
O1 Li1 Fe2 99.3(4) 2_665 1_655 ? 
O2 Li1 Fe2 125.0(5) 2_666 1_655 ? 
O5 Li1 Fe2 135.9(5) . 1_655 ? 
O1 Li1 Fe2 43.2(2) 1_545 1_655 ? 
P1 Li1 Fe2 144.8(5) 2_666 1_655 ? 
Li1 Li1 Fe2 63.7(4) 2_655 1_655 ? 
O3 Li1 Fe2 142.5(5) . . ? 
O1 Li1 Fe2 41.2(2) 2_665 . ? 
O2 Li1 Fe2 104.3(4) 2_666 . ? 
O5 Li1 Fe2 39.2(2) . . ? 
O1 Li1 Fe2 93.6(4) 1_545 . ? 
P1 Li1 Fe2 70.2(3) 2_666 . ? 
Li1 Li1 Fe2 60.4(4) 2_655 . ? 
Fe2 Li1 Fe2 124.1(4) 1_655 . ? 
O3 Li1 H1 21.8(19) . . ? 
O1 Li1 H1 122(2) 2_665 . ? 
O2 Li1 H1 88(2) 2_666 . ? 
O5 Li1 H1 157(2) . . ? 
O1 Li1 H1 89.9(19) 1_545 . ? 
P1 Li1 H1 123(2) 2_666 . ? 
Li1 Li1 H1 113(2) 2_655 . ? 
Fe2 Li1 H1 51.5(19) 1_655 . ? 
Fe2 Li1 H1 163(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.975 
_diffrn_reflns_theta_full              28.28 
_diffrn_measured_fraction_theta_full   0.975 
_refine_diff_density_max    1.063 
_refine_diff_density_min   -0.738 
_refine_diff_density_rms    0.224 
