#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 15/03/2013' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; ? # name ; ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable this reference if SIR97 was used for solving of the structure #Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., #Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). #SIR97. A Package for Crystal Structure Solution by Direct Methods #and Refinement, Bari, Rome, Italy. # use this reference if SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # use this reference if SIR2011 was used for solving of the structure #Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, #G.L., Giacovazzo, C., Mallamo. M., Mazzone, A., Polidori, G., Spagna, R. #SIR2011: a new package for crystal structure determination and refinement, #J.Appl.Cryst. (2012) 45, 357-361 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Fe2 H18 Mg2 Mn2 O26 P4' _chemical_formula_weight 828.2 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/a 1' _symmetry_space_group_name_Hall '-P 2ya' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x+1/2,y,-z 3 -x,-y,-z 4 x+1/2,-y,z _cell_length_a 15.177 _cell_length_b 7.176 _cell_length_c 10.006 _cell_angle_alpha 90 _cell_angle_beta 111.01 _cell_angle_gamma 90 _cell_volume 1017.306 loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 ? ? ? ? ? ? ? ? ? ? ? _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.7037 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 3.115 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,y,-z 3 -x,-y,-z 4 x+1/2,-y,z #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator ? _diffrn_measurement_device ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 26229 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 36.03 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_max 0.73 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 2619 _reflns_number_gt 1703 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_gt 0.0382 _refine_ls_R_factor_all 0.0819 _refine_ls_wR_factor_ref 0.0408 _refine_ls_goodness_of_fit_ref 1.72 _refine_ls_goodness_of_fit_gt 2.04 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 2619 _refine_ls_number_parameters 208 _refine_ls_number_restraints 9 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'refall' _refine_ls_shift/su_max 0.0451 _refine_ls_shift/su_mean 0.0029 _refine_diff_density_max 0.62 _refine_diff_density_min -0.85 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Mg 0.0486 0.0363 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Mn 0.3368 0.7283 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param Oh 1_655 Hoh . 0.95 0.03 Ow1 . Hw1a . 0.95 0.03 Ow1 . 0hw1b . 0.95 0.03 Ow2 . Hw2a . 0.95 0.03 Ow3 1_545 0hw3a . 0.95 0.03 Ow4 . Hw4a . 0.95 0.03 Ow4 . Hw4b . 0.95 0.03 Ow3 . Hx . 0.95 0.03 Ow1 . Hy . 0.95 0.03 #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1x Mn 0.25 0.96792(13) 0 Uani 0.0251(5) 2 0.752(3) d . . . Mn2m1 Mn 0.25 0.47096(10) 0 Uani 0.0204(3) 2 1 d . . . Mg1m2 Mg 0 0 0.5 Uani 0.0210(5) 2 0.657(3) d . . . Mg2m2 Mg 0.25 0.50247(14) 0.5 Uani 0.0203(5) 2 0.638(3) d . . . Fe2m3 Fe 0 0 0 Uani 0.0161(3) 2 0.911(3) d . . . Fe3m3 Fe 0 0.5 0 Uani 0.0158(3) 2 0.927(3) d . . . P1 P 0.18375(6) 0.25857(11) 0.18949(11) Uani 0.0179(3) 4 1 d . . . P2 P 0.08308(6) 0.74765(11) 0.80000(11) Uani 0.0187(3) 4 1 d . . . O1a O 0.27184(18) 0.2209(4) 0.1498(3) Uani 0.0406(12) 4 1 d . . . O2a O 0.21084(19) 0.2991(3) 0.3470(3) Uani 0.0326(11) 4 1 d . . . O3a O 0.11932(18) 0.0894(3) 0.1481(3) Uani 0.0420(11) 4 1 d . . . O4a O 0.13872(15) 0.4305(3) 0.0914(3) Uani 0.0220(9) 4 1 d . . . O5a O 0.18926(17) 0.6906(3) 0.8555(3) Uani 0.0287(10) 4 1 d . . . O6a O 0.05200(17) 0.7841(3) 0.6403(3) Uani 0.0268(10) 4 1 d . . . O7a O 0.08063(18) 0.9270(3) 0.8855(3) Uani 0.0304(11) 4 1 d . . . O8a O 0.02288(17) 0.5922(3) 0.8282(3) Uani 0.0261(10) 4 1 d . . . Oh O 0.02584(17) 0.7504(3) 0.0961(3) Uani 0.0231(10) 4 1 d . . . Ow1 O 0.2258(2) 0.7240(4) 0.3430(3) Uani 0.0369(13) 4 1 d . . . Ow2 O 0.4489(2) 0.2152(3) 0.3427(3) Uani 0.0421(13) 4 1 d . . . Ow3 O 0.6316(2) 0.9909(4) 0.4672(4) Uani 0.0403(13) 4 1 d . . . Ow4 O 0.39346(19) 0.5136(3) 0.5170(3) Uani 0.0363(13) 4 1 d . . . Hoh H 1.009(5) 0.749(10) 0.177(5) Uiso 0.166(10) 4 1 d . . . Hw1a H 0.253(5) 0.825(7) 0.398(6) Uiso 0.166(10) 4 1 d . . . 0hw1b H 0.159(2) 0.719(11) 0.291(7) Uiso 0.166(10) 4 1 d . . . Hw2a H 0.425(5) 0.300(9) 0.395(7) Uiso 0.166(10) 4 1 d . . . Hw2b H 0.396(6) 0.257(10) 0.251(9) Uiso 0.166(10) 4 1 d . . . 0hw3a H 0.614(6) -0.004(11) 0.365(3) Uiso 0.166(10) 4 1 d . . . 0hw3b H 0.582(5) 1.022(10) 0.607(8) Uiso 0.166(10) 4 1 d . . . Hw4a H 0.418(5) 0.618(7) 0.487(8) Uiso 0.166(10) 4 1 d . . . Hw4b H 0.427(5) 0.450(9) 0.599(5) Uiso 0.166(10) 4 1 d . . . Hx H 0.666(5) 0.893(8) 0.442(8) Uiso 0.166(10) 4 1 d . . . Hy H 0.245(5) 0.706(10) 0.263(6) Uiso 0.166(10) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn1x Mn 0.0267(6) 0.0159(5) 0.0257(9) 0 0.0007(5) 0 Mn2m1 Mn 0.0238(4) 0.0183(3) 0.0206(6) 0 0.0099(4) 0 Mg1m2 Mg 0.0247(7) 0.0187(6) 0.0176(10) 0.0010(4) 0.0052(6) 0.0052(5) Mg2m2 Mg 0.0236(7) 0.0189(6) 0.0203(10) 0 0.0103(6) 0 Fe2m3 Fe 0.0190(4) 0.0108(4) 0.0189(6) -0.0001(3) 0.0072(4) 0.0003(3) Fe3m3 Fe 0.0193(4) 0.0111(3) 0.0185(6) 0.0005(2) 0.0088(4) 0.0005(3) P1 P 0.0198(4) 0.0165(4) 0.0171(6) 0.0013(3) 0.0061(4) -0.0010(4) P2 P 0.0212(4) 0.0181(4) 0.0177(7) 0.0025(3) 0.0082(4) 0.0028(4) O1a O 0.0330(15) 0.0659(19) 0.0259(19) 0.0254(14) 0.0143(14) 0.0111(15) O2a O 0.0476(17) 0.0319(14) 0.0177(18) 0.0017(12) 0.0111(14) -0.0042(12) O3a O 0.0431(17) 0.0173(12) 0.043(2) -0.0044(11) -0.0119(15) 0.0048(12) O4a O 0.0224(12) 0.0209(11) 0.0223(17) 0.0006(9) 0.0074(12) 0.0017(11) O5a O 0.0267(13) 0.0356(13) 0.0233(18) 0.0064(11) 0.0083(12) 0.0015(12) O6a O 0.0337(14) 0.0282(13) 0.0161(17) 0.0037(10) 0.0059(12) 0.0047(11) O7a O 0.0449(16) 0.0176(11) 0.036(2) -0.0025(11) 0.0240(14) -0.0036(12) O8a O 0.0365(14) 0.0192(11) 0.0283(18) -0.0030(10) 0.0187(13) 0.0010(11) Oh O 0.0293(13) 0.0153(10) 0.0254(18) -0.0008(9) 0.0106(12) -0.0041(11) Ow1 O 0.0504(18) 0.0335(15) 0.031(2) 0.0086(13) 0.0189(16) 0.0023(14) Ow2 O 0.0562(19) 0.0253(14) 0.029(2) -0.0038(13) -0.0041(16) 0.0004(13) Ow3 O 0.0414(18) 0.0346(16) 0.050(2) -0.0044(12) 0.0221(17) -0.0097(15) Ow4 O 0.0305(14) 0.0338(15) 0.045(2) -0.0021(11) 0.0141(15) 0.0021(14) loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_D_label _jana_atom_site_ADP_D_type_symbol _jana_atom_site_ADP_D_1111 _jana_atom_site_ADP_D_1112 _jana_atom_site_ADP_D_1113 _jana_atom_site_ADP_D_1122 _jana_atom_site_ADP_D_1123 _jana_atom_site_ADP_D_1133 _jana_atom_site_ADP_D_1222 _jana_atom_site_ADP_D_1223 _jana_atom_site_ADP_D_1233 _jana_atom_site_ADP_D_1333 _jana_atom_site_ADP_D_2222 _jana_atom_site_ADP_D_2223 _jana_atom_site_ADP_D_2233 _jana_atom_site_ADP_D_2333 _jana_atom_site_ADP_D_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_E_label _jana_atom_site_ADP_E_type_symbol _jana_atom_site_ADP_E_11111 _jana_atom_site_ADP_E_11112 _jana_atom_site_ADP_E_11113 _jana_atom_site_ADP_E_11122 _jana_atom_site_ADP_E_11123 _jana_atom_site_ADP_E_11133 _jana_atom_site_ADP_E_11222 _jana_atom_site_ADP_E_11223 _jana_atom_site_ADP_E_11233 _jana_atom_site_ADP_E_11333 _jana_atom_site_ADP_E_12222 _jana_atom_site_ADP_E_12223 _jana_atom_site_ADP_E_12233 _jana_atom_site_ADP_E_12333 _jana_atom_site_ADP_E_13333 _jana_atom_site_ADP_E_22222 _jana_atom_site_ADP_E_22223 _jana_atom_site_ADP_E_22233 _jana_atom_site_ADP_E_22333 _jana_atom_site_ADP_E_23333 _jana_atom_site_ADP_E_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_F_label _jana_atom_site_ADP_F_type_symbol _jana_atom_site_ADP_F_111111 _jana_atom_site_ADP_F_111112 _jana_atom_site_ADP_F_111113 _jana_atom_site_ADP_F_111122 _jana_atom_site_ADP_F_111123 _jana_atom_site_ADP_F_111133 _jana_atom_site_ADP_F_111222 _jana_atom_site_ADP_F_111223 _jana_atom_site_ADP_F_111233 _jana_atom_site_ADP_F_111333 _jana_atom_site_ADP_F_112222 _jana_atom_site_ADP_F_112223 _jana_atom_site_ADP_F_112233 _jana_atom_site_ADP_F_112333 _jana_atom_site_ADP_F_113333 _jana_atom_site_ADP_F_122222 _jana_atom_site_ADP_F_122223 _jana_atom_site_ADP_F_122233 _jana_atom_site_ADP_F_122333 _jana_atom_site_ADP_F_123333 _jana_atom_site_ADP_F_133333 _jana_atom_site_ADP_F_222222 _jana_atom_site_ADP_F_222223 _jana_atom_site_ADP_F_222233 _jana_atom_site_ADP_F_222333 _jana_atom_site_ADP_F_223333 _jana_atom_site_ADP_F_233333 _jana_atom_site_ADP_F_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Xmn P1 . 1_565 3.2129(12) ? Xmn P1 . 2_565 3.2129(12) ? Xmn P2 . 1_554 3.0471(9) ? Xmn P2 . 2_556 3.0471(9) ? Xmn O1a . 1_565 2.302(3) ? Xmn O1a . 2_565 2.302(3) ? Xmn O3a . 1_565 3.000(3) ? Xmn O3a . 2_565 3.000(3) ? Xmn O5a . 1_554 2.439(3) ? Xmn O5a . 2_556 2.439(3) ? Xmn O7a . 1_554 2.428(2) ? Xmn O7a . 2_556 2.428(2) ? Xmn Hy . . 3.24(7) ? Xmn Hy . 2_555 3.24(7) ? Fe1m1 P1 . . 2.8802(12) ? Fe1m1 P1 . 2_555 2.8802(12) ? Fe1m1 P2 . 1_554 3.2754(9) ? Fe1m1 P2 . 2_556 3.2754(9) ? Fe1m1 O1a . . 2.284(3) ? Fe1m1 O1a . 2_555 2.284(3) ? Fe1m1 O4a . . 2.210(3) ? Fe1m1 O4a . 2_555 2.210(3) ? Fe1m1 O5a . 1_554 2.114(2) ? Fe1m1 O5a . 2_556 2.114(2) ? Fe1m1 O8a . 1_554 3.368(2) ? Fe1m1 O8a . 2_556 3.368(2) ? Fe1m1 Hw2b . . 3.11(7) ? Fe1m1 Hw2b . 2_555 3.11(7) ? Fe1m1 Hy . . 3.15(7) ? Fe1m1 Hy . 2_555 3.15(7) ? Mg1m2 P2 . 1_545 3.3418(10) ? Mg1m2 P2 . 3_566 3.3418(10) ? Mg1m2 O6a . 1_545 2.049(2) ? Mg1m2 O6a . 3_566 2.049(2) ? Mg1m2 Ow2 . 2_556 2.143(3) ? Mg1m2 Ow2 . 4_455 2.143(3) ? Mg1m2 Ow3 . 2_546 2.139(3) ? Mg1m2 Ow3 . 4_465 2.139(3) ? Mg1m2 Hw2a . 2_556 2.51(6) ? Mg1m2 Hw2a . 4_455 2.51(6) ? Mg1m2 Hw2b . 2_556 3.04(7) ? Mg1m2 Hw2b . 4_455 3.04(7) ? Mg1m2 0hw3a . 2_556 2.6147 ? Mg1m2 0hw3a . 4_455 2.6147 ? Mg1m2 0hw3b . 2_546 1.31(7) ? Mg1m2 0hw3b . 4_465 1.31(7) ? Mg1m2 Hw4a . 2_546 2.99(6) ? Mg1m2 Hw4a . 4_465 2.99(6) ? Mg1m2 Hx . 2_546 2.84(8) ? Mg1m2 Hx . 4_465 2.84(8) ? Mg2m2 P1 . . 3.3891(11) ? Mg2m2 P1 . 2_556 3.3891(11) ? Mg2m2 O2a . . 2.043(3) ? Mg2m2 O2a . 2_556 2.043(3) ? Mg2m2 Ow1 . . 2.171(3) ? Mg2m2 Ow1 . 2_556 2.171(3) ? Mg2m2 Ow4 . . 2.124(3) ? Mg2m2 Ow4 . 2_556 2.124(3) ? Mg2m2 Hw1a . . 2.51(5) ? Mg2m2 Hw1a . 2_556 2.51(5) ? Mg2m2 0hw1b . . 2.58(7) ? Mg2m2 0hw1b . 2_556 2.58(7) ? Mg2m2 Hw4a . . 2.73(8) ? Mg2m2 Hw4a . 2_556 2.73(8) ? Mg2m2 Hw4b . . 2.53(7) ? Mg2m2 Hw4b . 2_556 2.53(7) ? Mg2m2 Hx . 3_666 3.10(5) ? Mg2m2 Hx . 4_465 3.10(5) ? Mg2m2 Hy . . 2.78(7) ? Mg2m2 Hy . 2_556 2.78(7) ? Fe2m3 P1 . . 3.3204(8) ? Fe2m3 P1 . 3_555 3.3204(8) ? Fe2m3 P2 . 1_544 3.2685(11) ? Fe2m3 P2 . 3_566 3.2685(11) ? Fe2m3 O3a . . 1.990(2) ? Fe2m3 O3a . 3_555 1.990(2) ? Fe2m3 O7a . 1_544 2.022(3) ? Fe2m3 O7a . 3_566 2.022(3) ? Fe2m3 Oh . 1_545 2.004(2) ? Fe2m3 Oh . 3_565 2.004(2) ? Fe2m3 Hoh . 1_445 2.48(7) ? Fe2m3 Hoh . 3_665 2.48(7) ? Fe3m3 P1 . 2_555 3.2532(8) ? Fe3m3 P1 . 4_565 3.2532(8) ? Fe3m3 P2 . 2_556 3.2499(11) ? Fe3m3 P2 . 4_564 3.2499(11) ? Fe3m3 O4a . 2_555 2.034(2) ? Fe3m3 O4a . 4_565 2.034(2) ? Fe3m3 O8a . 2_556 1.986(3) ? Fe3m3 O8a . 4_564 1.986(3) ? Fe3m3 Oh . 2_555 2.009(2) ? Fe3m3 Oh . 4_565 2.009(2) ? Fe3m3 Hoh . 2_655 2.47(7) ? Fe3m3 Hoh . 4_465 2.47(7) ? P1 O1a . . 1.549(3) ? P1 O2a . . 1.507(3) ? P1 O3a . . 1.520(2) ? P1 O4a . . 1.572(2) ? P1 O8a . 3_566 3.259(3) ? P1 Hw2b . . 3.08(8) ? P1 0hw3a . 4_455 3.2179(10) ? P1 Hx . 4_465 2.80(8) ? P1 Hy . . 3.36(7) ? P2 O5a . . 1.559(3) ? P2 O6a . . 1.519(3) ? P2 O7a . . 1.553(3) ? P2 O8a . . 1.530(3) ? P2 Oh . 1_556 3.373(3) ? P2 0hw3b . 4_475 2.52(8) ? P2 Hw4a . 2_556 3.01(8) ? P2 Hw4b . 4_465 2.88(6) ? P2 Hy . 2_556 2.93(9) ? O1a O1a . 2_555 2.829(4) ? O1a O2a . . 2.524(5) ? O1a O3a . . 2.495(4) ? O1a O4a . . 2.416(3) ? O1a O7a . 2_546 3.187(4) ? O1a Ow2 . . 2.687(4) ? O1a Hw2a . . 2.71(6) ? O1a Hw2b . . 1.83(7) ? O1a 0hw3b . 3_666 3.18(7) ? O2a O2a . 2_556 2.861(4) ? O2a O3a . . 2.484(3) ? O2a O4a . . 2.572(4) ? O2a Ow1 . . 3.058(4) ? O2a Ow3 . 3_666 3.210(3) ? O2a Ow3 . 4_465 2.872(4) ? O2a Ow4 . . 3.092(4) ? O2a Ow4 . 2_556 2.877(5) ? O2a 0hw1b . . 3.10(7) ? O2a Hw2a . . 3.06(8) ? O2a Hw2b . . 3.31(10) ? O2a 0hw3a . 4_455 2.908(3) ? O2a Hw4b . 2_556 2.58(7) ? O2a Hx . 3_666 2.74(6) ? O2a Hx . 4_465 1.92(7) ? O2a Hy . . 3.14(8) ? O3a O4a . . 2.552(3) ? O3a O7a . 1_544 2.738(4) ? O3a O7a . 3_566 2.933(4) ? O3a O8a . 3_566 3.209(4) ? O3a Oh . 1_545 2.771(3) ? O3a Oh . 3_565 2.878(3) ? O3a Ow1 . 1_545 3.322(4) ? O3a Ow3 . 4_465 3.183(5) ? O3a Hoh . 1_445 3.05(8) ? O3a Hoh . 3_665 3.30(5) ? O3a Hw1a . 1_545 3.26(5) ? O3a 0hw1b . 1_545 2.98(7) ? O3a 0hw3a . 4_455 2.433(3) ? O3a Hx . 4_465 2.70(7) ? O3a Hy . 1_545 3.28(7) ? O4a O5a . 1_554 3.308(4) ? O4a O5a . 2_556 3.097(3) ? O4a O8a . 1_554 2.839(3) ? O4a O8a . 3_566 2.847(4) ? O4a Oh . . 2.875(3) ? O4a Oh . 3_565 2.843(3) ? O4a Ow1 . . 3.184(4) ? O4a Hoh . 1_455 3.34(8) ? O4a Hoh . 3_665 3.05(6) ? O4a 0hw1b . . 2.78(7) ? O4a Hy . . 2.73(7) ? O5a O5a . 2_557 2.818(3) ? O5a O6a . . 2.493(3) ? O5a O7a . . 2.458(4) ? O5a O8a . . 2.540(4) ? O5a Ow1 . 2_556 2.739(5) ? O5a Hw1a . 2_556 3.12(7) ? O5a 0hw1b . 2_556 3.13(6) ? O5a Hw2b . 2_556 3.39(7) ? O5a 0hw3b . 4_475 3.19(7) ? O5a Hw4a . 2_556 3.27(7) ? O5a Hy . 2_556 1.82(8) ? O6a O7a . . 2.550(4) ? O6a O8a . . 2.494(4) ? O6a Ow1 . 2_556 3.345(4) ? O6a Ow2 . 2_566 3.099(3) ? O6a Ow2 . 4_465 2.824(4) ? O6a Ow3 . 2_556 2.994(4) ? O6a Ow3 . 4_475 2.929(5) ? O6a Ow4 . 2_556 2.804(4) ? O6a Ow4 . 4_465 3.121(3) ? O6a Hw1a . 2_556 3.11(8) ? O6a Hw2a . 4_465 2.64(6) ? O6a 0hw3a . 2_566 3.205(3) ? O6a 0hw3b . 2_556 3.09(7) ? O6a 0hw3b . 4_475 1.52(8) ? O6a Hw4a . 2_556 1.91(7) ? O6a Hw4b . 4_465 2.46(7) ? O6a Hx . 2_556 3.10(7) ? O6a Hy . 2_556 2.96(8) ? O7a O8a . . 2.551(3) ? O7a Oh . 1_556 2.827(4) ? O7a Oh . 3_576 2.867(3) ? O7a Ow2 . 2_566 2.993(4) ? O7a Hoh . 3_676 2.63(7) ? O7a Hw2b . 2_566 2.82(8) ? O7a 0hw3a . 2_566 3.318(2) ? O7a 0hw3b . 4_475 2.81(9) ? O8a Oh . 1_556 2.897(4) ? O8a Oh . 3_566 2.751(3) ? O8a Ow2 . 2_556 3.309(4) ? O8a Ow4 . 4_465 3.121(4) ? O8a Hoh . 3_666 2.48(7) ? O8a Hw2a . 2_556 3.36(8) ? O8a Hw2b . 2_556 2.92(8) ? O8a Hw4b . 4_465 2.26(5) ? Oh Ow1 . . 3.158(3) ? Oh Ow2 . 4_465 3.096(5) ? Oh Hoh . 1_455 0.93(7) ? Oh 0hw1b . . 2.25(5) ? Oh Hw2b . 4_465 2.90(10) ? Oh 0hw3a . 4_465 2.966(2) ? Oh Hy . . 3.13(7) ? Ow1 Ow1 . 2_556 2.959(5) ? Ow1 Ow3 . 3_676 3.089(4) ? Ow1 Ow3 . 4_475 3.009(5) ? Ow1 Ow4 . . 2.935(4) ? Ow1 Ow4 . 2_556 3.055(5) ? Ow1 Hoh . 1_455 3.16(7) ? Ow1 Hw1a . . 0.92(5) ? Ow1 Hw1a . 2_556 2.57(6) ? Ow1 0hw1b . . 0.96(3) ? Ow1 0hw3a . 3_666 3.397(3) ? Ow1 0hw3a . 4_465 2.365(3) ? Ow1 0hw3b . 3_676 3.34(8) ? Ow1 Hw4a . . 2.86(6) ? Ow1 Hw4a . 2_556 3.31(8) ? Ow1 Hw4b . 2_556 3.24(7) ? Ow1 Hx . 4_475 3.19(6) ? Ow1 Hy . . 0.95(7) ? Ow2 Ow3 . 1_545 3.062(4) ? Ow2 Ow3 . 3_666 2.992(5) ? Ow2 Ow4 . . 3.063(5) ? Ow2 Ow4 . 3_666 3.013(4) ? Ow2 Hoh . 4_465 2.18(8) ? Ow2 Hw2a . . 0.96(8) ? Ow2 Hw2b . . 1.01(7) ? Ow2 0hw3a . . 2.779(3) ? Ow2 0hw3b . 1_545 3.01(7) ? Ow2 0hw3b . 3_666 1.88(8) ? Ow2 Hw4a . . 3.33(6) ? Ow2 Hw4a . 3_666 2.44(6) ? Ow2 Hw4b . . 3.19(6) ? Ow2 Hw4b . 3_666 2.97(7) ? Ow2 Hx . 3_666 3.30(8) ? Ow3 Hw1a . 3_676 2.20(6) ? Ow3 Hw1a . 4_575 2.58(7) ? Ow3 0hw1b . 4_575 2.89(8) ? Ow3 Hw2a . 3_666 2.79(8) ? Ow3 0hw3a . 1_565 1.018(4) ? Ow3 0hw3b . . 1.85(9) ? Ow3 0hw3b . 3_676 3.03(8) ? Ow3 Hw4a . 3_676 2.99(6) ? Ow3 Hw4b . 3_666 3.29(7) ? Ow3 Hx . . 0.96(7) ? Ow3 Hx . 2_656 3.06(7) ? Ow4 Ow4 . 3_666 3.376(5) ? Ow4 Hoh . 2_656 3.38(6) ? Ow4 Hw1a . . 2.98(6) ? Ow4 0hw1b . 2_556 2.77(7) ? Ow4 Hw2a . . 2.12(8) ? Ow4 Hw2a . 3_666 2.95(7) ? Ow4 Hw2b . . 3.24(9) ? Ow4 0hw3a . 3_666 3.361(3) ? Ow4 Hw4a . . 0.93(7) ? Ow4 Hw4a . 3_666 3.02(8) ? Ow4 Hw4b . . 0.91(5) ? Ow4 Hw4b . 3_666 3.33(8) ? Ow4 Hx . 3_666 3.09(6) ? Ow4 Hy . . 3.09(6) ? Hoh 0hw1b . 1_655 2.21(8) ? Hoh Hw2a . 4_565 2.92(12) ? Hoh Hw2b . 4_565 2.06(13) ? Hoh 0hw3a . 4_565 2.55(6) ? Hoh Hw4a . 2_656 3.31(9) ? Hoh Hw4b . 2_656 3.02(9) ? Hw1a Hw1a . 2_556 2.04(10) ? Hw1a 0hw1b . . 1.68(7) ? Hw1a 0hw1b . 2_556 3.00(9) ? Hw1a 0hw3a . 3_666 2.56(5) ? Hw1a 0hw3a . 4_465 2.17(7) ? Hw1a 0hw3b . 3_676 2.76(11) ? Hw1a Hw4a . . 2.74(9) ? Hw1a Hx . 3_676 2.68(8) ? Hw1a Hx . 4_475 2.62(9) ? Hw1a Hy . . 1.58(9) ? 0hw1b 0hw3a . 4_465 2.04(7) ? 0hw1b Hw4a . 2_556 2.98(11) ? 0hw1b Hw4b . 2_556 2.77(10) ? 0hw1b Hx . 4_475 3.18(10) ? 0hw1b Hy . . 1.39(10) ? Hw2a Hw2b . . 1.34(11) ? Hw2a 0hw3b . 1_545 3.26(9) ? Hw2a 0hw3b . 3_666 2.31(10) ? Hw2a Hw4a . . 2.48(9) ? Hw2a Hw4a . 3_666 2.38(9) ? Hw2a Hw4b . . 2.32(10) ? Hw2a Hw4b . 3_666 2.90(10) ? Hw2a Hx . 3_666 2.81(11) ? Hw2b 0hw3b . 3_666 2.41(11) ? Hw2b Hw4a . 3_666 3.19(9) ? Hw2b Hw4b . 3_666 3.29(10) ? 0hw3a 0hw3b . 1_545 2.66(9) ? 0hw3a 0hw3b . 3_666 3.17(9) ? 0hw3a Hw4a . 3_666 2.95(7) ? 0hw3a Hx . 1_545 1.34(5) ? 0hw3a Hy . 4_565 3.02(8) ? 0hw3b 0hw3b . 3_676 2.62(9) ? 0hw3b Hw4a . 3_676 2.75(9) ? 0hw3b Hx . . 2.62(12) ? 0hw3b Hy . 3_676 3.18(10) ? Hw4a Hw4a . 3_666 2.93(10) ? Hw4a Hw4b . . 1.61(9) ? Hw4a Hw4b . 3_666 2.82(11) ? Hw4a Hy . . 2.88(9) ? Hw4b Hx . 3_666 2.73(9) ? Hx Hx . 2_656 2.62(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag Oh Hoh Ow2 1_655 . 4_565 0.93(7) 2.18(8) 3.096(5) 171(6) ? Ow1 Hw1a Ow3 . . 3_676 0.92(5) 2.20(6) 3.089(4) 160(6) ? Ow1 0hw1b Oh . . . 0.96(3) 2.25(5) 3.158(3) 157(6) ? Ow2 Hw2a Ow4 . . . 0.96(8) 2.12(8) 3.063(5) 166(6) ? Ow2 Hw2b O1a . . . 1.01(7) 1.83(7) 2.687(4) 141(7) ? Ow3 0hw3a O3a 1_545 . 4_555 1.018(4) 2.433(3) 3.183(5) 129.96(17) ? Ow3 0hw3a Oh 1_545 . 4_565 1.018(4) 2.966(2) 3.943(4) 161.17(18) ? Ow3 0hw3a Ow1 1_545 . 4_565 1.018(4) 2.365(3) 3.009(5) 120.29(16) ? Mg1m2 0hw3b P2 2_566 . 4_575 1.31(7) 2.52(8) 3.3418(10) 118(5) ? Mg1m2 0hw3b O7a 2_566 . 4_575 1.31(7) 2.81(9) 3.643(3) 120(5) ? Ow4 Hw4a O6a . . 2_556 0.93(7) 1.91(7) 2.804(4) 159(6) ? Ow4 Hw4a Ow2 . . 3_666 0.93(7) 2.44(6) 3.013(4) 120(5) ? Ow4 Hw4b P2 . . 4_565 0.91(5) 2.88(6) 3.738(3) 158(6) ? Ow4 Hw4b O6a . . 4_565 0.91(5) 2.46(7) 3.121(3) 129(5) ? Ow4 Hw4b O8a . . 4_565 0.91(5) 2.26(5) 3.121(4) 158(6) ? Ow3 Hx P1 . . 4_565 0.96(7) 2.80(8) 3.622(4) 144(5) ? Ow3 Hx O2a . . 3_666 0.96(7) 2.74(6) 3.210(3) 111(5) ? Ow3 Hx O2a . . 4_565 0.96(7) 1.92(7) 2.872(4) 174(6) ? Ow3 Hx O3a . . 4_565 0.96(7) 2.70(7) 3.183(5) 112(4) ? Ow1 Hy P2 . . 2_556 0.95(7) 2.93(9) 3.670(4) 136(5) ? Ow1 Hy O4a . . . 0.95(7) 2.73(7) 3.184(4) 110(6) ? Ow1 Hy O5a . . 2_556 0.95(7) 1.82(8) 2.739(5) 163(6) ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 347.33 431.23 13.78 o 4 0 0 32167.70 32603.70 128.73 o 6 0 0 741.65 725.59 23.34 o 8 0 0 12986.50 12272.20 78.69 o 10 0 0 1106.32 1071.62 30.61 o 12 0 0 8094.14 8949.60 64.04 o 14 0 0 0.54 47.97 33.21 < 16 0 0 4069.06 4411.52 61.54 o 18 0 0 203.74 187.99 39.83 o 0 1 0 380.04 483.01 14.76 o 1 1 0 727.38 823.28 13.02 o 2 1 0 6294.21 5963.32 34.19 o 3 1 0 6551.25 6858.24 41.03 o 4 1 0 1451.36 1356.21 23.01 o 5 1 0 5180.26 5028.46 35.06 o 6 1 0 498.14 534.24 11.07 o 7 1 0 69.27 57.31 10.85 o 8 1 0 67.08 71.42 10.85 o 9 1 0 39.28 73.26 12.48 o 10 1 0 545.49 539.99 16.39 o 11 1 0 75.99 193.74 13.78 o 12 1 0 11.98 51.56 14.87 o 13 1 0 167.17 183.65 22.58 o 14 1 0 701.23 675.12 27.57 o 15 1 0 1003.88 1037.65 25.62 o 16 1 0 2.42 1.74 21.38 < 17 1 0 4.27 52.42 25.83 < 18 1 0 249.59 306.19 29.31 o 19 1 0 43.12 10.64 35.06 < 0 2 0 2660.00 2578.81 41.35 o 1 2 0 138.67 127.97 13.02 o 2 2 0 3152.77 3066.16 33.21 o 3 2 0 370.24 376.09 12.70 o 4 2 0 5257.43 4636.09 30.50 o 5 2 0 213.82 202.86 9.99 o 6 2 0 540.93 605.98 13.02 o 7 2 0 467.92 427.98 13.35 o 8 2 0 47467.30 48195.80 95.08 o 9 2 0 1.51 18.34 14.33 < 10 2 0 37.31 28.00 13.24 < 11 2 0 766.62 767.71 16.28 o 12 2 0 4537.14 4661.49 35.71 o 13 2 0 1.14 30.72 24.20 < 14 2 0 252.99 261.69 24.53 o 15 2 0 3.85 24.42 20.95 < 16 2 0 2632.83 2600.52 42.66 o 17 2 0 31.81 -31.69 25.07 < 18 2 0 263.46 223.49 29.96 o 19 2 0 71.49 75.44 31.15 < 0 3 0 149.54 150.22 11.94 o 1 3 0 32.50 49.49 8.36 o 2 3 0 61.70 55.79 9.33 o 3 3 0 2451.91 2459.20 20.19 o 4 3 0 11.41 11.51 9.77 < 5 3 0 0.19 6.95 10.31 < 6 3 0 4678.42 4935.23 32.56 o 7 3 0 1872.43 1888.82 22.90 o 8 3 0 293.30 320.52 13.78 o 9 3 0 472.07 549.22 14.11 o 10 3 0 2004.54 1980.00 21.06 o 11 3 0 98.49 165.42 14.98 o 12 3 0 34.42 17.26 22.36 < 13 3 0 87.02 76.52 19.54 o 14 3 0 649.38 591.65 23.23 o 15 3 0 450.49 446.10 24.10 o 16 3 0 2.65 -16.82 24.20 < 17 3 0 8.12 -84.23 28.33 < 18 3 0 21.19 -36.36 29.74 < 0 4 0 70239.10 70894.80 147.40 o 1 4 0 2412.50 2596.83 22.68 o 2 4 0 210.88 198.30 11.72 o 3 4 0 1392.97 1514.79 20.62 o 4 4 0 14897.00 15490.20 57.74 o 5 4 0 1202.22 1160.30 19.43 o 6 4 0 5.39 31.15 13.57 < 7 4 0 1065.85 1052.95 17.26 o 8 4 0 3663.07 3588.89 25.83 o 9 4 0 287.30 284.92 13.57 o 10 4 0 1020.61 996.29 20.19 o 11 4 0 1293.06 1252.45 26.70 o 12 4 0 5982.63 6280.59 47.43 o 13 4 0 127.43 156.19 22.25 o 14 4 0 22.28 -2.17 22.90 < 15 4 0 37.09 12.92 25.40 < 16 4 0 2056.06 2095.27 43.09 o 17 4 0 171.62 202.97 32.89 o 18 4 0 2.26 -52.32 34.73 < 0 5 0 294.93 386.51 20.73 o 1 5 0 274.89 325.73 14.33 o 2 5 0 5329.41 5636.07 36.25 o 3 5 0 2010.23 1961.54 23.01 o 4 5 0 99.21 124.60 12.92 o 5 5 0 2461.05 2316.80 22.58 o 6 5 0 1471.11 1405.82 18.23 o 7 5 0 680.05 660.58 15.85 o 8 5 0 85.21 90.41 16.72 o 9 5 0 39.46 38.86 22.90 < 10 5 0 92.73 99.64 22.47 o 11 5 0 30.98 40.16 18.56 < 12 5 0 49.19 66.86 20.30 o 13 5 0 57.28 63.17 22.36 < 14 5 0 389.49 416.25 25.18 o 15 5 0 722.33 752.40 31.59 o 16 5 0 19.52 115.49 38.86 < 17 5 0 18.54 -19.54 40.38 < 0 6 0 41.13 53.08 17.04 o 1 6 0 993.44 976.86 16.61 o 2 6 0 117.82 130.25 12.48 o 3 6 0 608.11 575.59 15.63 o 4 6 0 6411.00 6481.71 37.45 o 5 6 0 451.05 451.31 18.99 o 6 6 0 878.45 878.42 24.86 o 7 6 0 238.02 265.38 27.79 o 8 6 0 7083.52 7136.64 48.30 o 9 6 0 333.61 308.36 26.92 o 10 6 0 97.81 96.49 19.10 o 11 6 0 255.06 276.56 20.84 o 12 6 0 1015.22 998.14 25.51 o 13 6 0 206.58 218.49 27.35 o 14 6 0 241.74 230.97 32.67 o 15 6 0 185.44 128.95 49.49 < 0 7 0 11.36 50.69 38.42 < 1 7 0 42.47 26.70 25.72 < 2 7 0 1.86 -6.95 28.33 < 3 7 0 465.86 457.39 20.73 o 4 7 0 1.23 -21.71 18.02 < 5 7 0 996.92 902.73 25.83 o 6 7 0 1645.10 1525.43 25.72 o 7 7 0 263.44 228.70 19.10 o 8 7 0 0.98 -5.21 20.19 < 9 7 0 122.14 117.33 20.73 o 10 7 0 412.49 382.06 23.01 o 11 7 0 54.46 54.49 26.59 < 12 7 0 15.54 -26.70 36.69 < 13 7 0 9.37 85.75 46.46 < 14 7 0 217.31 182.67 44.94 o 0 8 0 5379.13 5428.54 56.55 o 1 8 0 366.62 329.85 19.54 o 2 8 0 1141.94 1183.42 24.10 o 3 8 0 435.49 416.47 20.30 o 4 8 0 1671.84 1557.01 26.38 o 5 8 0 873.13 807.65 21.82 o 6 8 0 594.56 559.96 21.60 o 7 8 0 551.18 524.68 22.79 o 8 8 0 723.28 652.33 25.83 o 9 8 0 613.42 568.86 33.43 o 10 8 0 1109.94 1098.10 47.11 o 11 8 0 148.91 137.96 43.42 o 0 9 0 24.35 -11.07 34.19 < 1 9 0 2.99 15.85 26.27 < 2 9 0 418.38 411.48 25.51 o 3 9 0 345.74 295.01 28.65 o 4 9 0 29.58 -37.34 30.61 < 5 9 0 60.93 90.74 32.78 < 6 9 0 149.82 148.92 38.86 o 7 9 0 342.42 315.31 44.39 o 8 9 0 29.23 -10.42 45.04 < 0 10 0 298.93 312.60 60.89 o 1 10 0 164.68 206.99 37.99 o -20 0 1 123.21 116.14 45.26 < -18 0 1 17.88 75.87 38.21 < -16 0 1 319.11 213.61 29.85 o -14 0 1 362.11 288.28 37.23 o -12 0 1 7646.48 7914.01 55.36 o -10 0 1 2374.19 2337.74 42.87 o -8 0 1 6455.56 6046.03 48.95 o -6 0 1 34.39 121.67 16.61 o -4 0 1 943.93 852.80 25.07 o -2 0 1 51.00 106.04 9.44 o 0 0 1 21575.60 22717.60 54.38 o 2 0 1 472.49 479.21 15.74 o 4 0 1 54139.20 52350.20 145.44 o 6 0 1 5048.19 5164.79 46.89 o 8 0 1 1539.25 1642.43 35.17 o 10 0 1 52.05 33.86 19.86 < 12 0 1 1732.45 1710.81 38.42 o 14 0 1 591.76 610.21 34.19 o 16 0 1 1641.02 1584.91 44.50 o 18 0 1 365.73 383.91 45.48 o -20 1 1 0.77 23.01 30.61 < -19 1 1 471.71 552.36 33.43 o -18 1 1 2.78 6.40 28.44 < -17 1 1 0.01 7.92 24.96 < -16 1 1 86.23 85.42 21.06 o -15 1 1 800.12 855.73 33.43 o -14 1 1 585.23 631.16 30.17 o -13 1 1 6.86 -21.27 17.69 < -12 1 1 348.84 361.11 14.44 o -11 1 1 4496.55 4454.39 35.28 o -10 1 1 130.37 173.01 14.98 o -9 1 1 1479.65 1453.14 20.08 o -8 1 1 5.15 33.21 10.96 o -7 1 1 35.76 27.35 11.51 < -6 1 1 8990.50 9649.90 42.87 o -5 1 1 202.87 218.82 11.61 o -4 1 1 313.95 317.48 14.76 o -3 1 1 766.61 820.67 16.72 o -2 1 1 2369.37 2468.21 22.36 o -1 1 1 3665.61 3479.81 23.34 o 0 1 1 341.92 281.66 9.12 o 1 1 1 9442.62 8533.56 37.23 o 2 1 1 1179.84 1260.81 18.34 o 3 1 1 10828.70 10421.30 51.99 o 4 1 1 92.97 85.42 10.42 o 5 1 1 745.49 686.63 13.02 o 6 1 1 4753.09 5013.27 29.20 o 7 1 1 2164.70 2055.97 19.75 o 8 1 1 557.64 550.52 15.41 o 9 1 1 172.45 222.83 16.61 o 10 1 1 134.90 153.37 14.54 o 11 1 1 2008.14 1975.22 24.75 o 12 1 1 88.17 107.46 19.75 o 13 1 1 247.01 256.26 27.03 o 14 1 1 402.02 386.95 22.03 o 15 1 1 9.02 33.00 20.41 < 16 1 1 37.87 68.60 22.68 o 17 1 1 35.64 31.91 26.59 < 18 1 1 13.71 0.87 34.30 < 19 1 1 165.09 73.81 33.65 < -19 2 1 5.70 -20.08 31.59 < -18 2 1 13.10 22.47 28.00 < -17 2 1 96.14 94.32 24.53 o -16 2 1 1334.50 1360.99 31.69 o -15 2 1 16.72 26.48 20.84 < -14 2 1 947.47 902.62 28.44 o -13 2 1 91.77 100.51 18.23 o -12 2 1 48.26 76.85 13.89 o -11 2 1 577.92 610.43 15.30 o -10 2 1 483.80 406.38 14.22 o -9 2 1 359.79 386.62 15.96 o -8 2 1 1216.29 1235.30 19.86 o -7 2 1 1215.25 1263.41 16.06 o -6 2 1 1101.83 1112.65 17.48 o -5 2 1 1400.27 1433.39 18.99 o -4 2 1 36924.10 35654.10 85.53 o -3 2 1 16.52 20.51 10.31 < -2 2 1 3287.84 3362.37 33.97 o -1 2 1 184.76 149.68 13.13 o 0 2 1 3004.72 3091.45 31.15 o 1 2 1 1237.46 1342.32 23.01 o 2 2 1 390.01 378.37 11.61 o 3 2 1 21.31 32.56 9.33 o 4 2 1 790.36 808.52 12.05 o 5 2 1 2903.75 2997.89 21.93 o 6 2 1 663.02 584.49 14.00 o 7 2 1 552.43 605.76 14.87 o 8 2 1 5372.74 5107.05 33.43 o 9 2 1 128.96 106.48 14.44 o 10 2 1 79.33 64.36 13.35 o 11 2 1 399.52 419.51 16.50 o 12 2 1 3193.73 3328.72 37.34 o 13 2 1 16.90 -2.93 27.35 < 14 2 1 137.77 138.82 22.14 o 15 2 1 6.35 28.00 21.60 < 16 2 1 189.46 168.67 24.64 o 17 2 1 17.14 -44.61 29.20 < 18 2 1 354.00 301.20 35.49 o -19 3 1 280.05 296.42 31.80 o -18 3 1 41.04 64.26 29.31 < -17 3 1 20.25 3.15 25.83 < -16 3 1 44.01 44.18 23.55 < -15 3 1 138.64 94.10 20.73 o -14 3 1 682.42 662.31 22.79 o -13 3 1 35.12 38.97 20.51 < -12 3 1 110.54 89.11 19.43 o -11 3 1 3249.30 3234.18 29.41 o -10 3 1 3.99 2.28 12.16 < -9 3 1 253.24 234.99 13.35 o -8 3 1 1128.09 1082.26 21.93 o -7 3 1 2619.49 2574.36 25.40 o -6 3 1 171.23 202.97 12.16 o -5 3 1 129.42 173.01 12.48 o -4 3 1 103.55 141.10 11.07 o -3 3 1 140.99 134.37 10.09 o -2 3 1 8.11 24.42 9.01 < -1 3 1 134.29 170.08 9.66 o 0 3 1 16.18 -0.98 8.25 < 1 3 1 429.68 476.49 10.20 o 2 3 1 373.22 355.36 9.99 o 3 3 1 3986.44 3914.19 22.58 o 4 3 1 94.65 91.28 9.88 o 5 3 1 209.09 251.16 11.61 o 6 3 1 2811.64 2762.57 24.42 o 7 3 1 510.93 480.94 16.17 o 8 3 1 427.23 411.69 14.76 o 9 3 1 1740.69 1685.96 20.62 o 10 3 1 382.46 394.76 15.85 o 11 3 1 1760.75 1699.64 27.79 o 12 3 1 72.23 59.70 22.79 < 13 3 1 0.53 18.02 21.60 < 14 3 1 429.37 388.14 22.68 o 15 3 1 0.05 6.19 23.99 < 16 3 1 15.85 21.06 32.56 < 17 3 1 9.04 0.65 38.42 < 18 3 1 24.35 -51.01 45.15 < -18 4 1 135.36 146.10 32.45 o -17 4 1 300.27 303.48 31.69 o -16 4 1 90.95 53.84 26.92 < -15 4 1 67.11 81.73 24.10 o -14 4 1 0.62 -14.98 21.60 < -13 4 1 34.70 73.92 18.99 o -12 4 1 5011.42 5077.85 43.20 o -11 4 1 164.58 181.80 19.21 o -10 4 1 966.85 988.70 19.32 o -9 4 1 412.83 526.42 15.74 o -8 4 1 2570.55 2469.84 24.96 o -7 4 1 3199.05 3103.82 26.81 o -6 4 1 2969.33 3110.99 27.46 o -5 4 1 951.64 940.18 18.67 o -4 4 1 603.33 605.76 15.52 o -3 4 1 3045.86 2955.23 25.40 o -2 4 1 60.05 94.86 11.51 o -1 4 1 5935.93 5973.85 32.35 o 0 4 1 1410.42 1418.41 17.91 o 1 4 1 2806.77 2731.53 23.77 o 2 4 1 647.27 605.33 14.65 o 3 4 1 9.40 83.14 10.75 o 4 4 1 17166.50 16912.00 54.05 o 5 4 1 596.24 548.56 15.63 o 6 4 1 106.83 92.26 12.27 o 7 4 1 110.01 141.10 12.16 o 8 4 1 38.08 36.80 12.70 < 9 4 1 278.09 301.31 15.63 o 10 4 1 216.49 224.03 24.42 o 11 4 1 1104.85 1048.07 33.00 o 12 4 1 334.99 337.67 30.07 o 13 4 1 194.68 228.80 26.27 o 14 4 1 294.91 305.32 28.87 o 15 4 1 127.73 89.00 35.06 < 16 4 1 671.65 561.26 44.94 o 17 4 1 64.07 15.74 41.14 < -17 5 1 9.15 -13.78 32.56 < -16 5 1 12.10 10.75 32.13 < -15 5 1 409.59 503.95 26.70 o -14 5 1 95.15 88.79 23.01 o -13 5 1 22.84 24.10 20.08 < -12 5 1 9.08 31.15 18.23 < -11 5 1 1082.09 1109.07 22.68 o -10 5 1 784.09 773.03 25.94 o -9 5 1 408.12 369.04 19.75 o -8 5 1 77.89 93.34 14.33 o -7 5 1 198.47 209.38 13.46 o -6 5 1 2332.61 2400.48 22.14 o -5 5 1 0.06 8.25 12.81 < -4 5 1 27.01 51.56 12.27 o -3 5 1 1.14 34.95 13.78 < -2 5 1 2995.49 3308.10 28.87 o -1 5 1 228.23 256.37 13.68 o 0 5 1 207.80 239.98 13.68 o 1 5 1 2988.48 2920.72 26.16 o 2 5 1 431.31 436.33 14.98 o 3 5 1 2441.44 2312.67 24.96 o 4 5 1 138.12 194.29 12.27 o 5 5 1 1059.91 979.03 17.04 o 6 5 1 2.24 22.47 12.59 < 7 5 1 337.19 319.65 15.63 o 8 5 1 85.02 72.72 19.86 o 9 5 1 126.11 174.32 25.72 o 10 5 1 7.68 20.95 23.55 < 11 5 1 836.69 832.40 25.72 o 12 5 1 0.02 15.85 27.35 < 13 5 1 2.83 12.59 31.48 < 14 5 1 98.58 97.14 37.01 < 15 5 1 58.97 57.63 41.90 < 16 5 1 265.19 259.95 43.09 o -16 6 1 788.26 812.75 39.07 o -15 6 1 253.26 249.75 30.61 o -14 6 1 1121.28 1201.54 30.83 o -13 6 1 500.61 486.37 23.77 o -12 6 1 34.70 13.68 21.71 < -11 6 1 536.50 507.43 19.75 o -10 6 1 52.11 33.00 18.67 < -9 6 1 856.12 874.08 22.14 o -8 6 1 5.70 4.45 20.95 < -7 6 1 675.80 672.19 25.07 o -6 6 1 562.56 548.78 21.06 o -5 6 1 199.60 173.12 17.15 o -4 6 1 9800.25 9553.84 42.55 o -3 6 1 22.90 1.63 13.89 < -2 6 1 253.82 229.35 13.24 o -1 6 1 1043.12 989.24 16.93 o 0 6 1 395.69 391.18 13.57 o 1 6 1 1855.33 1766.93 19.75 o 2 6 1 240.52 205.36 14.22 o 3 6 1 1302.06 1268.84 20.19 o 4 6 1 5.92 -2.39 17.91 < 5 6 1 1020.35 982.07 24.96 o 6 6 1 599.71 656.78 28.87 o 7 6 1 1172.65 1165.83 35.06 o 8 6 1 1471.64 1473.11 32.78 o 9 6 1 594.60 578.74 24.64 o 10 6 1 215.10 242.70 24.96 o 11 6 1 171.59 175.40 27.24 o 12 6 1 965.35 856.82 36.58 o 13 6 1 161.97 101.59 41.46 < 14 6 1 5.95 24.96 39.94 < 15 6 1 91.17 95.73 42.76 < -14 7 1 243.27 227.39 31.48 o -13 7 1 68.42 113.32 31.48 o -12 7 1 104.51 107.35 27.24 o -11 7 1 399.89 394.44 23.34 o -10 7 1 310.23 329.75 21.49 o -9 7 1 2.76 -15.41 19.75 < -8 7 1 126.93 123.95 18.89 o -7 7 1 367.57 362.96 18.99 o -6 7 1 21.04 14.44 18.45 < -5 7 1 48.32 27.46 19.21 < -4 7 1 67.94 92.69 18.78 o -3 7 1 0.52 -26.59 19.65 < -2 7 1 16.03 24.53 23.44 < -1 7 1 402.88 379.24 28.65 o 0 7 1 0.14 -8.79 27.68 < 1 7 1 838.47 762.60 31.26 o 2 7 1 559.04 595.34 33.32 o 3 7 1 467.73 432.32 31.37 o 4 7 1 0.07 -3.04 23.01 < 5 7 1 566.31 579.50 20.95 o 6 7 1 450.38 407.03 22.58 o 7 7 1 3.59 -16.39 22.25 < 8 7 1 32.22 31.69 25.29 < 9 7 1 167.68 183.43 27.14 o 10 7 1 155.91 109.08 30.83 o 11 7 1 590.59 501.67 38.10 o 12 7 1 5.19 90.74 44.07 < 13 7 1 30.32 24.31 57.63 < -12 8 1 700.39 665.57 36.25 o -11 8 1 44.56 46.67 35.28 < -10 8 1 568.93 433.29 31.04 o -9 8 1 333.07 293.49 26.48 o -8 8 1 280.34 237.38 23.23 o -7 8 1 628.65 604.14 22.79 o -6 8 1 1770.25 1704.52 27.14 o -5 8 1 1173.02 1156.50 23.66 o -4 8 1 38.25 116.25 20.41 o -3 8 1 399.54 385.64 19.75 o -2 8 1 975.55 919.99 21.27 o -1 8 1 972.78 917.60 21.82 o 0 8 1 236.09 234.66 19.32 o 1 8 1 397.28 381.09 19.86 o 2 8 1 935.57 923.79 23.44 o 3 8 1 325.78 278.73 23.66 o 4 8 1 1936.53 1820.66 32.67 o 5 8 1 105.79 85.86 24.96 o 6 8 1 232.96 200.58 26.92 o 7 8 1 424.87 416.69 30.61 o 8 8 1 145.23 155.00 35.93 o 9 8 1 637.62 590.24 42.11 o 10 8 1 670.77 591.98 48.73 o 11 8 1 219.04 107.78 45.26 < -9 9 1 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14.22 50.15 < 5 4 9 216.01 147.51 59.48 < 6 4 9 275.20 273.41 99.53 < -16 5 9 64.03 4.88 108.32 < -14 5 9 281.59 321.61 147.83 < -13 5 9 11.94 -4.78 62.84 < -12 5 9 20.22 13.13 60.46 < -11 5 9 406.77 233.25 105.93 < -10 5 9 530.86 265.82 103.87 < -9 5 9 109.28 252.57 93.89 < -8 5 9 0.80 89.55 88.68 < -7 5 9 405.18 340.27 82.92 o -6 5 9 113.42 51.01 82.17 < -5 5 9 2.49 96.06 81.51 < -4 5 9 586.34 364.80 91.61 o -3 5 9 638.56 548.89 74.89 o -2 5 9 299.00 219.14 54.05 o -1 5 9 95.90 -17.15 54.70 < 0 5 9 44.37 148.16 82.06 < 1 5 9 488.78 448.38 67.73 o 2 5 9 30.26 -0.43 76.09 < 3 5 9 191.83 204.27 60.13 o 4 5 9 3.20 -146.31 82.71 < -14 6 9 12.74 43.42 77.28 < -13 6 9 59.46 65.99 98.99 < -12 6 9 244.15 252.36 154.89 < -11 6 9 221.76 187.34 160.64 < -9 6 9 61.24 26.05 121.13 < -8 6 9 1208.11 911.74 131.01 o -7 6 9 330.76 -261.26 109.84 < -6 6 9 1094.04 827.40 109.08 o -5 6 9 67.62 -107.67 103.33 < -4 6 9 3.41 94.97 103.55 < -3 6 9 417.83 363.39 88.03 o -2 6 9 165.73 189.29 90.74 < -1 6 9 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32.20 -2.39 102.03 < -4 5 10 0.59 -141.97 102.68 < -3 5 10 990.65 1026.47 88.24 o -2 5 10 89.55 191.25 99.86 < -1 5 10 57.37 -30.07 81.84 < 0 5 10 18.45 -180.94 82.82 < 2 5 10 4.37 161.29 148.16 < -2 0 11 42.13 43.09 113.86 < 0 0 11 3018.95 3629.70 125.91 o 2 0 11 111.28 135.24 94.32 < 4 0 11 998.48 762.60 136.11 o -12 1 11 198.31 150.55 94.86 < -11 1 11 147.63 47.22 89.22 < -10 1 11 17.62 133.83 88.79 < -9 1 11 173.11 145.66 90.31 < -8 1 11 104.54 -16.61 87.48 < -7 1 11 1097.03 910.65 107.13 o -3 1 11 91.54 189.84 80.54 < -2 1 11 264.81 192.66 65.12 < -1 1 11 8.34 -205.68 125.15 < 0 1 11 96.57 230.43 59.70 o 1 1 11 561.35 687.39 63.93 o 2 1 11 50.65 43.09 67.08 < 3 1 11 312.37 344.29 60.24 o 4 1 11 0.11 -31.91 141.10 < -12 2 11 134.12 161.18 102.90 < -11 2 11 48.53 40.59 96.38 < -10 2 11 4.64 -300.87 89.76 < -9 2 11 29.60 3.47 93.78 < -8 2 11 787.07 749.69 97.79 o -7 2 11 131.44 32.67 90.52 < -6 2 11 14.18 56.33 96.17 < -3 2 11 43.58 140.13 109.08 < -2 2 11 92.59 122.22 117.22 < -1 2 11 426.80 337.34 118.31 < 0 2 11 19.18 54.70 86.29 < 1 2 11 134.92 267.23 72.07 o 2 2 11 8.96 -98.88 88.68 < 3 2 11 31.78 109.52 76.74 < -12 3 11 0.29 -114.73 117.77 < -11 3 11 0.32 26.59 105.93 < -10 3 11 108.68 -285.03 100.18 < -9 3 11 312.78 307.93 99.64 o -8 3 11 69.45 45.70 101.81 < -7 3 11 860.18 886.23 102.79 o -6 3 11 297.93 50.69 99.97 < -5 3 11 147.51 302.29 104.20 < -4 3 11 59.05 -224.68 114.08 < -3 3 11 30.42 42.44 112.34 < -2 3 11 343.63 546.61 121.13 o -1 3 11 136.66 169.32 123.41 < 0 3 11 18.66 55.36 100.07 < 1 3 11 387.79 349.07 81.62 o 2 3 11 114.27 61.98 97.36 < 3 3 11 169.81 415.93 152.07 < -10 4 11 430.50 305.76 119.39 < -9 4 11 248.45 262.02 109.41 < -8 4 11 313.39 360.68 111.25 o -7 4 11 483.36 248.23 105.39 < -6 4 11 255.84 155.00 103.76 < -5 4 11 13.21 5.10 86.94 < -4 4 11 23.90 -233.04 133.07 < -3 4 11 34.78 -31.26 138.82 < -2 4 11 39.68 267.12 145.12 < 0 4 11 1390.85 1024.62 167.48 o -4 0 12 704.35 620.42 136.65 o -2 0 12 2.87 -59.48 143.38 < 0 0 12 2086.44 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