 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H4 Fe0.62 Mg0.12 O4 P0.50' 
_chemical_formula_weight          121.46 
 
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   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.1023   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0000 
 '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' 
 'Mg'  'Mg'   0.0486   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x, -y, z' 
 'x+1/2, y+1/2, z' 
 'x+1/2, -y+1/2, z' 
 '-x, -y, -z' 
 '-x, y, -z' 
 '-x+1/2, -y+1/2, -z' 
 '-x+1/2, y+1/2, -z' 
 
_cell_length_a                    10.1288(17) 
_cell_length_b                    13.492(3) 
_cell_length_c                    4.7036(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  104.704(13) 
_cell_angle_gamma                 90.00 
_cell_volume                      621.7(2) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.595 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              490 
_exptl_absorpt_coefficient_mu     3.267 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3105 
_diffrn_reflns_av_R_equivalents   0.0225 
_diffrn_reflns_av_sigmaI/netI     0.0174 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        6 
_diffrn_reflns_theta_min          4.16 
_diffrn_reflns_theta_max          30.00 
_reflns_number_total              915 
_reflns_number_gt                 852 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0558P)²+2.1226P] 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      SHELXL 
_refine_ls_extinction_coef        0.0033(19) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          915 
_refine_ls_number_parameters      57 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0340 
_refine_ls_R_factor_gt            0.0308 
_refine_ls_wR_factor_ref          0.0990 
_refine_ls_wR_factor_gt           0.0973 
_refine_ls_goodness_of_fit_ref    1.200 
_refine_ls_restrained_S_all       1.200 
_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 0.0000 0.0000 0.0105(2) Uani 1 4 d S . . 
Fe2 Fe 0.0000 0.38984(4) 0.0000 0.0074(2) Uani 0.712(7) 2 d SP . . 
Mg2 Mg 0.0000 0.38984(4) 0.0000 0.0074(2) Uani 0.288(7) 2 d SP . . 
P1 P 0.31449(8) 0.0000 0.37804(19) 0.0050(2) Uani 1 2 d S . . 
O1 O 0.34550(17) 0.09514(13) 0.2246(4) 0.0084(4) Uani 1 1 d . . . 
O2 O 0.6074(2) 0.0000 0.2961(6) 0.0082(5) Uani 1 2 d S . . 
O3 O 0.1585(2) 0.0000 0.3651(6) 0.0090(5) Uani 1 2 d S . . 
O11 O 0.1027(2) 0.27639(16) 0.2857(5) 0.0172(4) Uani 1 1 d . . . 
O12 O 0.39893(19) 0.38359(14) 0.1988(5) 0.0126(4) Uani 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 
Fe1 0.0074(3) 0.0143(4) 0.0092(4) 0.000 0.0010(3) 0.000 
Fe2 0.0069(3) 0.0088(3) 0.0066(4) 0.000 0.0021(2) 0.000 
Mg2 0.0069(3) 0.0088(3) 0.0066(4) 0.000 0.0021(2) 0.000 
P1 0.0037(4) 0.0078(4) 0.0034(4) 0.000 0.0008(3) 0.000 
O1 0.0088(7) 0.0088(8) 0.0085(9) 0.0017(6) 0.0038(6) 0.0004(6) 
O2 0.0076(10) 0.0130(11) 0.0028(12) 0.000 -0.0008(8) 0.000 
O3 0.0040(10) 0.0172(12) 0.0057(12) 0.000 0.0013(8) 0.000 
O11 0.0223(10) 0.0155(9) 0.0132(11) 0.0028(7) 0.0034(8) 0.0032(7) 
O12 0.0104(8) 0.0166(9) 0.0104(10) 0.0005(7) 0.0019(7) 0.0002(6) 
 
_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 O3 2.031(3) 5 ? 
Fe1 O3 2.031(3) . ? 
Fe1 O12 2.2081(19) 7 ? 
Fe1 O12 2.2081(19) 3_445 ? 
Fe1 O12 2.2081(19) 8_545 ? 
Fe1 O12 2.2081(19) 4_455 ? 
Fe2 O1 2.1084(17) 4_455 ? 
Fe2 O1 2.1084(17) 7 ? 
Fe2 O11 2.126(2) 6 ? 
Fe2 O11 2.126(2) . ? 
Fe2 O2 2.1364(19) 3_455 ? 
Fe2 O2 2.1364(19) 7 ? 
Fe2 Mg2 2.9727(13) 5_565 ? 
Fe2 Fe2 2.9727(13) 5_565 ? 
P1 O2 1.536(3) 5_656 ? 
P1 O1 1.5435(18) 2 ? 
P1 O1 1.5435(18) . ? 
P1 O3 1.566(2) . ? 
O1 Mg2 2.1084(17) 7 ? 
O1 Fe2 2.1084(17) 7 ? 
O2 P1 1.536(3) 5_656 ? 
O2 Fe2 2.1364(19) 3_545 ? 
O2 Mg2 2.1364(19) 3_545 ? 
O2 Fe2 2.1364(19) 7 ? 
O2 Mg2 2.1364(19) 7 ? 
O12 Fe1 2.2081(19) 3 ? 
 
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 
O3 Fe1 O3 180.00(19) 5 . ? 
O3 Fe1 O12 89.65(7) 5 7 ? 
O3 Fe1 O12 90.35(7) . 7 ? 
O3 Fe1 O12 90.35(7) 5 3_445 ? 
O3 Fe1 O12 89.65(7) . 3_445 ? 
O12 Fe1 O12 180.00(11) 7 3_445 ? 
O3 Fe1 O12 89.65(7) 5 8_545 ? 
O3 Fe1 O12 90.35(7) . 8_545 ? 
O12 Fe1 O12 90.68(10) 7 8_545 ? 
O12 Fe1 O12 89.32(10) 3_445 8_545 ? 
O3 Fe1 O12 90.35(7) 5 4_455 ? 
O3 Fe1 O12 89.65(7) . 4_455 ? 
O12 Fe1 O12 89.32(10) 7 4_455 ? 
O12 Fe1 O12 90.68(10) 3_445 4_455 ? 
O12 Fe1 O12 180.00(11) 8_545 4_455 ? 
O1 Fe2 O1 168.97(10) 4_455 7 ? 
O1 Fe2 O11 94.57(8) 4_455 6 ? 
O1 Fe2 O11 93.37(8) 7 6 ? 
O1 Fe2 O11 93.37(8) 4_455 . ? 
O1 Fe2 O11 94.57(8) 7 . ? 
O11 Fe2 O11 87.92(12) 6 . ? 
O1 Fe2 O2 85.78(8) 4_455 3_455 ? 
O1 Fe2 O2 86.55(8) 7 3_455 ? 
O11 Fe2 O2 178.03(8) 6 3_455 ? 
O11 Fe2 O2 90.13(8) . 3_455 ? 
O1 Fe2 O2 86.55(8) 4_455 7 ? 
O1 Fe2 O2 85.78(8) 7 7 ? 
O11 Fe2 O2 90.13(8) 6 7 ? 
O11 Fe2 O2 178.03(8) . 7 ? 
O2 Fe2 O2 91.83(10) 3_455 7 ? 
O1 Fe2 Mg2 84.48(5) 4_455 5_565 ? 
O1 Fe2 Mg2 84.48(5) 7 5_565 ? 
O11 Fe2 Mg2 136.04(6) 6 5_565 ? 
O11 Fe2 Mg2 136.04(6) . 5_565 ? 
O2 Fe2 Mg2 45.91(5) 3_455 5_565 ? 
O2 Fe2 Mg2 45.91(5) 7 5_565 ? 
O1 Fe2 Fe2 84.48(5) 4_455 5_565 ? 
O1 Fe2 Fe2 84.48(5) 7 5_565 ? 
O11 Fe2 Fe2 136.04(6) 6 5_565 ? 
O11 Fe2 Fe2 136.04(6) . 5_565 ? 
O2 Fe2 Fe2 45.91(5) 3_455 5_565 ? 
O2 Fe2 Fe2 45.91(5) 7 5_565 ? 
Mg2 Fe2 Fe2 0.0 5_565 5_565 ? 
O2 P1 O1 110.62(9) 5_656 2 ? 
O2 P1 O1 110.62(9) 5_656 . ? 
O1 P1 O1 112.54(14) 2 . ? 
O2 P1 O3 107.33(14) 5_656 . ? 
O1 P1 O3 107.75(9) 2 . ? 
O1 P1 O3 107.75(9) . . ? 
P1 O1 Mg2 125.40(10) . 7 ? 
P1 O1 Fe2 125.40(10) . 7 ? 
Mg2 O1 Fe2 0.00(3) 7 7 ? 
P1 O2 Fe2 134.32(6) 5_656 3_545 ? 
P1 O2 Mg2 134.32(6) 5_656 3_545 ? 
Fe2 O2 Mg2 0.00(2) 3_545 3_545 ? 
P1 O2 Fe2 134.32(6) 5_656 7 ? 
Fe2 O2 Fe2 88.17(10) 3_545 7 ? 
Mg2 O2 Fe2 88.17(10) 3_545 7 ? 
P1 O2 Mg2 134.32(6) 5_656 7 ? 
Fe2 O2 Mg2 88.17(10) 3_545 7 ? 
Mg2 O2 Mg2 88.17(10) 3_545 7 ? 
Fe2 O2 Mg2 0.00(2) 7 7 ? 
P1 O3 Fe1 127.32(15) . . ? 
 
_diffrn_measured_fraction_theta_max    0.962 
_diffrn_reflns_theta_full              30.00 
_diffrn_measured_fraction_theta_full   0.962 
_refine_diff_density_max    0.893 
_refine_diff_density_min   -0.924 
_refine_diff_density_rms    0.142 
