 
data_sad1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
  
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'Cl Fe2 H3 Li3 O9 P3'
_chemical_formula_sum 
 'Cl Fe2 H3 Li3 O9 P3' 
_chemical_formula_weight          407.90 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'H'  'H'   0.0000   0.0000 
 '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' 
 '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' 
 
_symmetry_cell_setting           'Orthorhombic'
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'
 
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' 
 
_cell_length_a                    9.139(2) 
_cell_length_b                    15.266(4) 
_cell_length_c                    7.0940(17) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      989.8(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     986
_cell_measurement_theta_min        3.87
_cell_measurement_theta_max       25.68
 
_exptl_crystal_description       'broken'
_exptl_crystal_colour            'green'
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.13 
_exptl_crystal_density_meas       'none' 
_exptl_crystal_density_diffrn     2.737 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              792 
_exptl_absorpt_coefficient_mu     3.714 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.4693 
_exptl_absorpt_correction_T_max   0.6439 
_exptl_absorpt_process_details    '(SADABS; Bruker, 2008)' 
 
_exptl_special_details 
; 
  
; 
 
_diffrn_ambient_temperature       200(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             9437 
_diffrn_reflns_av_R_equivalents   0.0295 
_diffrn_reflns_av_sigmaI/netI     0.0145 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        8 
_diffrn_reflns_theta_min          2.67 
_diffrn_reflns_theta_max          25.68 
_reflns_number_total              982 
_reflns_number_gt                 941 
_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)+(0.0411P)²+1.1744P] 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          982 
_refine_ls_number_parameters      93 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0240 
_refine_ls_R_factor_gt            0.0230 
_refine_ls_wR_factor_ref          0.0661 
_refine_ls_wR_factor_gt           0.0654 
_refine_ls_goodness_of_fit_ref    1.125 
_refine_ls_restrained_S_all       1.125 
_refine_ls_shift/su_max           0.001 
_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 0.62631(4) 0.63532(2) 0.48115(5) 0.00814(15) Uani 1 1 d . . . 
P1 P 0.60170(6) 0.45227(4) 0.22508(8) 0.00813(17) Uani 1 1 d . . . 
P2 P 0.39091(9) 0.7500 0.19558(12) 0.0084(2) Uani 1 2 d S . . 
O1 O 0.75611(18) 0.45578(10) 0.1447(2) 0.0119(4) Uani 1 1 d . . . 
O2 O 0.55165(18) 0.54337(10) 0.2834(2) 0.0106(3) Uani 1 1 d . . . 
O3 O 0.58452(17) 0.38610(11) 0.3872(2) 0.0109(3) Uani 1 1 d . . . 
O4 O 0.29833(18) 0.66721(10) 0.1918(2) 0.0130(4) Uani 1 1 d . . . 
O5 O 0.4923(2) 0.7500 0.3676(3) 0.0098(5) Uani 1 2 d S . . 
Cl1 Cl 0.66554(9) 0.7500 0.72893(11) 0.0130(2) Uani 1 2 d S . . 
Li1 Li 0.3491(4) 0.5690(3) 0.3526(6) 0.0145(8) Uani 1 1 d . . . 
Li2 Li 0.3929(7) 0.7500 0.6221(10) 0.0193(13) Uani 1 2 d S . . 
H1 H 0.510(3) 0.420(2) 0.101(5) 0.029 Uiso 1 1 d . . . 
H2 H 0.475(5) 0.7500 0.036(6) 0.029 Uiso 1 2 d S . . 
 
 
_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 O4 2.0529(17) 6_656 ? 
Fe1 O2 2.0985(16) . ? 
Fe1 O1 2.1059(16) 2_665 ? 
Fe1 O3 2.1661(17) 5_666 ? 
Fe1 O5 2.2833(15) . ? 
Fe1 Cl1 2.5066(8) . ? 
Fe1 Li1 2.877(4) . ? 
Fe1 Li2 2.935(5) . ? 
P1 O2 1.5213(16) . ? 
P1 O1 1.5231(17) . ? 
P1 O3 1.5386(17) . ? 
P1 Li1 2.931(4) 6_656 ? 
P1 Li1 3.047(4) 5_666 ? 
P1 Li1 3.053(4) . ? 
P1 H1 1.31(3) . ? 
P2 O4 1.5211(17) . ? 
P2 O4 1.5211(17) 7_575 ? 
P2 O5 1.532(2) . ? 
P2 Li1 3.004(4) 7_575 ? 
P2 Li1 3.004(4) . ? 
P2 Li2 3.025(7) . ? 
P2 H2 1.37(4) . ? 
O1 Li1 1.926(4) 6_656 ? 
O1 Fe1 2.1059(16) 2_664 ? 
O2 Li1 1.955(4) . ? 
O3 Li1 2.061(5) 5_666 ? 
O3 Li2 2.0890(18) 5_666 ? 
O3 Fe1 2.1661(17) 5_666 ? 
O4 Li1 1.940(4) . ? 
O4 Fe1 2.0529(17) 6_556 ? 
O5 Li2 2.021(7) . ? 
O5 Fe1 2.2833(15) 7_575 ? 
Cl1 Li2 2.331(6) 6_657 ? 
Cl1 Fe1 2.5066(8) 7_575 ? 
Cl1 Li2 2.605(7) . ? 
Li1 O1 1.926(4) 6_556 ? 
Li1 O3 2.061(5) 5_666 ? 
Li1 P1 2.931(4) 6_556 ? 
Li1 P1 3.047(4) 5_666 ? 
Li1 Li2 3.384(6) . ? 
Li2 O3 2.0890(18) 3_656 ? 
Li2 O3 2.0890(18) 5_666 ? 
Li2 Cl1 2.331(6) 6_557 ? 
Li2 Fe1 2.935(5) 7_575 ? 
Li2 Li1 3.384(6) 7_575 ? 
 
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 
O4 Fe1 O2 90.46(7) 6_656 . ? 
O4 Fe1 O1 95.46(7) 6_656 2_665 ? 
O2 Fe1 O1 95.31(6) . 2_665 ? 
O4 Fe1 O3 167.10(7) 6_656 5_666 ? 
O2 Fe1 O3 84.15(6) . 5_666 ? 
O1 Fe1 O3 96.70(7) 2_665 5_666 ? 
O4 Fe1 O5 91.02(7) 6_656 . ? 
O2 Fe1 O5 95.89(6) . . ? 
O1 Fe1 O5 167.01(7) 2_665 . ? 
O3 Fe1 O5 77.93(7) 5_666 . ? 
O4 Fe1 Cl1 98.27(5) 6_656 . ? 
O2 Fe1 Cl1 169.25(5) . . ? 
O1 Fe1 Cl1 90.11(5) 2_665 . ? 
O3 Fe1 Cl1 86.00(5) 5_666 . ? 
O5 Fe1 Cl1 77.80(5) . . ? 
O4 Fe1 Li1 124.64(10) 6_656 . ? 
O2 Fe1 Li1 42.80(10) . . ? 
O1 Fe1 Li1 113.05(10) 2_665 . ? 
O3 Fe1 Li1 45.59(10) 5_666 . ? 
O5 Fe1 Li1 71.69(9) . . ? 
Cl1 Fe1 Li1 126.45(9) . . ? 
O4 Fe1 Li2 128.22(9) 6_656 . ? 
O2 Fe1 Li2 112.97(13) . . ? 
O1 Fe1 Li2 125.25(13) 2_665 . ? 
O3 Fe1 Li2 45.30(9) 5_666 . ? 
O5 Fe1 Li2 43.37(13) . . ? 
Cl1 Fe1 Li2 56.54(12) . . ? 
Li1 Fe1 Li2 71.20(14) . . ? 
O2 P1 O1 110.38(9) . . ? 
O2 P1 O3 111.48(9) . . ? 
O1 P1 O3 113.42(9) . . ? 
O2 P1 Li1 74.18(10) . 6_656 ? 
O1 P1 Li1 36.24(10) . 6_656 ? 
O3 P1 Li1 128.20(11) . 6_656 ? 
O2 P1 Li1 82.78(10) . 5_666 ? 
O1 P1 Li1 103.60(10) . 5_666 ? 
O3 P1 Li1 37.84(10) . 5_666 ? 
Li1 P1 Li1 97.80(10) 6_656 5_666 ? 
O2 P1 Li1 32.72(10) . . ? 
O1 P1 Li1 142.29(10) . . ? 
O3 P1 Li1 94.85(10) . . ? 
Li1 P1 Li1 106.52(13) 6_656 . ? 
Li1 P1 Li1 83.25(11) 5_666 . ? 
O2 P1 H1 109.4(13) . . ? 
O1 P1 H1 110.8(13) . . ? 
O3 P1 H1 101.0(13) . . ? 
Li1 P1 H1 126.5(13) 6_656 . ? 
Li1 P1 H1 135.6(13) 5_666 . ? 
Li1 P1 H1 86.2(13) . . ? 
O4 P2 O4 112.37(14) . 7_575 ? 
O4 P2 O5 110.52(8) . . ? 
O4 P2 O5 110.52(8) 7_575 . ? 
O4 P2 Li1 134.43(11) . 7_575 ? 
O4 P2 Li1 34.04(10) 7_575 7_575 ? 
O5 P2 Li1 77.40(9) . 7_575 ? 
O4 P2 Li1 34.04(10) . . ? 
O4 P2 Li1 134.43(11) 7_575 . ? 
O5 P2 Li1 77.40(9) . . ? 
Li1 P2 Li1 133.84(16) 7_575 . ? 
O4 P2 Li2 91.20(10) . . ? 
O4 P2 Li2 91.20(10) 7_575 . ? 
O5 P2 Li2 36.89(15) . . ? 
Li1 P2 Li2 68.28(8) 7_575 . ? 
Li1 P2 Li2 68.28(8) . . ? 
O4 P2 H2 107.4(10) . . ? 
O4 P2 H2 107.4(10) 7_575 . ? 
O5 P2 H2 108(2) . . ? 
Li1 P2 H2 112.2(2) 7_575 . ? 
Li1 P2 H2 112.2(2) . . ? 
Li2 P2 H2 145.4(19) . . ? 
P1 O1 Li1 115.89(15) . 6_656 ? 
P1 O1 Fe1 130.99(9) . 2_664 ? 
Li1 O1 Fe1 111.90(14) 6_656 2_664 ? 
P1 O2 Li1 122.40(15) . . ? 
P1 O2 Fe1 134.07(10) . . ? 
Li1 O2 Fe1 90.36(14) . . ? 
P1 O3 Li1 114.90(15) . 5_666 ? 
P1 O3 Li2 128.3(2) . 5_666 ? 
Li1 O3 Li2 109.3(2) 5_666 5_666 ? 
P1 O3 Fe1 120.81(9) . 5_666 ? 
Li1 O3 Fe1 85.75(13) 5_666 5_666 ? 
Li2 O3 Fe1 87.21(18) 5_666 5_666 ? 
P2 O4 Li1 119.93(16) . . ? 
P2 O4 Fe1 129.31(10) . 6_556 ? 
Li1 O4 Fe1 110.55(14) . 6_556 ? 
P2 O5 Li2 116.0(2) . . ? 
P2 O5 Fe1 127.26(6) . 7_575 ? 
Li2 O5 Fe1 85.75(14) . 7_575 ? 
P2 O5 Fe1 127.26(6) . . ? 
Li2 O5 Fe1 85.75(14) . . ? 
Fe1 O5 Fe1 100.13(9) 7_575 . ? 
Li2 Cl1 Fe1 116.45(11) 6_657 . ? 
Li2 Cl1 Fe1 116.45(11) 6_657 7_575 ? 
Fe1 Cl1 Fe1 88.60(3) . 7_575 ? 
Li2 Cl1 Li2 169.96(12) 6_657 . ? 
Fe1 Cl1 Li2 70.06(10) . . ? 
Fe1 Cl1 Li2 70.06(10) 7_575 . ? 
O1 Li1 O4 126.4(2) 6_556 . ? 
O1 Li1 O2 103.9(2) 6_556 . ? 
O4 Li1 O2 103.5(2) . . ? 
O1 Li1 O3 114.8(2) 6_556 5_666 ? 
O4 Li1 O3 109.9(2) . 5_666 ? 
O2 Li1 O3 90.72(18) . 5_666 ? 
O1 Li1 Fe1 134.53(19) 6_556 . ? 
O4 Li1 Fe1 97.17(16) . . ? 
O2 Li1 Fe1 46.83(10) . . ? 
O3 Li1 Fe1 48.66(10) 5_666 . ? 
O1 Li1 P1 27.88(8) 6_556 6_556 ? 
O4 Li1 P1 100.08(16) . 6_556 ? 
O2 Li1 P1 124.18(19) . 6_556 ? 
O3 Li1 P1 126.72(18) 5_666 6_556 ? 
Fe1 Li1 P1 162.36(16) . 6_556 ? 
O1 Li1 P2 152.3(2) 6_556 . ? 
O4 Li1 P2 26.03(8) . . ? 
O2 Li1 P2 88.30(15) . . ? 
O3 Li1 P2 89.34(15) 5_666 . ? 
Fe1 Li1 P2 71.43(9) . . ? 
P1 Li1 P2 126.00(14) 6_556 . ? 
O1 Li1 P1 87.69(15) 6_556 5_666 ? 
O4 Li1 P1 134.07(19) . 5_666 ? 
O2 Li1 P1 94.92(15) . 5_666 ? 
O3 Li1 P1 27.26(8) 5_666 5_666 ? 
Fe1 Li1 P1 66.15(9) . 5_666 ? 
P1 Li1 P1 103.54(12) 6_556 5_666 ? 
P2 Li1 P1 116.34(13) . 5_666 ? 
O1 Li1 P1 79.22(14) 6_556 . ? 
O4 Li1 P1 117.23(18) . . ? 
O2 Li1 P1 24.88(8) . . ? 
O3 Li1 P1 103.70(16) 5_666 . ? 
Fe1 Li1 P1 68.49(9) . . ? 
P1 Li1 P1 99.96(12) 6_556 . ? 
P2 Li1 P1 109.31(13) . . ? 
P1 Li1 P1 96.75(11) 5_666 . ? 
O1 Li1 Li2 141.2(2) 6_556 . ? 
O4 Li1 Li2 74.29(16) . . ? 
O2 Li1 Li2 101.13(19) . . ? 
O3 Li1 Li2 35.64(13) 5_666 . ? 
Fe1 Li1 Li2 55.20(13) . . ? 
P1 Li1 Li2 133.94(18) 6_556 . ? 
P2 Li1 Li2 56.16(12) . . ? 
P1 Li1 Li2 60.92(12) 5_666 . ? 
P1 Li1 Li2 123.67(17) . . ? 
O5 Li2 O3 85.85(19) . 3_656 ? 
O5 Li2 O3 85.85(19) . 5_666 ? 
O3 Li2 O3 168.1(4) 3_656 5_666 ? 
O5 Li2 Cl1 143.7(3) . 6_557 ? 
O3 Li2 Cl1 95.87(18) 3_656 6_557 ? 
O3 Li2 Cl1 95.87(18) 5_666 6_557 ? 
O5 Li2 Cl1 80.2(2) . . ? 
O3 Li2 Cl1 85.10(18) 3_656 . ? 
O3 Li2 Cl1 85.10(18) 5_666 . ? 
Cl1 Li2 Cl1 136.1(3) 6_557 . ? 
O5 Li2 Fe1 50.87(12) . 7_575 ? 
O3 Li2 Fe1 47.48(11) 3_656 7_575 ? 
O3 Li2 Fe1 120.7(2) 5_666 7_575 ? 
Cl1 Li2 Fe1 143.34(8) 6_557 7_575 ? 
Cl1 Li2 Fe1 53.40(11) . 7_575 ? 
O5 Li2 Fe1 50.87(12) . . ? 
O3 Li2 Fe1 120.7(2) 3_656 . ? 
O3 Li2 Fe1 47.48(11) 5_666 . ? 
Cl1 Li2 Fe1 143.34(8) 6_557 . ? 
Cl1 Li2 Fe1 53.40(11) . . ? 
Fe1 Li2 Fe1 73.23(15) 7_575 . ? 
O5 Li2 P2 27.07(12) . . ? 
O3 Li2 P2 88.2(2) 3_656 . ? 
O3 Li2 P2 88.2(2) 5_666 . ? 
Cl1 Li2 P2 116.6(2) 6_557 . ? 
Cl1 Li2 P2 107.3(2) . . ? 
Fe1 Li2 P2 70.35(14) 7_575 . ? 
Fe1 Li2 P2 70.35(14) . . ? 
O5 Li2 Li1 63.17(14) . . ? 
O3 Li2 Li1 143.7(3) 3_656 . ? 
O3 Li2 Li1 35.09(13) 5_666 . ? 
Cl1 Li2 Li1 98.67(16) 6_557 . ? 
Cl1 Li2 Li1 106.12(15) . . ? 
Fe1 Li2 Li1 112.4(2) 7_575 . ? 
Fe1 Li2 Li1 53.60(9) . . ? 
P2 Li2 Li1 55.56(12) . . ? 
O5 Li2 Li1 63.17(14) . 7_575 ? 
O3 Li2 Li1 35.09(13) 3_656 7_575 ? 
O3 Li2 Li1 143.7(3) 5_666 7_575 ? 
Cl1 Li2 Li1 98.67(16) 6_557 7_575 ? 
Cl1 Li2 Li1 106.12(15) . 7_575 ? 
Fe1 Li2 Li1 53.60(9) 7_575 7_575 ? 
Fe1 Li2 Li1 112.4(2) . 7_575 ? 
P2 Li2 Li1 55.56(12) . 7_575 ? 
Li1 Li2 Li1 109.5(2) . 7_575 ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.68 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.600 
_refine_diff_density_min   -0.403 
_refine_diff_density_rms    0.108 
