data_Beusite-(Ca) _audit_creation_method SHELXL-2014 _chemical_name_systematic ;Calcium manganese iron phosphate ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca Fe Mn O28 P2' _chemical_formula_weight 340.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O2-' 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' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7990(18) _cell_length_b 11.724(2) _cell_length_c 6.1700(12) _cell_angle_alpha 90 _cell_angle_beta 99.23(3) _cell_angle_gamma 90 _cell_volume 628.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4083 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description Small irregular flake _exptl_crystal_colour Very pale brown _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.610 _exptl_crystal_F_000 710 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 60 microns _exptl_crystal_size_mid 30 microns _exptl_crystal_size_min 30 microns _exptl_absorpt_coefficient_mu 5.654 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _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_source rotating-anode _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7192 _diffrn_reflns_av_unetI/netI 0.0115 _diffrn_reflns_av_R_equivalents 0.0125 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.345 _diffrn_reflns_theta_max 30.108 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1852 _reflns_number_gt 1832 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.5251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0064(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1852 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_gt 0.0155 _refine_ls_wR_factor_ref 0.0425 _refine_ls_wR_factor_gt 0.0425 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group M1 Ca 0.94894(3) 0.12351(2) 0.82833(4) 0.01288(9) Uani 1.078(2) 1 d . . P . . M2 Fe 0.71246(2) 0.07833(2) 0.32707(3) 0.01370(8) Uani 0.9973(16) 1 d . . P . . M3 Mn 0.35905(2) 0.19028(2) 0.13246(3) 0.01182(8) Uani 1.0254(18) 1 d . . P . . P1 P 0.09269(4) 0.13378(3) 0.39637(5) 0.00804(8) Uani 1 1 d . . . . . P2 P 0.60018(4) 0.08968(3) 0.80755(5) 0.00780(8) Uani 1 1 d . . . . . O1 O2- 0.08211(12) 0.07072(9) 0.17752(16) 0.01284(19) Uani 1 1 d . . . . . O2 O2- 0.47152(11) 0.17524(9) 0.83172(16) 0.01230(19) Uani 1 1 d . . . . . O3 O2- 0.93707(12) 0.18677(9) 0.42698(17) 0.01399(19) Uani 1 1 d . . . . . O4 O2- 0.68584(11) 0.12832(8) 0.62280(16) 0.01166(18) Uani 1 1 d . . . . . O5 O2- 0.20745(12) 0.23269(9) 0.38288(17) 0.0146(2) Uani 1 1 d . . . . . O6 O2- 0.72454(11) 0.09121(9) 0.01365(16) 0.01148(18) Uani 1 1 d . . . . . O7 O2- 0.14462(12) 0.05912(9) 0.59685(16) 0.01334(19) Uani 1 1 d . . . . . O8 O2- 0.53394(11) -0.03234(8) 0.76444(16) 0.01110(18) 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 M1 0.01427(13) 0.01039(13) 0.01330(13) -0.00136(8) 0.00017(9) 0.00011(8) M2 0.01367(11) 0.02039(12) 0.00700(10) 0.00024(6) 0.00153(7) 0.00437(7) M3 0.01322(11) 0.01207(11) 0.01001(11) 0.00025(6) 0.00141(7) 0.00250(6) P1 0.00773(14) 0.00825(14) 0.00829(15) -0.00009(10) 0.00169(11) -0.00055(10) P2 0.00756(14) 0.00931(15) 0.00675(14) 0.00004(10) 0.00175(11) 0.00054(10) O1 0.0169(5) 0.0115(4) 0.0100(4) -0.0024(3) 0.0019(3) 0.0005(3) O2 0.0113(4) 0.0143(4) 0.0119(4) 0.0013(3) 0.0036(3) 0.0048(3) O3 0.0107(4) 0.0169(5) 0.0151(5) -0.0005(3) 0.0043(3) 0.0037(3) O4 0.0123(4) 0.0150(4) 0.0085(4) 0.0004(3) 0.0043(3) -0.0017(3) O5 0.0168(5) 0.0157(5) 0.0117(4) -0.0007(4) 0.0037(4) -0.0092(4) O6 0.0091(4) 0.0177(5) 0.0074(4) -0.0003(3) 0.0004(3) -0.0001(3) O7 0.0164(4) 0.0117(4) 0.0113(4) 0.0032(3) 0.0007(3) 0.0006(3) O8 0.0108(4) 0.0095(4) 0.0129(4) 0.0000(3) 0.0014(3) -0.0010(3) _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 M1 O1 2.2932(11) 3_656 ? M1 O3 2.3127(11) 4_566 ? M1 O1 2.3640(12) 1_656 ? M1 O4 2.4555(13) . ? M1 O6 2.4645(12) 1_556 ? M1 O7 2.5225(12) 1_655 ? M1 O3 2.5711(12) . ? M1 O5 2.8078(12) 4_666 ? M1 P2 3.0765(8) . ? M1 P1 3.1149(7) 4_666 ? M1 P1 3.1303(8) 1_655 ? M1 P1 3.3155(7) 3_656 ? M2 O6 1.9595(10) . ? M2 O4 1.9659(10) . ? M2 O7 2.0517(11) 3_656 ? M2 O8 2.2176(11) 3_656 ? M2 O3 2.3477(12) . ? M2 M3 3.4113(8) . ? M3 O5 2.0755(12) 4_565 ? M3 O8 2.1278(10) 3_656 ? M3 O2 2.1416(11) 4_565 ? M3 O2 2.2455(11) 1_554 ? M3 O5 2.2528(12) . ? M3 O1 2.8631(11) . ? M3 P1 3.1317(9) . ? M3 P1 3.2825(8) 4_565 ? M3 P2 3.3160(7) 3_656 ? M3 P2 3.3578(9) 1_554 ? M3 M3 3.3879(6) 4_565 ? M3 M3 3.3879(6) 4_566 ? P1 O7 1.5243(10) . ? P1 O1 1.5291(10) . ? P1 O3 1.5427(11) 1_455 ? P1 O5 1.5486(10) . ? P1 M1 3.1150(7) 4_465 ? P1 M1 3.1303(8) 1_455 ? P1 M3 3.2825(8) 4_566 ? P1 M1 3.3155(7) 3_656 ? P1 M1 3.5322(10) 1_454 ? P2 O4 1.5324(10) . ? P2 O2 1.5377(10) . ? P2 O6 1.5390(11) 1_556 ? P2 O8 1.5515(10) . ? P2 M3 3.3160(7) 3_656 ? P2 M3 3.3579(9) 1_556 ? P2 M3 3.4042(7) 4_566 ? O1 M1 2.2932(11) 3_656 ? O1 M1 2.3639(12) 1_454 ? O2 M3 2.1416(11) 4_566 ? O2 M3 2.2455(11) 1_556 ? O3 P1 1.5426(11) 1_655 ? O3 M1 2.3128(11) 4_565 ? O5 M3 2.0755(12) 4_566 ? O5 M1 2.8078(12) 4_465 ? O6 P2 1.5390(11) 1_554 ? O6 M1 2.4645(12) 1_554 ? O7 M2 2.0517(11) 3_656 ? O7 M1 2.5225(12) 1_455 ? O8 M3 2.1278(10) 3_656 ? O8 M2 2.2175(11) 3_656 ? 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 O1 M1 O3 161.60(4) 3_656 4_566 ? O1 M1 O1 78.16(4) 3_656 1_656 ? O3 M1 O1 92.79(4) 4_566 1_656 ? O1 M1 O4 85.10(4) 3_656 . ? O3 M1 O4 92.02(4) 4_566 . ? O1 M1 O4 139.93(4) 1_656 . ? O1 M1 O6 75.66(3) 3_656 1_556 ? O3 M1 O6 87.27(4) 4_566 1_556 ? O1 M1 O6 81.60(4) 1_656 1_556 ? O4 M1 O6 58.93(4) . 1_556 ? O1 M1 O7 77.55(4) 3_656 1_655 ? O3 M1 O7 120.04(4) 4_566 1_655 ? O1 M1 O7 98.87(4) 1_656 1_655 ? O4 M1 O7 112.77(4) . 1_655 ? O6 M1 O7 152.51(4) 1_556 1_655 ? O1 M1 O3 106.56(4) 3_656 . ? O3 M1 O3 88.82(3) 4_566 . ? O1 M1 O3 153.00(4) 1_656 . ? O4 M1 O3 66.83(4) . . ? O6 M1 O3 125.41(4) 1_556 . ? O7 M1 O3 57.79(4) 1_655 . ? O1 M1 O5 133.66(3) 3_656 4_666 ? O3 M1 O5 57.38(3) 4_566 4_666 ? O1 M1 O5 76.96(4) 1_656 4_666 ? O4 M1 O5 136.61(3) . 4_666 ? O6 M1 O5 136.93(3) 1_556 4_666 ? O7 M1 O5 68.54(3) 1_655 4_666 ? O3 M1 O5 81.33(4) . 4_666 ? O1 M1 P2 75.86(3) 3_656 . ? O3 M1 P2 92.76(3) 4_566 . ? O1 M1 P2 110.46(4) 1_656 . ? O4 M1 P2 29.53(2) . . ? O6 M1 P2 29.71(3) 1_556 . ? O7 M1 P2 134.80(3) 1_655 . ? O3 M1 P2 96.36(4) . . ? O5 M1 P2 149.98(2) 4_666 . ? O1 M1 P1 162.57(3) 3_656 4_666 ? O3 M1 P1 28.42(3) 4_566 4_666 ? O1 M1 P1 89.15(3) 1_656 4_666 ? O4 M1 P1 112.18(3) . 4_666 ? O6 M1 P1 114.59(3) 1_556 4_666 ? O7 M1 P1 92.89(3) 1_655 4_666 ? O3 M1 P1 79.58(3) . 4_666 ? O5 M1 P1 29.74(2) 4_666 4_666 ? P2 M1 P1 120.276(13) . 4_666 ? O1 M1 P1 95.06(3) 3_656 1_655 ? O3 M1 P1 103.21(3) 4_566 1_655 ? O1 M1 P1 125.25(3) 1_656 1_655 ? O4 M1 P1 92.04(3) . 1_655 ? O6 M1 P1 149.78(3) 1_556 1_655 ? O7 M1 P1 28.81(3) 1_655 1_655 ? O3 M1 P1 29.36(2) . 1_655 ? O5 M1 P1 69.44(3) 4_666 1_655 ? P2 M1 P1 120.40(3) . 1_655 ? P1 M1 P1 82.464(14) 4_666 1_655 ? O1 M1 P1 23.80(3) 3_656 3_656 ? O3 M1 P1 168.07(3) 4_566 3_656 ? O1 M1 P1 98.53(3) 1_656 3_656 ? O4 M1 P1 76.89(3) . 3_656 ? O6 M1 P1 90.64(3) 1_556 3_656 ? O7 M1 P1 62.01(3) 1_655 3_656 ? O3 M1 P1 82.82(3) . 3_656 ? O5 M1 P1 129.01(2) 4_666 3_656 ? P2 M1 P1 79.785(16) . 3_656 ? P1 M1 P1 154.519(12) 4_666 3_656 ? P1 M1 P1 73.236(12) 1_655 3_656 ? O6 M2 O4 157.88(4) . . ? O6 M2 O7 99.10(4) . 3_656 ? O4 M2 O7 100.47(5) . 3_656 ? O6 M2 O8 88.45(5) . 3_656 ? O4 M2 O8 92.96(5) . 3_656 ? O7 M2 O8 113.93(4) 3_656 3_656 ? O6 M2 O3 92.34(5) . . ? O4 M2 O3 79.36(4) . . ? O7 M2 O3 84.61(4) 3_656 . ? O8 M2 O3 161.09(4) 3_656 . ? O6 M2 M3 79.26(4) . . ? O4 M2 M3 88.54(4) . . ? O7 M2 M3 150.86(3) 3_656 . ? O8 M2 M3 37.35(3) 3_656 . ? O3 M2 M3 124.44(3) . . ? O6 M2 M1 138.24(3) . . ? O4 M2 M1 43.37(3) . . ? O7 M2 M1 70.06(3) 3_656 . ? O8 M2 M1 133.17(3) 3_656 . ? O3 M2 M1 47.63(3) . . ? M3 M2 M1 129.47(2) . . ? O5 M3 O8 143.27(4) 4_565 3_656 ? O5 M3 O2 106.76(5) 4_565 4_565 ? O8 M3 O2 109.11(4) 3_656 4_565 ? O5 M3 O2 74.76(4) 4_565 1_554 ? O8 M3 O2 86.92(4) 3_656 1_554 ? O2 M3 O2 107.93(4) 4_565 1_554 ? O5 M3 O5 91.83(4) 4_565 . ? O8 M3 O5 105.62(4) 3_656 . ? O2 M3 O5 73.36(4) 4_565 . ? O2 M3 O5 166.40(4) 1_554 . ? O5 M3 O1 80.17(4) 4_565 . ? O8 M3 O1 83.55(4) 3_656 . ? O2 M3 O1 128.81(4) 4_565 . ? O2 M3 O1 122.45(4) 1_554 . ? O5 M3 O1 55.57(4) . . ? O5 M3 P1 91.85(3) 4_565 . ? O8 M3 P1 89.58(3) 3_656 . ? O2 M3 P1 99.94(3) 4_565 . ? O2 M3 P1 151.50(3) 1_554 . ? O5 M3 P1 27.78(3) . . ? O1 M3 P1 29.12(2) . . ? O5 M3 P1 21.42(3) 4_565 4_565 ? O8 M3 P1 158.39(3) 3_656 4_565 ? O2 M3 P1 91.34(4) 4_565 4_565 ? O2 M3 P1 93.47(3) 1_554 4_565 ? O5 M3 P1 72.93(3) . 4_565 ? O1 M3 P1 78.02(3) . 4_565 ? P1 M3 P1 79.807(16) . 4_565 ? O5 M3 P2 123.97(3) 4_565 3_656 ? O8 M3 P2 21.65(3) 3_656 3_656 ? O2 M3 P2 129.26(3) 4_565 3_656 ? O2 M3 P2 87.73(3) 1_554 3_656 ? O5 M3 P2 101.96(3) . 3_656 ? O1 M3 P2 65.36(2) . 3_656 ? P1 M3 P2 78.999(10) . 3_656 ? P1 M3 P2 136.743(13) 4_565 3_656 ? O5 M3 P2 95.88(3) 4_565 1_554 ? O8 M3 P2 65.24(3) 3_656 1_554 ? O2 M3 P2 108.86(3) 4_565 1_554 ? O2 M3 P2 22.29(3) 1_554 1_554 ? O5 M3 P2 170.86(3) . 1_554 ? O1 M3 P2 121.00(3) . 1_554 ? P1 M3 P2 146.440(15) . 1_554 ? P1 M3 P2 115.489(16) 4_565 1_554 ? P2 M3 P2 69.608(12) 3_656 1_554 ? O5 M3 M3 40.40(3) 4_565 4_565 ? O8 M3 M3 124.56(3) 3_656 4_565 ? O2 M3 M3 98.69(3) 4_565 4_565 ? O2 M3 M3 38.34(3) 1_554 4_565 ? O5 M3 M3 128.30(3) . 4_565 ? O1 M3 M3 114.52(3) . 4_565 ? P1 M3 M3 132.08(2) . 4_565 ? P1 M3 M3 55.98(2) 4_565 4_565 ? P2 M3 M3 119.667(11) 3_656 4_565 ? P2 M3 M3 60.613(17) 1_554 4_565 ? O5 M3 M3 113.70(3) 4_565 4_566 ? O8 M3 M3 98.75(3) 3_656 4_566 ? O2 M3 M3 40.57(3) 4_565 4_566 ? O2 M3 M3 148.13(3) 1_554 4_566 ? O5 M3 M3 36.66(3) . 4_566 ? O1 M3 M3 89.41(3) . 4_566 ? P1 M3 M3 60.31(2) . 4_566 ? P1 M3 M3 92.30(2) 4_565 4_566 ? P2 M3 M3 108.860(11) 3_656 4_566 ? P2 M3 M3 141.358(16) 1_554 4_566 ? M3 M3 M3 131.173(17) 4_565 4_566 ? O7 P1 O1 114.01(6) . . ? O7 P1 O3 106.76(6) . 1_455 ? O1 P1 O3 111.92(6) . 1_455 ? O7 P1 O5 111.12(6) . . ? O1 P1 O5 105.22(6) . . ? O3 P1 O5 107.71(6) 1_455 . ? O7 P1 M1 134.13(4) . 4_465 ? O1 P1 M1 110.90(4) . 4_465 ? O3 P1 M1 45.52(4) 1_455 4_465 ? O5 P1 M1 64.08(5) . 4_465 ? O7 P1 M1 52.88(4) . 1_455 ? O1 P1 M1 139.25(4) . 1_455 ? O3 P1 M1 54.79(5) 1_455 1_455 ? O5 P1 M1 115.50(4) . 1_455 ? M1 P1 M1 86.507(14) 4_465 1_455 ? O7 P1 M3 113.04(5) . . ? O1 P1 M3 65.65(4) . . ? O3 P1 M3 137.01(4) 1_455 . ? O5 P1 M3 42.68(4) . . ? M1 P1 M3 93.340(14) 4_465 . ? M1 P1 M3 152.761(19) 1_455 . ? O7 P1 M3 84.31(5) . 4_566 ? O1 P1 M3 129.32(5) . 4_566 ? O3 P1 M3 106.09(4) 1_455 4_566 ? O5 P1 M3 29.31(4) . 4_566 ? M1 P1 M3 74.42(2) 4_465 4_566 ? M1 P1 M3 90.204(19) 1_455 4_566 ? M3 P1 M3 63.716(13) . 4_566 ? O7 P1 M1 79.37(4) . 3_656 ? O1 P1 M1 37.24(4) . 3_656 ? O3 P1 M1 112.14(4) 1_455 3_656 ? O5 P1 M1 133.48(4) . 3_656 ? M1 P1 M1 139.421(18) 4_465 3_656 ? M1 P1 M1 106.764(12) 1_455 3_656 ? M3 P1 M1 90.960(14) . 3_656 ? M3 P1 M1 141.301(13) 4_566 3_656 ? O7 P1 M1 143.00(4) . 1_454 ? O1 P1 M1 31.34(4) . 1_454 ? O3 P1 M1 87.22(5) 1_455 1_454 ? O5 P1 M1 96.03(4) . 1_454 ? M1 P1 M1 79.883(15) 4_465 1_454 ? M1 P1 M1 135.580(17) 1_455 1_454 ? M3 P1 M1 70.73(2) . 1_454 ? M3 P1 M1 125.33(2) 4_566 1_454 ? M1 P1 M1 63.647(11) 3_656 1_454 ? O4 P2 O2 109.69(6) . . ? O4 P2 O6 103.99(6) . 1_556 ? O2 P2 O6 110.44(6) . 1_556 ? O4 P2 O8 111.17(6) . . ? O2 P2 O8 110.85(6) . . ? O6 P2 O8 110.50(6) 1_556 . ? O4 P2 M1 52.16(4) . . ? O2 P2 M1 131.06(4) . . ? O6 P2 M1 52.54(4) 1_556 . ? O8 P2 M1 118.09(4) . . ? O4 P2 M3 108.57(4) . 3_656 ? O2 P2 M3 134.67(4) . 3_656 ? O6 P2 M3 82.50(4) 1_556 3_656 ? O8 P2 M3 30.39(4) . 3_656 ? M1 P2 M3 91.929(11) . 3_656 ? O4 P2 M3 140.67(4) . 1_556 ? O2 P2 M3 33.64(4) . 1_556 ? O6 P2 M3 86.34(4) 1_556 1_556 ? O8 P2 M3 99.80(4) . 1_556 ? M1 P2 M3 130.64(2) . 1_556 ? M3 P2 M3 110.391(11) 3_656 1_556 ? O4 P2 M3 84.02(4) . 4_566 ? O2 P2 M3 26.53(4) . 4_566 ? O6 P2 M3 125.29(4) 1_556 4_566 ? O8 P2 M3 116.52(4) . 4_566 ? M1 P2 M3 118.833(16) . 4_566 ? M3 P2 M3 146.748(13) 3_656 4_566 ? M3 P2 M3 60.130(12) 1_556 4_566 ? P1 O1 M1 118.96(6) . 3_656 ? P1 O1 M1 129.00(6) . 1_454 ? M1 O1 M1 101.84(4) 3_656 1_454 ? P1 O1 M3 85.23(5) . . ? M1 O1 M3 125.86(4) 3_656 . ? M1 O1 M3 95.08(4) 1_454 . ? P2 O2 M3 134.77(6) . 4_566 ? P2 O2 M3 124.07(6) . 1_556 ? M3 O2 M3 101.09(4) 4_566 1_556 ? P1 O3 M1 106.06(5) 1_655 4_565 ? P1 O3 M2 118.43(6) 1_655 . ? M1 O3 M2 121.56(5) 4_565 . ? P1 O3 M1 95.85(5) 1_655 . ? M1 O3 M1 122.30(4) 4_565 . ? M2 O3 M1 89.95(4) . . ? P2 O4 M2 138.44(6) . . ? P2 O4 M1 98.31(5) . . ? M2 O4 M1 103.28(5) . . ? P1 O5 M3 129.27(6) . 4_566 ? P1 O5 M3 109.54(6) . . ? M3 O5 M3 102.95(5) 4_566 . ? P1 O5 M1 86.18(5) . 4_465 ? M3 O5 M1 103.86(5) 4_566 4_465 ? M3 O5 M1 127.42(5) . 4_465 ? P2 O6 M2 132.12(6) 1_554 . ? P2 O6 M1 97.75(5) 1_554 1_554 ? M2 O6 M1 130.09(5) . 1_554 ? P1 O7 M2 136.86(7) . 3_656 ? P1 O7 M1 98.32(5) . 1_455 ? M2 O7 M1 123.68(5) 3_656 1_455 ? P2 O8 M3 127.96(6) . 3_656 ? P2 O8 M2 126.36(5) . 3_656 ? M3 O8 M2 103.43(4) 3_656 3_656 ? _refine_diff_density_max 0.857 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.117 _shelxl_version_number 2014-3 _shelx_res_file ; TITL p21c in P2(1)/c CELL 0.71073 8.7990 11.7240 6.1700 90.000 99.227 90.000 ZERR 4.00 0.0018 0.0023 0.0012 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC O2- 3.04484 7.98437 0.50181 3.73146 1.55609 0.32297 4.20924 = 23.9207 0.23641 0.0106 0.006 32.5 0.66 15.9994 SFAC P CA MN FE UNIT 32 8 4 4 4 L.S. 10 BOND FMAP 2 PLAN 20 ACTA WGHT 0.024100 0.525100 EXTI 0.006444 FVAR 0.56795 1.07811 0.99734 1.02544 M1 3 0.948944 0.123513 0.828334 21.00000 0.01427 0.01039 = 0.01330 -0.00136 0.00017 0.00011 M2 5 0.712462 0.078330 0.327074 31.00000 0.01367 0.02039 = 0.00700 0.00024 0.00153 0.00437 CONN 12 2 M3 M3 4 0.359054 0.190280 0.132458 41.00000 0.01322 0.01207 = 0.01001 0.00025 0.00141 0.00250 P1 2 0.092692 0.133776 0.396372 11.00000 0.00773 0.00825 = 0.00829 -0.00009 0.00169 -0.00055 P2 2 0.600179 0.089677 0.807549 11.00000 0.00756 0.00931 = 0.00675 0.00004 0.00175 0.00054 O1 1 0.082114 0.070725 0.177523 11.00000 0.01694 0.01148 = 0.01003 -0.00237 0.00193 0.00047 O2 1 0.471517 0.175241 0.831721 11.00000 0.01128 0.01430 = 0.01190 0.00135 0.00361 0.00484 O3 1 0.937072 0.186774 0.426981 11.00000 0.01068 0.01689 = 0.01510 -0.00051 0.00426 0.00370 O4 1 0.685841 0.128322 0.622804 11.00000 0.01230 0.01503 = 0.00852 0.00042 0.00426 -0.00174 O5 1 0.207446 0.232688 0.382883 11.00000 0.01684 0.01568 = 0.01171 -0.00068 0.00367 -0.00917 O6 1 0.724536 0.091205 0.013649 11.00000 0.00911 0.01766 = 0.00737 -0.00026 0.00038 -0.00006 O7 1 0.144622 0.059122 0.596848 11.00000 0.01642 0.01174 = 0.01135 0.00323 0.00068 0.00059 O8 1 0.533943 -0.032343 0.764443 11.00000 0.01076 0.00948 = 0.01289 -0.00002 0.00138 -0.00095 HKLF 4 REM p21c in P2(1)/c REM R1 = 0.0155 for 1832 Fo > 4sig(Fo) and 0.0156 for all 1852 data REM 122 parameters refined using 0 restraints END WGHT 0.0198 0.5381 REM Highest difference peak 0.857, deepest hole -0.556, 1-sigma level 0.117 Q1 1 0.6794 0.0244 0.3290 11.00000 0.05 0.86 Q2 1 0.9070 0.1119 0.9048 11.00000 0.05 0.59 Q3 1 0.6607 0.0876 -0.0849 11.00000 0.05 0.35 Q4 1 0.9984 0.1604 0.3974 11.00000 0.05 0.33 Q5 1 0.5729 0.0189 0.7969 11.00000 0.05 0.33 Q6 1 0.0715 0.0934 0.2648 11.00000 0.05 0.33 Q7 1 0.6445 -0.0729 0.5614 11.00000 0.05 0.32 Q8 1 0.2561 0.0811 0.8392 11.00000 0.05 0.32 Q9 1 0.4304 0.1865 0.2174 11.00000 0.05 0.32 Q10 1 0.9608 0.2380 0.4131 11.00000 0.05 0.32 Q11 1 0.0940 0.0424 0.1905 11.00000 0.05 0.31 Q12 1 0.7366 0.2218 0.7613 11.00000 0.05 0.31 Q13 1 0.3277 0.0562 0.5919 11.00000 0.05 0.31 Q14 1 0.7247 0.2150 -0.1373 11.00000 0.05 0.29 Q15 1 0.2775 0.0460 0.7521 11.00000 0.05 0.29 Q16 1 0.8010 0.2223 0.6564 11.00000 0.05 0.29 Q17 1 0.3375 0.0970 0.5934 11.00000 0.05 0.29 Q18 1 0.6473 0.1032 0.7145 11.00000 0.05 0.29 Q19 1 0.6382 0.2670 0.5764 11.00000 0.05 0.28 Q20 1 0.7967 -0.0444 0.0730 11.00000 0.05 0.26 ; _shelx_res_checksum 55335 _shelx_hkl_file ; -1 0 0 4.11 0.22 1 0 0 3.88 0.14 -2 0 0 3.46 0.22 2 0 0 3.71 0.13 -3 0 0 5544.34 108.98 3 0 0 5592.18 68.51 -4 0 0 454.85 6.54 4 0 0 453.95 6.51 -5 0 0 2881.43 48.23 5 0 0 2878.46 39.61 -6 0 0 689.55 11.74 6 0 0 699.50 9.97 -7 0 0 450.28 8.07 7 0 0 463.44 6.82 -8 0 0 167.06 3.85 8 0 0 167.59 2.91 -9 0 0 1256.85 21.97 9 0 0 1269.31 18.13 -10 0 0 27.41 2.17 10 0 0 26.83 0.94 -11 0 0 204.27 6.42 11 0 0 200.02 3.65 -12 0 0 354.13 9.94 12 0 0 349.94 6.69 -1 -1 0 79.70 1.38 1 -1 0 78.90 1.17 -1 1 0 79.74 1.54 1 1 0 79.77 1.37 -2 -1 0 22.29 0.69 2 -1 0 22.08 0.53 -2 1 0 23.16 0.63 2 1 0 21.81 0.39 -3 -1 0 692.29 11.03 3 -1 0 690.86 9.14 -3 1 0 651.56 12.00 3 1 0 687.52 7.81 -4 -1 0 1843.96 28.64 4 -1 0 1800.14 22.36 -4 1 0 1841.21 34.98 4 1 0 1793.71 22.40 -5 -1 0 2766.97 38.40 5 -1 0 2750.83 38.24 -5 1 0 2772.56 38.66 5 1 0 2782.06 43.40 -6 -1 0 150.47 3.54 6 -1 0 149.80 2.52 -6 1 0 153.49 2.19 6 1 0 149.39 2.49 -7 -1 0 169.45 3.44 7 -1 0 165.22 2.83 -7 1 0 168.15 3.70 7 1 0 169.02 2.81 -8 -1 0 3598.43 57.55 8 -1 0 3573.31 44.19 -8 1 0 3508.43 58.70 8 1 0 3535.39 57.00 -9 -1 0 417.96 9.99 9 -1 0 413.73 6.46 -9 1 0 422.72 8.14 9 1 0 408.01 7.50 -10 -1 0 38.03 1.72 10 -1 0 34.31 1.24 -10 1 0 38.30 1.69 10 1 0 33.95 1.07 -11 -1 0 13.61 1.76 11 -1 0 10.45 0.82 -11 1 0 9.08 1.47 11 1 0 10.82 0.71 -12 -1 0 474.78 12.40 12 -1 0 458.36 8.64 -12 1 0 466.89 12.31 12 1 0 479.60 7.51 0 -2 0 79.89 1.04 0 2 0 81.51 1.20 -1 -2 0 0.76 0.12 1 -2 0 0.93 0.10 -1 2 0 0.70 0.09 1 2 0 0.50 0.07 -2 -2 0 69.32 1.33 2 -2 0 67.94 0.86 -2 2 0 66.32 1.63 2 2 0 67.42 1.25 -3 -2 0 141.38 2.55 3 -2 0 141.06 1.94 -3 2 0 142.05 2.20 3 2 0 144.76 1.78 -4 -2 0 526.57 7.65 4 -2 0 524.70 6.71 -4 2 0 536.29 6.60 4 2 0 525.09 6.17 -5 -2 0 863.76 12.40 5 -2 0 868.14 10.41 -5 2 0 860.47 10.76 5 2 0 877.18 10.07 -6 -2 0 348.94 5.18 6 -2 0 332.10 4.57 -6 2 0 335.78 4.52 6 2 0 336.94 5.04 -7 -2 0 2247.52 36.81 7 -2 0 2247.72 31.48 -7 2 0 2257.66 30.96 7 2 0 2281.37 36.38 -8 -2 0 76.33 2.03 8 -2 0 72.70 1.57 -8 2 0 73.36 1.61 8 2 0 74.87 1.87 -9 -2 0 256.86 6.91 9 -2 0 265.21 4.33 -9 2 0 263.75 5.62 9 2 0 267.47 5.11 -10 -2 0 286.95 7.46 10 -2 0 268.92 5.29 -10 2 0 274.38 7.67 10 2 0 272.45 5.37 -11 -2 0 55.06 2.25 11 -2 0 53.00 1.71 -11 2 0 53.24 2.87 11 2 0 55.38 1.46 -12 -2 0 0.48 1.01 12 -2 0 1.22 0.49 -12 2 0 2.85 1.09 12 2 0 1.68 0.43 0 -3 0 0.17 0.09 0 3 0 0.51 0.09 -1 -3 0 6405.45 186.99 1 -3 0 6422.11 85.79 -1 3 0 6997.79 129.19 1 3 0 6674.66 109.29 -2 -3 0 8085.07 100.46 2 -3 0 6942.08 147.97 -2 3 0 7605.23 153.44 2 3 0 6682.79 132.54 -3 -3 0 1703.65 23.37 3 -3 0 1685.29 21.02 -3 3 0 1693.30 27.88 3 3 0 1719.51 21.20 -4 -3 0 1341.51 18.93 4 -3 0 1326.42 16.75 -4 3 0 1361.77 19.19 4 3 0 1356.53 15.39 -5 -3 0 268.15 4.81 5 -3 0 272.86 3.90 -5 3 0 276.37 4.19 5 3 0 284.05 3.76 -6 -3 0 158.70 2.70 6 -3 0 153.51 2.61 -6 3 0 155.76 2.63 6 3 0 155.10 2.08 -7 -3 0 31.81 1.18 7 -3 0 28.70 0.85 -7 3 0 30.08 0.89 7 3 0 30.32 1.01 -8 -3 0 1963.55 32.37 8 -3 0 1955.02 27.60 -8 3 0 1967.68 27.19 8 3 0 1979.13 31.87 -9 -3 0 25.30 1.20 9 -3 0 23.46 0.87 -9 3 0 24.72 1.10 9 3 0 23.10 1.02 -10 -3 0 114.43 3.96 10 -3 0 109.27 2.67 -10 3 0 113.67 2.77 10 3 0 109.93 2.70 -11 -3 0 326.63 8.65 11 -3 0 317.65 6.19 -11 3 0 309.55 8.82 11 3 0 325.88 5.29 -12 -3 0 10.07 1.26 12 -3 0 10.48 0.91 -12 3 0 13.30 1.76 12 3 0 12.83 0.83 0 -4 0 6944.35 114.69 0 4 0 7089.45 115.94 -1 -4 0 1297.12 23.28 1 -4 0 1377.30 13.84 -1 4 0 1341.64 16.87 1 4 0 1384.77 19.05 -2 -4 0 235.95 4.08 2 -4 0 239.36 2.82 -2 4 0 244.04 3.58 2 4 0 242.65 2.90 -3 -4 0 2492.43 33.77 3 -4 0 2414.74 28.52 -3 4 0 2488.76 40.23 3 4 0 2513.43 28.12 -4 -4 0 42.12 0.89 4 -4 0 39.04 0.76 -4 4 0 37.31 1.12 4 4 0 40.49 0.75 -5 -4 0 1306.57 17.80 5 -4 0 1263.21 15.96 -5 4 0 1287.13 21.32 5 4 0 1257.87 16.10 -6 -4 0 1177.23 17.22 6 -4 0 1132.25 16.36 -6 4 0 1150.78 19.55 6 4 0 1155.27 14.70 -7 -4 0 0.24 0.35 7 -4 0 0.26 0.23 -7 4 0 1.19 0.40 7 4 0 0.64 0.20 -8 -4 0 248.83 5.09 8 -4 0 250.15 4.12 -8 4 0 253.66 5.20 8 4 0 251.32 4.75 -9 -4 0 534.06 9.76 9 -4 0 527.90 8.09 -9 4 0 516.13 12.60 9 4 0 543.81 9.36 -10 -4 0 79.44 3.18 10 -4 0 75.83 1.93 -10 4 0 69.67 3.19 10 4 0 78.22 2.11 -11 -4 0 17.02 1.75 11 -4 0 14.49 1.01 -11 4 0 10.34 1.52 11 4 0 14.60 0.86 0 -5 0 0.34 0.10 0 5 0 0.35 0.12 -1 -5 0 136.28 2.05 1 -5 0 136.65 1.92 -1 5 0 136.92 1.92 1 5 0 137.56 2.16 -2 -5 0 2032.60 31.92 2 -5 0 2040.56 20.62 -2 5 0 2015.21 28.19 2 5 0 2006.08 25.38 -3 -5 0 248.56 3.81 3 -5 0 247.19 2.98 -3 5 0 255.04 3.79 3 5 0 253.65 3.13 -4 -5 0 117.08 1.99 4 -5 0 113.18 1.75 -4 5 0 117.07 2.42 4 5 0 117.84 1.57 -5 -5 0 146.95 2.93 5 -5 0 143.09 2.17 -5 5 0 146.19 3.03 5 5 0 149.34 2.17 -6 -5 0 578.44 9.79 6 -5 0 569.79 8.50 -6 5 0 580.20 10.22 6 5 0 583.92 7.60 -7 -5 0 698.44 12.34 7 -5 0 707.48 10.34 -7 5 0 712.41 12.45 7 5 0 704.47 9.23 -8 -5 0 4.32 0.65 8 -5 0 4.60 0.45 -8 5 0 3.71 0.83 8 5 0 4.89 0.39 -9 -5 0 107.73 2.81 9 -5 0 100.74 2.13 -9 5 0 99.04 3.70 9 5 0 103.25 3.07 -10 -5 0 141.58 3.55 10 -5 0 142.74 2.79 -10 5 0 135.18 4.77 10 5 0 145.68 4.04 -11 -5 0 137.66 4.80 11 -5 0 133.80 3.25 -11 5 0 133.98 4.88 11 5 0 139.63 4.07 0 -6 0 1563.75 17.18 0 6 0 1551.07 21.92 -1 -6 0 41.83 0.76 1 -6 0 42.68 0.69 -1 6 0 41.81 0.91 1 6 0 42.72 0.96 -2 -6 0 2394.92 32.40 2 -6 0 2425.48 24.41 -2 6 0 2397.83 29.75 2 6 0 2361.83 33.58 -3 -6 0 103.30 1.82 3 -6 0 100.03 1.41 -3 6 0 100.15 1.78 3 6 0 102.77 1.57 -4 -6 0 388.08 5.92 4 -6 0 372.86 5.05 -4 6 0 381.37 6.79 4 6 0 382.15 4.27 -5 -6 0 37.39 1.18 5 -6 0 35.88 0.81 -5 6 0 38.49 1.16 5 6 0 37.47 0.85 -6 -6 0 692.84 11.47 6 -6 0 666.74 9.91 -6 6 0 678.31 11.84 6 6 0 680.46 9.95 -7 -6 0 1939.58 38.26 7 -6 0 1935.50 27.19 -7 6 0 1907.65 40.04 7 6 0 1935.98 27.35 -8 -6 0 61.81 1.99 8 -6 0 61.34 1.49 -8 6 0 56.52 2.55 8 6 0 62.26 1.44 -9 -6 0 783.11 13.91 9 -6 0 781.98 11.62 -9 6 0 763.03 17.65 9 6 0 796.17 13.64 -10 -6 0 769.55 13.53 10 -6 0 735.47 11.18 -10 6 0 727.32 17.18 10 6 0 743.39 15.86 -11 -6 0 81.40 3.50 11 -6 0 78.29 2.30 -11 6 0 78.78 3.57 11 6 0 81.50 2.88 0 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710.45 10.30 -6 5 -2 682.66 12.31 6 -5 2 680.65 9.03 6 5 2 696.95 10.17 -7 -5 -2 391.26 6.31 -7 5 -2 381.64 7.57 7 -5 2 383.24 6.04 7 5 2 395.98 6.06 -8 -5 -2 47.44 1.73 -8 5 -2 43.84 2.20 8 -5 2 45.27 1.26 8 5 2 47.72 1.51 -9 -5 -2 10.12 1.34 -9 5 -2 6.95 1.19 9 -5 2 8.94 0.66 9 5 2 10.22 1.00 -10 -5 -2 60.80 2.39 -10 5 -2 61.86 2.45 10 -5 2 61.16 1.67 10 5 2 62.94 2.37 11 -6 -2 357.21 6.97 11 6 -2 359.97 8.55 -11 -6 2 360.62 7.37 -11 6 2 347.11 9.46 10 -6 -2 484.57 7.65 10 6 -2 482.98 10.88 -10 -6 2 490.08 7.48 -10 6 2 478.23 11.85 9 -6 -2 36.30 1.17 9 6 -2 36.68 1.33 -9 -6 2 35.34 1.56 -9 6 2 36.08 2.06 8 -6 -2 922.67 13.40 8 6 -2 928.01 13.52 -8 -6 2 910.35 15.90 -8 6 2 905.31 16.08 7 -6 -2 250.00 4.18 7 6 -2 260.68 4.24 -7 -6 2 251.88 5.14 -7 6 2 254.68 5.16 6 -6 -2 367.24 4.87 6 6 -2 371.01 5.09 -6 -6 2 368.25 6.54 -6 6 2 366.14 5.75 5 -6 -2 619.09 7.14 5 6 -2 615.20 8.11 -5 -6 2 610.40 10.37 -5 6 2 620.15 9.12 4 -6 -2 373.94 4.47 4 6 -2 378.10 5.08 -4 -6 2 372.42 6.54 -4 6 2 377.07 5.77 3 -6 -2 363.46 5.57 3 6 -2 356.76 5.42 -3 -6 2 356.83 6.21 -3 6 2 358.20 5.39 2 -6 -2 67.74 1.37 2 6 -2 67.95 1.38 -2 -6 2 68.33 1.29 -2 6 2 66.92 1.29 1 -6 -2 298.38 5.45 1 6 -2 317.98 5.47 -1 -6 2 321.73 5.30 -1 6 2 312.83 5.24 0 -6 -2 540.84 9.20 0 6 -2 546.35 8.04 0 -6 2 548.52 7.78 0 6 2 544.95 7.88 -1 -6 -2 466.48 12.25 -1 6 -2 482.55 8.24 1 -6 2 478.49 5.49 1 6 2 473.20 6.94 -2 -6 -2 0.51 0.20 -2 6 -2 0.99 0.29 2 -6 2 0.45 0.12 2 6 2 0.76 0.18 -3 -6 -2 286.90 4.57 -3 6 -2 297.38 5.48 3 -6 2 290.68 4.52 3 6 2 299.31 4.05 -4 -6 -2 1.61 0.32 -4 6 -2 1.65 0.40 4 -6 2 1.63 0.27 4 6 2 2.58 0.20 -5 -6 -2 472.94 6.46 -5 6 -2 462.52 8.60 5 -6 2 470.61 6.30 5 6 2 471.28 6.29 -6 -6 -2 2280.64 36.13 -6 6 -2 2236.67 37.21 6 -6 2 2209.89 28.03 6 6 2 2256.48 31.74 -7 -6 -2 1.73 0.49 -7 6 -2 3.84 0.67 7 -6 2 2.28 0.38 7 6 2 2.10 0.42 -8 -6 -2 347.91 6.89 -8 6 -2 339.90 7.06 8 -6 2 341.14 5.56 8 6 2 346.99 6.47 -9 -6 -2 870.26 15.27 -9 6 -2 850.31 15.58 9 -6 2 839.79 12.67 9 6 2 869.82 17.81 -10 -6 -2 43.05 2.66 -10 6 -2 47.19 2.20 10 -6 2 46.75 1.42 10 6 2 43.86 2.86 11 -7 -2 121.14 3.11 11 7 -2 123.67 3.03 -11 -7 2 120.05 3.41 -11 7 2 113.77 6.25 10 -7 -2 178.06 3.42 10 7 -2 179.44 3.89 -10 -7 2 178.43 4.33 -10 7 2 174.12 5.53 9 -7 -2 77.84 1.85 9 7 -2 77.61 1.85 -9 -7 2 76.00 2.38 -9 7 2 74.25 2.34 8 -7 -2 83.03 1.85 8 7 -2 79.87 1.83 -8 -7 2 76.56 2.34 -8 7 2 81.34 2.39 7 -7 -2 182.53 3.24 7 7 -2 181.11 3.25 -7 -7 2 181.38 4.76 -7 7 2 188.87 4.03 6 -7 -2 12.97 0.54 6 7 -2 14.33 0.69 -6 -7 2 13.94 0.81 -6 7 2 14.04 0.90 5 -7 -2 762.90 8.76 5 7 -2 763.07 11.17 -5 -7 2 752.69 12.74 -5 7 2 768.23 11.16 4 -7 -2 617.34 7.08 4 7 -2 602.62 9.02 -4 -7 2 594.91 10.30 -4 7 2 622.56 8.99 3 -7 -2 2933.82 35.30 3 7 -2 2864.36 40.94 -3 -7 2 2931.77 40.16 -3 7 2 2953.83 40.78 2 -7 -2 105.94 2.24 2 7 -2 104.98 2.09 -2 -7 2 107.87 2.02 -2 7 2 104.33 1.87 1 -7 -2 207.96 3.87 1 7 -2 207.25 3.93 -1 -7 2 209.70 3.76 -1 7 2 206.85 3.28 0 -7 -2 3317.78 53.81 0 7 -2 3292.23 46.07 0 -7 2 3275.91 45.06 0 7 2 3275.77 45.75 -1 -7 -2 188.30 3.57 -1 7 -2 187.30 3.18 1 -7 2 189.00 2.64 1 7 2 189.02 3.03 -2 -7 -2 7.63 0.55 -2 7 -2 6.21 0.54 2 -7 2 7.14 0.29 2 7 2 7.43 0.43 -3 -7 -2 3.12 0.44 -3 7 -2 3.08 0.45 3 -7 2 3.21 0.33 3 7 2 2.93 0.32 -4 -7 -2 816.27 13.53 -4 7 -2 809.11 13.94 4 -7 2 802.81 11.69 4 7 2 808.64 11.74 -5 -7 -2 17.27 0.88 -5 7 -2 17.00 1.02 5 -7 2 17.70 0.69 5 7 2 17.22 0.80 -6 -7 -2 130.84 3.00 -6 7 -2 126.94 3.15 6 -7 2 122.05 2.10 6 7 2 125.78 2.81 -7 -7 -2 423.55 7.70 -7 7 -2 412.00 8.10 7 -7 2 411.58 6.52 7 7 2 419.59 9.46 -8 -7 -2 30.08 1.53 -8 7 -2 30.91 1.65 8 -7 2 26.39 1.00 8 7 2 26.87 1.46 -9 -7 -2 88.06 2.73 -9 7 -2 84.04 2.83 9 -7 2 83.68 2.00 9 7 2 90.10 3.04 -10 -7 -2 0.76 0.84 -10 7 -2 0.81 0.71 10 -7 2 1.10 0.43 10 7 2 0.29 0.78 10 -8 -2 721.86 12.80 10 8 -2 714.72 12.57 -10 -8 2 730.17 13.29 -10 8 2 698.72 23.99 9 -8 -2 182.38 3.39 9 8 -2 179.52 3.38 -9 -8 2 179.53 4.28 -9 8 2 169.53 5.36 8 -8 -2 490.15 7.58 8 8 -2 489.85 7.62 -8 -8 2 486.50 9.19 -8 8 2 472.10 11.47 7 -8 -2 586.75 8.86 7 8 -2 584.44 8.92 -7 -8 2 574.64 12.67 -7 8 2 597.79 10.66 6 -8 -2 49.81 1.05 6 8 -2 48.92 1.27 -6 -8 2 52.88 1.55 -6 8 2 48.39 1.58 5 -8 -2 513.96 6.51 5 8 -2 496.48 7.66 -5 -8 2 502.82 8.83 -5 8 2 512.77 7.66 4 -8 -2 665.93 9.42 4 8 -2 676.51 9.92 -4 -8 2 668.33 11.34 -4 8 2 673.17 9.86 3 -8 -2 38.58 0.96 3 8 -2 40.63 1.22 -3 -8 2 39.79 1.22 -3 8 2 39.42 0.99 2 -8 -2 65.15 1.60 2 8 -2 62.57 1.61 -2 -8 2 65.09 1.34 -2 8 2 63.58 1.33 1 -8 -2 5623.15 89.27 1 8 -2 5606.87 90.69 -1 -8 2 5611.35 76.85 -1 8 2 5626.26 77.93 0 -8 -2 65.10 2.14 0 8 -2 66.90 1.45 0 -8 2 67.23 1.36 0 8 2 70.82 1.49 -1 -8 -2 1390.32 28.06 -1 8 -2 1382.78 20.06 1 -8 2 1422.16 17.48 1 8 2 1403.77 19.85 -2 -8 -2 1264.69 25.25 -2 8 -2 1262.71 20.94 2 -8 2 1248.09 13.98 2 8 2 1250.25 17.83 -3 -8 -2 46.03 1.47 -3 8 -2 48.58 1.49 3 -8 2 47.80 1.16 3 8 2 49.00 1.15 -4 -8 -2 348.61 6.28 -4 8 -2 335.56 6.47 4 -8 2 339.17 5.32 4 8 2 340.72 5.34 -5 -8 -2 1556.04 25.68 -5 8 -2 1566.46 26.29 5 -8 2 1556.83 22.20 5 8 2 1582.27 22.38 -6 -8 -2 82.86 2.31 -6 8 -2 84.42 2.42 6 -8 2 81.90 1.80 6 8 2 86.23 2.59 -7 -8 -2 89.50 2.45 -7 8 -2 88.76 2.62 7 -8 2 87.40 1.95 7 8 2 87.58 2.82 -8 -8 -2 113.82 3.77 -8 8 -2 119.89 3.32 8 -8 2 116.59 2.49 8 8 2 121.64 3.63 -9 -8 -2 10.30 1.11 -9 8 -2 8.11 1.06 9 -8 2 9.37 0.74 9 8 2 11.37 1.16 10 -9 -2 313.52 7.64 10 9 -2 309.78 6.22 -10 -9 2 308.08 6.63 -10 9 2 290.77 11.89 9 -9 -2 353.62 8.28 9 9 -2 348.24 5.80 -9 -9 2 347.25 7.17 -9 9 2 325.72 12.79 8 -9 -2 21.96 1.34 8 9 -2 22.76 0.96 -8 -9 2 22.34 1.67 -8 9 2 25.05 2.71 7 -9 -2 1415.91 28.52 7 9 -2 1405.56 20.24 -7 -9 2 1403.16 28.42 -7 9 2 1343.83 42.60 6 -9 -2 207.02 3.78 6 9 -2 202.12 3.54 -6 -9 2 202.09 4.17 -6 9 2 204.47 4.28 5 -9 -2 76.75 1.55 5 9 -2 74.45 1.66 -5 -9 2 77.47 2.03 -5 9 2 75.86 2.48 4 -9 -2 282.21 4.31 4 9 -2 280.61 5.28 -4 -9 2 275.02 5.29 -4 9 2 284.67 4.51 3 -9 -2 157.67 2.62 3 9 -2 154.84 3.23 -3 -9 2 157.99 3.26 -3 9 2 157.50 2.73 2 -9 -2 1954.27 26.46 2 9 -2 1975.69 32.20 -2 -9 2 1963.54 27.25 -2 9 2 1958.60 27.62 1 -9 -2 279.93 6.53 1 9 -2 284.84 5.31 -1 -9 2 289.58 4.46 -1 9 2 285.39 4.49 0 -9 -2 325.24 7.33 0 9 -2 326.06 5.98 0 -9 2 330.29 4.99 0 9 2 322.89 5.05 -1 -9 -2 909.82 18.57 -1 9 -2 913.98 13.26 1 -9 2 906.27 12.79 1 9 2 895.91 13.06 -2 -9 -2 36.56 1.29 -2 9 -2 35.55 1.25 2 -9 2 37.37 1.00 2 9 2 37.24 0.99 -3 -9 -2 13.11 0.88 -3 9 -2 13.92 0.86 3 -9 2 13.92 0.67 3 9 2 12.90 0.64 -4 -9 -2 2007.34 31.77 -4 9 -2 1968.25 32.72 4 -9 2 1972.97 27.77 4 9 2 1941.21 32.66 -5 -9 -2 1.63 0.51 -5 9 -2 2.79 0.56 5 -9 2 1.98 0.36 5 9 2 2.60 0.32 -6 -9 -2 80.95 2.31 -6 9 -2 76.38 2.33 6 -9 2 78.24 2.08 6 9 2 77.07 2.09 -7 -9 -2 1926.01 31.35 -7 9 -2 1906.39 32.25 7 -9 2 1885.75 31.51 7 9 2 1942.53 39.41 -8 -9 -2 314.35 7.81 -8 9 -2 307.60 6.59 8 -9 2 306.08 6.06 8 9 2 307.71 7.56 -9 -9 -2 83.74 2.82 -9 9 -2 87.01 2.89 9 -9 2 86.49 2.43 9 9 2 83.60 3.04 9 -10 -2 16.41 1.41 9 10 -2 19.09 1.13 -9 -10 2 18.42 1.43 -9 10 2 17.57 2.39 8 -10 -2 135.33 3.90 8 10 -2 129.66 3.14 -8 -10 2 127.07 4.06 -8 10 2 124.28 6.10 7 -10 -2 116.80 3.47 7 10 -2 112.93 2.81 -7 -10 2 115.72 3.66 -7 10 2 115.74 3.55 6 -10 -2 472.15 9.19 6 10 -2 443.72 8.35 -6 -10 2 461.74 8.30 -6 10 2 449.68 15.41 5 -10 -2 224.16 4.11 5 10 -2 223.02 4.49 -5 -10 2 221.69 4.52 -5 10 2 224.00 5.60 4 -10 -2 566.23 8.13 4 10 -2 570.08 12.44 -4 -10 2 562.83 9.85 -4 10 2 564.22 9.79 3 -10 -2 258.65 4.00 3 10 -2 258.29 4.91 -3 -10 2 251.80 4.90 -3 10 2 254.38 4.82 2 -10 -2 438.13 7.43 2 10 -2 450.31 7.93 -2 -10 2 440.78 7.81 -2 10 2 444.80 7.81 1 -10 -2 941.95 15.17 1 10 -2 950.00 16.18 -1 -10 2 977.97 15.76 -1 10 2 965.26 16.02 0 -10 -2 71.10 2.35 0 10 -2 69.22 1.85 0 -10 2 72.01 1.53 0 10 2 73.99 1.55 -1 -10 -2 439.71 8.03 -1 10 -2 458.47 8.15 1 -10 2 459.02 7.79 1 10 2 456.05 6.89 -2 -10 -2 359.59 6.73 -2 10 -2 375.76 6.87 2 -10 2 378.56 5.75 2 10 2 361.47 5.74 -3 -10 -2 463.76 8.34 -3 10 -2 476.52 8.57 3 -10 2 468.62 7.14 3 10 2 466.91 7.17 -4 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1246.71 20.51 1 -11 -2 562.58 8.24 1 11 -2 576.21 12.54 -1 -11 2 580.61 8.50 -1 11 2 569.87 9.93 0 -11 -2 72.62 1.60 0 11 -2 74.89 2.47 0 -11 2 78.87 1.90 0 11 2 72.70 1.90 -1 -11 -2 1404.89 23.10 -1 11 -2 1414.21 29.33 1 -11 2 1433.70 28.33 1 11 2 1405.99 23.37 -2 -11 -2 121.83 3.05 -2 11 -2 129.51 3.67 2 -11 2 128.89 3.49 2 11 2 132.25 2.88 -3 -11 -2 491.44 8.84 -3 11 -2 514.20 11.27 3 -11 2 497.80 8.83 3 11 2 480.70 11.08 -4 -11 -2 8.75 1.06 -4 11 -2 10.29 1.07 4 -11 2 12.32 1.04 4 11 2 9.93 0.77 -5 -11 -2 10.96 1.01 -5 11 -2 13.05 1.04 5 -11 2 11.63 0.88 5 11 2 11.74 0.86 -6 -11 -2 475.21 9.00 -6 11 -2 482.09 9.15 6 -11 2 471.46 8.74 6 11 2 483.02 7.46 -7 -11 -2 44.87 1.84 -7 11 -2 46.08 1.91 7 -11 2 44.92 1.63 7 11 2 44.75 2.02 -8 -11 -2 17.72 1.77 -8 11 -2 17.57 1.68 8 -11 2 18.40 1.22 8 11 2 19.03 1.54 8 -12 -2 2.17 1.06 8 12 -2 3.90 0.68 -8 -12 2 4.07 1.08 -8 12 2 4.57 1.47 7 -12 -2 776.88 23.71 7 12 -2 769.07 13.72 -7 -12 2 792.43 16.82 -7 12 2 744.27 24.99 6 -12 -2 232.51 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