data_61_32co _audit_creation_date 2012-08-29 _audit_creation_method ; Olex2 1.2-alpha (compiled Mar 30 2012 14:36:40, GUI svn.r4156) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. Bruker (2011). APEX2 Version 2011.2-4. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2009). SAINT-Plus Version 7.68a. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). SADABS Version 2008-1. Bruker AXS Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C48 H56 Co2 N4 O12), 0.5(H4 O2), 2(O)' _chemical_formula_sum 'C24 H34 Co N2 O9' _chemical_formula_weight 553.46 _chemical_absolute_configuration unk _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 5 _space_group_name_H-M_alt 'C 1 2 1' _space_group_name_Hall 'C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.4467(3) _cell_length_b 8.3661(2) _cell_length_c 9.1549(2) _cell_angle_alpha 90 _cell_angle_beta 107.6420(10) _cell_angle_gamma 90 _cell_volume 1200.42(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5603 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 31.49 _cell_measurement_theta_min 2.60 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0757 before and 0.0583 after correction. The Ratio of minimum to maximum transmission is 0.5803. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'purple' _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 582 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.256 _exptl_crystal_size_min 0.24 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7273 _diffrn_reflns_point_group_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_sigmaI/netI 0.0460 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.507 _diffrn_reflns_theta_min 2.334 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 diffractometer with APEX2 detector' _diffrn_measurement_method '\f and \w scans with a narrow frame width' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.765 _reflns_Friedel_fraction_full 0.939 _reflns_Friedel_fraction_max 0.862 _reflns_number_gt 3360 _reflns_number_total 3413 _reflns_special_details ; The reflections were merged according to the crystal class for structure refinement and the calculation of statistics. _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'APEX2 v2011.2-4 (Bruker, 2011)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.844 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.086 _refine_ls_abs_structure_details ; Flack x determined using 1438 quotients [(I+)-I(-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.164(5) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 3413 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0342 _refine_ls_restrained_S_all 1.463 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.0860 _refine_special_details ; ? ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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 _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.40522(15) 0.4902(3) 0.7830(3) 0.0202(4) Uani 1 1 d D . . C2 C 0.33883(16) 0.9343(4) 0.8625(3) 0.0263(5) Uani 1 1 d D . . H2A H 0.301(2) 0.843(5) 0.843(4) 0.032 Uiso 1 1 d D . . H2B H 0.313(2) 1.028(5) 0.805(4) 0.032 Uiso 1 1 d D . . C3 C 0.44792(18) 0.9881(4) 0.7411(3) 0.0276(6) Uani 1 1 d D . . H3A H 0.4634 1.0866 0.8032 0.033 Uiso 1 1 calc RD . . H3B H 0.4086 1.0166 0.6392 0.033 Uiso 1 1 calc RD . . C4 C 0.52671(16) 0.9068(3) 0.7250(3) 0.0243(5) Uani 1 1 d D . . H4A H 0.5097 0.8156 0.6533 0.029 Uiso 1 1 calc RD . . H4B H 0.5593 0.9831 0.6818 0.029 Uiso 1 1 calc RD . . C5 C 0.62728(17) 0.9838(3) 0.9711(3) 0.0245(5) Uani 1 1 d D . . H5A H 0.5879 1.0755 0.9613 0.029 Uiso 1 1 calc RD . . H5B H 0.6752 1.0182 0.9342 0.029 Uiso 1 1 calc RD . . C6 C 0.64218(12) 0.7244(4) 0.8519(2) 0.0197(4) Uani 1 1 d D . . H6A H 0.6087 0.6287 0.8062 0.024 Uiso 1 1 calc RD . . H6B H 0.6808 0.6929 0.9536 0.024 Uiso 1 1 calc RD . . C7 C 0.69654(14) 0.7721(3) 0.7516(3) 0.0180(4) Uani 1 1 d D . . C8 C 0.67331(13) 0.7219(4) 0.5994(2) 0.0214(4) Uani 1 1 d D . . H8 H 0.6214 0.6652 0.5575 0.026 Uiso 1 1 calc RD . . C9 C 0.72525(15) 0.7539(3) 0.5080(3) 0.0234(5) Uani 1 1 d D . . H9 H 0.7091 0.7177 0.4048 0.028 Uiso 1 1 calc RD . . C10 C 0.80036(16) 0.8383(3) 0.5674(3) 0.0217(4) Uani 1 1 d D . . H10 H 0.8357 0.8602 0.5047 0.026 Uiso 1 1 calc RD . . C11 C 0.82456(14) 0.8915(3) 0.7193(3) 0.0176(4) Uani 1 1 d D . . C12 C 0.77271(14) 0.8565(3) 0.8108(3) 0.0175(4) Uani 1 1 d D . . H12 H 0.7894 0.8906 0.9146 0.021 Uiso 1 1 calc RD . . Co1 Co 0.5000 0.72994(2) 1.0000 0.01567(11) Uani 1 2 d SD . . N1 N 0.58147(13) 0.8486(3) 0.8759(2) 0.0188(4) Uani 1 1 d D . . O1 O 0.45741(14) 0.4994(3) 0.7095(2) 0.0314(5) Uani 1 1 d D . . O2 O 0.41170(11) 0.5608(2) 0.9079(2) 0.0236(4) Uani 1 1 d D . . O3 O 0.40907(11) 0.8748(2) 0.8158(2) 0.0228(4) Uani 1 1 d D . . O4 O 0.5000 0.3011(5) 0.5000 0.0441(8) Uani 1 2 d SGD . . H H 0.4562 0.2884 0.4149 0.066 Uiso 0.5 1 d PGD A -1 HA H 0.5359 0.3425 0.4612 0.066 Uiso 0.5 1 d PGD B -1 O5 O 0.6247(3) 0.3163(5) 0.8004(5) 0.0766(10) Uani 1 1 d 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 C1 0.0153(10) 0.0200(12) 0.0258(10) 0.0004(9) 0.0067(9) -0.0015(8) C2 0.0155(11) 0.0335(14) 0.0298(12) 0.0065(10) 0.0067(9) 0.0096(10) C3 0.0203(12) 0.0315(15) 0.0322(13) 0.0120(11) 0.0100(10) 0.0074(10) C4 0.0184(11) 0.0315(14) 0.0236(10) 0.0078(9) 0.0073(9) 0.0047(9) C5 0.0225(11) 0.0206(11) 0.0332(12) -0.0026(9) 0.0123(10) -0.0063(9) C6 0.0141(8) 0.0194(9) 0.0272(9) 0.0013(12) 0.0089(7) -0.0012(12) C7 0.0118(8) 0.0199(11) 0.0223(9) 0.0000(7) 0.0054(7) -0.0009(7) C8 0.0146(8) 0.0241(10) 0.0239(9) -0.0020(12) 0.0033(7) -0.0031(12) C9 0.0224(10) 0.0266(16) 0.0199(9) -0.0045(8) 0.0044(8) -0.0034(9) C10 0.0202(11) 0.0250(11) 0.0214(10) -0.0008(8) 0.0088(8) -0.0021(9) C11 0.0128(9) 0.0191(10) 0.0211(10) -0.0005(8) 0.0055(8) -0.0010(8) C12 0.0128(9) 0.0205(11) 0.0194(9) -0.0010(8) 0.0053(7) -0.0012(8) Co1 0.00956(17) 0.01699(19) 0.02051(18) 0.000 0.00464(12) 0.000 N1 0.0133(8) 0.0194(9) 0.0238(9) 0.0018(7) 0.0057(7) 0.0004(7) O1 0.0224(10) 0.0431(13) 0.0336(10) -0.0089(9) 0.0158(8) -0.0115(9) O2 0.0173(8) 0.0258(9) 0.0291(9) -0.0083(7) 0.0090(7) -0.0061(7) O3 0.0158(8) 0.0269(10) 0.0266(9) 0.0054(7) 0.0078(7) 0.0060(7) O4 0.0375(17) 0.056(2) 0.0455(18) 0.000 0.0228(15) 0.000 O5 0.076(2) 0.058(2) 0.084(2) 0.0152(18) 0.0057(19) 0.0072(18) _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 C1 C11 1.521(3) 3_445 ? C1 O1 1.243(3) . ? C1 O2 1.262(3) . ? C2 H2A 0.96(4) . ? C2 H2B 0.97(4) . ? C2 C5 1.512(4) 2_657 ? C2 O3 1.437(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.509(4) . ? C3 O3 1.428(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 N1 1.484(3) . ? C5 C2 1.512(4) 2_657 ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 N1 1.486(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.516(3) . ? C6 N1 1.503(4) . ? C7 C8 1.393(3) . ? C7 C12 1.397(3) . ? C8 H8 0.9500 . ? C8 C9 1.391(3) . ? C9 H9 0.9500 . ? C9 C10 1.383(3) . ? C10 H10 0.9500 . ? C10 C11 1.398(3) . ? C11 C1 1.521(3) 3 ? C11 C12 1.395(3) . ? C12 H12 0.9500 . ? Co1 N1 2.235(2) 2_657 ? Co1 N1 2.235(2) . ? Co1 O2 2.0203(18) . ? Co1 O2 2.0202(18) 2_657 ? Co1 O3 2.2404(18) 2_657 ? Co1 O3 2.2405(18) . ? O4 H 0.8930 . ? O4 HA 0.8500 . ? 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 C1 C11 119.4(2) . 3_445 ? O1 C1 O2 125.3(2) . . ? O2 C1 C11 115.2(2) . 3_445 ? H2A C2 H2B 113(3) . . ? C5 C2 H2A 115(2) 2_657 . ? C5 C2 H2B 107(2) 2_657 . ? O3 C2 H2A 101(2) . . ? O3 C2 H2B 113(2) . . ? O3 C2 C5 108.1(2) . 2_657 ? H3A C3 H3B 108.7 . . ? C4 C3 H3A 110.6 . . ? C4 C3 H3B 110.6 . . ? O3 C3 H3A 110.6 . . ? O3 C3 H3B 110.6 . . ? O3 C3 C4 105.7(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N1 C4 C3 110.7(2) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C2 C5 H5A 109.6 2_657 . ? C2 C5 H5B 109.6 2_657 . ? H5A C5 H5B 108.1 . . ? N1 C5 C2 110.4(2) . 2_657 ? N1 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? H6A C6 H6B 107.3 . . ? C7 C6 H6A 108.2 . . ? C7 C6 H6B 108.2 . . ? N1 C6 H6A 108.2 . . ? N1 C6 H6B 108.2 . . ? N1 C6 C7 116.5(2) . . ? C8 C7 C6 119.5(2) . . ? C8 C7 C12 118.8(2) . . ? C12 C7 C6 121.5(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 C7 120.8(2) . . ? C9 C8 H8 119.6 . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0(2) . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 119.8 . . ? C9 C10 C11 120.3(2) . . ? C11 C10 H10 119.8 . . ? C10 C11 C1 120.4(2) . 3 ? C12 C11 C1 120.3(2) . 3 ? C12 C11 C10 119.3(2) . . ? C7 C12 H12 119.6 . . ? C11 C12 C7 120.8(2) . . ? C11 C12 H12 119.6 . . ? N1 Co1 N1 127.25(11) 2_657 . ? N1 Co1 O3 77.07(7) 2_657 . ? N1 Co1 O3 75.13(7) . . ? N1 Co1 O3 77.07(7) . 2_657 ? N1 Co1 O3 75.13(7) 2_657 2_657 ? O2 Co1 N1 124.39(7) . . ? O2 Co1 N1 124.39(7) 2_657 2_657 ? O2 Co1 N1 93.31(7) 2_657 . ? O2 Co1 N1 93.31(7) . 2_657 ? O2 Co1 O2 91.05(11) 2_657 . ? O2 Co1 O3 157.60(7) . 2_657 ? O2 Co1 O3 157.60(7) 2_657 . ? O2 Co1 O3 80.40(8) . . ? O2 Co1 O3 80.40(8) 2_657 2_657 ? O3 Co1 O3 114.52(11) 2_657 . ? C4 N1 C5 110.7(2) . . ? C4 N1 C6 109.51(18) . . ? C4 N1 Co1 109.31(14) . . ? C5 N1 C6 111.77(19) . . ? C5 N1 Co1 108.37(14) . . ? C6 N1 Co1 107.11(15) . . ? C1 O2 Co1 123.95(16) . . ? C2 O3 Co1 112.14(14) . . ? C3 O3 C2 115.4(2) . . ? C3 O3 Co1 115.21(15) . . ? H O4 HA 99.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C6 H6A O1 0.99 2.61 3.475(3) 146.1 . C6 H6A O5 0.99 2.63 3.447(5) 140.0 . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C11 C12 C7 177.1(2) 3 . . . ? C2 C5 N1 C4 163.0(2) 2_657 . . . ? C2 C5 N1 C6 -74.7(2) 2_657 . . . ? C2 C5 N1 Co1 43.1(2) 2_657 . . . ? C3 C4 N1 C5 -74.9(3) . . . . ? C3 C4 N1 C6 161.4(2) . . . . ? C3 C4 N1 Co1 44.3(2) . . . . ? C4 C3 O3 C2 171.7(2) . . . . ? C4 C3 O3 Co1 38.5(3) . . . . ? C5 C2 O3 C3 -95.7(3) 2_657 . . . ? C5 C2 O3 Co1 38.9(3) 2_657 . . . ? C6 C7 C8 C9 -175.3(3) . . . . ? C6 C7 C12 C11 176.2(2) . . . . ? C7 C6 N1 C4 54.0(3) . . . . ? C7 C6 N1 C5 -69.0(2) . . . . ? C7 C6 N1 Co1 172.42(15) . . . . ? C7 C8 C9 C10 -0.9(4) . . . . ? C8 C7 C12 C11 0.5(4) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C9 C10 C11 C1 -177.5(2) . . . 3 ? C9 C10 C11 C12 0.9(4) . . . . ? C10 C11 C12 C7 -1.2(4) . . . . ? C11 C1 O2 Co1 -168.65(15) 3_445 . . . ? C12 C7 C8 C9 0.5(4) . . . . ? N1 C6 C7 C8 -100.5(3) . . . . ? N1 C6 C7 C12 83.8(3) . . . . ? O1 C1 O2 Co1 9.3(4) . . . . ? O3 C3 C4 N1 -54.3(3) . . . . ? _shelx_estimated_absorpt_T_max 0.836 _shelx_estimated_absorpt_T_min 0.753 _shelx_hkl_checksum 95650 _shelx_hkl_file ; 2 0 0 144.98 6.91 2 0 0 145.77 8.19 -2 0 0 153.23 7.28 -4 0 0 2.11 0.17 4 0 0 1.93 0.20 4 0 0 1.75 0.13 6 0 0 23.83 1.54 -6 0 0 26.09 1.35 6 0 0 27.12 1.25 8 0 0 1.20 0.13 8 0 0 1.13 0.21 -8 0 0 1.20 0.19 10 0 0 105.76 6.39 10 0 0 115.70 5.30 -10 0 0 115.66 5.64 12 0 0 45.13 2.82 -12 0 0 48.22 2.49 -14 0 0 12.37 0.84 14 0 0 12.17 0.96 16 0 0 0.34 0.24 -16 0 0 0.43 0.22 18 0 0 2.61 0.50 -18 0 0 2.27 0.41 -20 0 0 4.73 0.57 20 0 0 4.43 0.64 -22 0 0 31.27 1.96 1 -1 0 386.93 21.64 -1 -1 0 389.24 18.37 1 -1 0 361.85 19.09 -1 -1 0 427.23 19.19 1 1 0 389.54 21.66 -3 -1 0 6.06 0.40 3 -1 0 6.43 0.35 -3 -1 0 6.00 0.36 3 -1 0 6.28 0.44 3 1 0 7.07 0.46 -3 1 0 7.70 0.38 -5 -1 0 28.56 1.37 -5 -1 0 30.93 1.48 5 -1 0 28.64 1.35 5 -1 0 27.80 1.66 -5 1 0 28.27 1.45 5 1 0 25.07 1.66 7 -1 0 9.24 0.54 7 -1 0 9.14 0.71 -7 -1 0 9.75 0.64 7 1 0 10.89 0.74 -7 1 0 12.68 0.64 7 1 0 12.16 0.58 -9 -1 0 27.96 1.45 9 -1 0 25.53 1.63 9 -1 0 27.45 1.28 -9 1 0 26.86 1.42 9 1 0 23.65 1.62 9 1 0 26.14 1.31 -11 -1 0 61.49 3.25 11 -1 0 62.48 2.98 11 -1 0 60.90 3.68 -11 1 0 62.60 3.23 11 1 0 61.83 3.69 11 1 0 66.40 3.02 13 -1 0 41.35 2.62 -13 -1 0 41.54 2.32 13 1 0 43.58 2.64 -13 1 0 43.93 2.30 15 -1 0 7.03 0.71 -15 -1 0 7.81 0.65 -15 1 0 7.73 0.62 15 1 0 8.36 0.74 -17 -1 0 0.83 0.28 17 -1 0 0.83 0.31 17 1 0 0.30 0.24 -17 1 0 0.64 0.24 -19 -1 0 3.65 0.54 19 -1 0 2.61 0.53 -19 1 0 3.14 0.48 19 1 0 4.22 0.59 21 -1 0 14.68 1.24 -21 -1 0 14.32 1.09 -21 1 0 13.04 1.03 21 1 0 13.37 1.22 0 -2 0 595.94 29.85 0 -2 0 614.54 33.76 0 -2 0 621.72 28.67 0 2 0 607.30 33.75 2 -2 0 94.67 5.38 -2 -2 0 107.65 4.78 2 -2 0 93.94 4.74 -2 -2 0 98.42 4.57 2 2 0 88.95 5.39 4 -2 0 156.89 7.33 -4 -2 0 155.57 7.35 4 -2 0 153.93 8.70 -4 -2 0 160.29 7.71 -4 2 0 163.65 7.66 4 2 0 147.48 8.70 -6 -2 0 200.48 9.38 6 -2 0 207.16 9.35 -6 -2 0 204.03 9.85 6 -2 0 188.99 11.11 6 2 0 184.19 11.12 -6 2 0 212.80 9.80 -8 -2 0 93.06 4.32 8 -2 0 84.91 5.14 8 -2 0 94.87 4.27 -8 -2 0 92.39 4.58 8 2 0 82.05 5.15 -8 2 0 95.69 4.53 10 -2 0 86.55 3.99 -10 -2 0 82.18 4.30 10 -2 0 79.33 4.84 10 2 0 85.99 4.05 -10 2 0 87.38 4.26 12 -2 0 22.52 1.59 -12 2 0 24.33 1.38 12 2 0 25.92 1.63 12 2 0 25.57 1.28 14 -2 0 50.99 2.98 -14 -2 0 45.69 2.62 14 2 0 48.97 2.99 -14 2 0 47.88 2.58 -16 -2 0 32.22 1.91 16 -2 0 34.67 2.15 -16 2 0 31.04 1.84 16 2 0 32.12 2.15 -18 -2 0 8.97 0.77 18 -2 0 9.46 0.86 18 2 0 8.19 0.84 -18 2 0 7.18 0.67 -20 -2 0 7.53 0.74 20 -2 0 6.92 0.78 20 2 0 6.93 0.82 -22 -2 0 2.86 0.55 1 -3 0 8.63 0.53 -1 -3 0 8.29 0.48 1 -3 0 8.14 0.47 1 -3 0 8.22 0.48 3 -3 0 73.35 4.19 -3 -3 0 79.08 3.75 -3 -3 0 75.31 3.58 3 -3 0 69.77 3.69 3 3 0 75.99 4.21 -5 -3 0 448.93 21.57 5 -3 0 445.55 20.65 -5 -3 0 443.86 20.76 5 -3 0 444.09 24.38 5 3 0 408.59 24.38 -5 3 0 452.50 21.60 -7 -3 0 118.90 5.76 7 -3 0 110.07 6.47 7 -3 0 121.95 5.43 -7 -3 0 118.81 5.48 7 3 0 103.97 6.48 -7 3 0 115.54 5.68 9 -3 0 23.32 1.12 -9 -3 0 22.47 1.29 9 -3 0 21.23 1.40 -9 -3 0 22.76 1.18 -9 3 0 22.93 1.21 9 3 0 20.60 1.42 -11 -3 0 11.05 0.70 -11 -3 0 9.27 0.77 11 -3 0 10.62 0.86 11 3 0 13.25 0.92 -11 3 0 13.64 0.75 11 3 0 13.88 0.73 -13 -3 0 6.93 0.61 13 -3 0 7.24 0.66 13 3 0 7.67 0.51 -13 3 0 7.55 0.56 13 3 0 7.69 0.69 -15 -3 0 31.21 1.86 15 -3 0 32.87 2.08 -15 3 0 31.04 1.78 15 3 0 31.82 2.10 -17 -3 0 51.26 2.97 17 -3 0 54.41 3.33 17 3 0 55.10 3.36 -19 -3 0 5.68 0.64 19 -3 0 5.71 0.69 19 3 0 6.23 0.73 -21 -3 0 6.77 0.76 21 -3 0 6.91 0.81 21 3 0 7.60 0.87 0 -4 0 89.09 4.43 0 -4 0 95.04 4.60 0 -4 0 88.01 5.18 0 4 0 97.90 5.19 -2 -4 0 46.93 2.33 2 -4 0 45.27 2.24 -2 -4 0 45.62 2.25 2 -4 0 44.29 2.29 2 -4 0 47.18 2.60 2 4 0 44.39 2.61 -4 -4 0 32.91 1.66 -4 -4 0 32.77 1.73 4 -4 0 31.92 1.89 4 -4 0 32.25 1.62 4 4 0 30.24 1.91 -4 4 0 34.85 1.66 6 -4 0 145.42 6.66 6 -4 0 137.38 7.89 -6 -4 0 144.79 6.71 -6 -4 0 145.54 7.03 6 4 0 129.57 7.90 -6 4 0 142.26 6.94 8 -4 0 31.32 1.52 8 -4 0 29.65 1.85 -8 -4 0 31.52 1.58 -8 -4 0 29.33 1.68 8 4 0 29.10 1.86 -8 4 0 31.07 1.59 -10 -4 0 8.73 0.71 10 -4 0 9.05 0.75 -10 -4 0 9.39 0.63 10 4 0 12.01 0.82 -10 4 0 11.69 0.65 12 -4 0 4.66 0.47 -12 -4 0 4.27 0.36 -12 -4 0 4.37 0.45 -12 4 0 2.87 0.33 12 4 0 3.00 0.34 12 4 0 3.48 0.44 -14 -4 0 8.33 0.72 14 -4 0 8.76 0.78 14 4 0 8.48 0.60 14 4 0 11.12 0.85 -16 -4 0 17.51 1.24 16 -4 0 18.24 1.34 16 4 0 18.75 1.38 -18 -4 0 17.57 1.26 18 -4 0 17.47 1.34 18 4 0 17.36 1.37 20 -4 0 16.01 1.31 -20 -4 0 14.57 1.20 20 4 0 17.83 1.38 1 -5 0 144.41 6.75 1 -5 0 139.24 6.51 -1 -5 0 138.56 6.51 1 -5 0 134.52 7.61 -1 5 0 131.87 7.62 1 5 0 130.43 7.62 3 -5 0 37.93 1.82 3 -5 0 36.92 1.84 -3 -5 0 35.09 1.84 3 -5 0 37.07 2.09 -3 -5 0 38.94 1.91 3 5 0 29.94 2.09 -5 -5 0 108.41 5.33 -5 -5 0 105.23 5.10 5 -5 0 107.02 5.06 5 -5 0 102.73 5.95 -5 5 0 111.55 5.24 5 5 0 99.45 5.96 -7 -5 0 35.40 1.87 -7 -5 0 35.86 1.97 7 -5 0 36.41 2.15 7 -5 0 39.63 1.83 7 5 0 32.04 2.15 -7 5 0 36.96 1.86 9 -5 0 22.95 1.14 -9 -5 0 21.16 1.20 -9 -5 0 20.51 1.29 9 -5 0 21.28 1.39 -9 5 0 21.95 1.17 9 5 0 21.03 1.41 11 -5 0 9.70 0.74 -11 -5 0 9.10 0.71 -11 -5 0 8.91 0.63 11 5 0 8.26 0.73 -13 -5 0 15.01 1.05 13 -5 0 17.19 1.14 -13 -5 0 15.07 0.94 13 5 0 13.96 0.91 13 5 0 14.96 1.14 15 -5 0 7.66 0.74 -15 -5 0 7.39 0.71 15 5 0 8.28 0.77 17 -5 0 9.82 0.91 -17 -5 0 9.18 0.86 17 5 0 11.04 0.96 19 -5 0 5.93 0.72 -19 -5 0 5.58 0.68 19 5 0 6.83 0.76 0 -6 0 61.54 3.05 0 -6 0 66.61 3.14 0 6 0 56.48 3.50 2 -6 0 6.45 0.40 -2 -6 0 6.12 0.45 2 -6 0 6.14 0.44 2 -6 0 5.75 0.43 2 6 0 4.78 0.43 -2 6 0 4.60 0.42 4 -6 0 20.00 1.06 4 -6 0 18.53 1.20 4 -6 0 19.80 1.08 -4 -6 0 19.81 1.14 -4 -6 0 20.01 1.12 4 6 0 19.13 1.22 6 -6 0 41.08 2.50 -6 -6 0 44.42 2.22 -6 -6 0 43.28 2.31 6 -6 0 37.54 2.14 6 6 0 43.92 2.55 -6 6 0 46.69 2.19 -8 -6 0 5.94 0.55 8 -6 0 5.83 0.53 -8 -6 0 6.23 0.52 8 -6 0 6.68 0.47 8 6 0 7.29 0.58 -10 -6 0 15.38 1.05 -10 -6 0 15.76 0.98 10 -6 0 17.04 1.11 10 6 0 14.99 1.11 -12 -6 0 48.43 2.78 12 -6 0 55.37 3.06 -12 -6 0 47.68 2.60 12 6 0 49.67 3.07 -14 -6 0 5.53 0.51 14 -6 0 6.17 0.62 -14 -6 0 5.18 0.58 14 6 0 5.19 0.59 14 6 0 4.70 0.47 -16 -6 0 0.45 0.28 16 -6 0 0.47 0.27 16 6 0 1.01 0.35 -18 -6 0 2.54 0.52 18 6 0 3.73 0.56 1 -7 0 38.90 2.06 -1 -7 0 40.54 2.10 -1 -7 0 39.05 2.07 1 -7 0 41.67 2.08 1 7 0 39.65 2.33 -1 7 0 38.01 2.32 3 -7 0 10.30 0.70 3 -7 0 11.47 0.66 -3 -7 0 10.25 0.72 -3 -7 0 11.33 0.72 3 7 0 10.12 0.73 -3 7 0 10.02 0.72 -5 -7 0 14.79 0.96 5 -7 0 15.52 0.93 -5 -7 0 14.53 0.97 5 7 0 17.30 1.06 -7 -7 0 17.47 1.06 -7 -7 0 17.50 1.09 7 7 0 16.96 1.16 -9 -7 0 23.04 1.47 -9 -7 0 23.02 1.40 9 7 0 26.76 1.61 -11 -7 0 17.88 1.14 -11 -7 0 18.31 1.22 11 7 0 18.43 1.29 -13 -7 0 14.57 0.97 -13 -7 0 13.58 1.04 13 7 0 13.97 1.09 -15 -7 0 10.37 0.89 -15 -7 0 10.79 0.79 15 7 0 7.62 0.70 15 7 0 11.28 0.93 -17 -7 0 3.98 0.63 17 7 0 2.75 0.54 0 -8 0 60.95 3.11 -2 -8 0 7.00 0.53 2 -8 0 6.91 0.55 -2 -8 0 6.46 0.57 -4 -8 0 4.69 0.45 -4 -8 0 5.21 0.50 4 -8 0 5.30 0.48 -6 -8 0 1.62 0.32 -6 -8 0 1.74 0.32 6 -8 0 2.32 0.34 -8 -8 0 9.65 0.77 -8 -8 0 10.19 0.77 -10 -8 0 4.61 0.50 -10 -8 0 3.93 0.50 -12 -8 0 4.91 0.58 -12 -8 0 4.81 0.53 -14 -8 0 11.37 0.96 -14 -8 0 11.32 0.88 -16 -8 0 2.25 0.50 1 -9 0 12.00 0.86 -1 -9 0 13.05 0.90 3 -9 0 3.48 0.42 -3 -9 0 2.88 0.44 -5 -9 0 6.72 0.62 -5 -9 0 6.29 0.57 5 -9 0 7.26 0.59 -7 -9 0 18.21 1.22 -7 -9 0 20.00 1.26 7 -9 0 19.38 1.17 -9 -9 0 0.92 0.30 -9 -9 0 1.06 0.33 -11 -9 0 6.14 0.63 -11 -9 0 5.94 0.64 -13 -9 0 11.45 0.97 -13 -9 0 12.20 0.94 -15 -9 0 5.55 0.64 -15 -9 0 4.75 0.65 15 9 0 4.78 0.54 0 -10 0 2.08 0.41 -2 -10 0 5.37 0.56 2 -10 0 4.75 0.54 -4 -10 0 6.02 0.63 4 -10 0 6.27 0.60 -6 -10 0 20.92 1.37 6 -10 0 20.83 1.30 -8 -10 0 5.80 0.62 -8 -10 0 5.06 0.57 -10 -10 0 1.03 0.34 -10 -10 0 1.36 0.39 -12 -10 0 4.50 0.59 -12 -10 0 4.21 0.62 1 -11 0 3.63 0.55 -1 -11 0 3.60 0.55 3 -11 0 5.12 0.59 -3 -11 0 5.05 0.61 5 -11 0 6.16 0.65 -5 -11 0 5.80 0.67 -7 -11 0 8.18 0.79 0 -12 0 9.36 0.86 2 -12 0 7.59 0.76 4 -12 0 -0.12 0.29 22 0 -1 10.96 1.07 -22 0 1 10.77 0.91 -20 0 1 4.87 0.56 20 0 -1 6.05 0.71 18 0 -1 4.90 0.60 -18 0 1 4.20 0.49 -16 0 1 5.67 0.53 16 0 -1 6.48 0.65 -14 0 1 81.40 4.23 14 0 -1 82.96 4.83 12 0 -1 54.54 3.34 12 0 -1 56.87 2.73 -12 0 1 57.38 2.94 10 0 -1 4.93 0.32 10 0 -1 4.10 0.43 -10 0 1 4.76 0.38 -8 0 1 22.29 1.14 8 0 -1 19.01 1.30 8 0 -1 21.37 1.06 6 0 -1 42.23 1.96 6 0 -1 36.38 2.34 -6 0 1 42.85 2.07 -4 0 1 8.54 0.48 -2 0 1 482.75 23.24 2 0 -1 466.38 26.36 0 0 -1 258.92 11.92 0 0 -1 247.37 12.47 0 0 1 256.35 14.13 2 0 1 43.63 2.54 -2 0 -1 46.29 2.11 4 0 1 243.27 13.67 -4 0 -1 251.69 12.07 -4 0 -1 243.52 11.51 6 0 1 79.63 3.61 6 0 1 72.22 4.37 -6 0 -1 78.71 3.86 -8 0 -1 147.36 7.34 8 0 1 156.03 6.92 8 0 1 139.52 8.31 10 0 1 80.80 3.76 -10 0 -1 78.62 4.07 -12 0 -1 52.29 2.74 12 0 1 50.41 3.10 14 0 1 6.43 0.64 -14 0 -1 6.19 0.55 16 0 1 36.87 2.34 -16 0 -1 34.05 2.04 -18 0 -1 10.09 0.84 18 0 1 10.51 0.97 -20 0 -1 7.66 0.75 20 0 1 7.46 0.84 -22 0 -1 6.35 0.72 -23 -1 1 3.50 0.58 21 -1 -1 22.84 1.67 -21 -1 1 19.57 1.43 21 1 -1 23.33 1.71 -19 -1 1 7.62 0.72 19 -1 -1 8.49 0.85 -19 1 1 8.45 0.72 19 1 -1 9.84 0.89 -17 -1 1 0.23 0.19 17 -1 -1 0.36 0.24 -17 1 1 0.54 0.22 17 1 -1 0.46 0.26 -15 -1 1 36.58 2.13 15 -1 -1 38.25 2.42 -15 1 1 40.13 2.12 15 1 -1 38.68 2.45 -13 -1 1 46.25 2.42 13 -1 -1 43.81 2.72 -13 1 1 43.97 2.37 13 1 -1 45.21 2.75 13 1 -1 45.01 2.22 -11 -1 1 99.68 4.88 11 -1 -1 92.51 5.51 11 -1 -1 97.26 4.57 -11 1 1 96.60 4.84 11 1 -1 93.60 5.53 11 1 -1 98.07 4.61 9 -1 -1 43.57 2.09 -9 -1 1 44.65 2.26 9 -1 -1 40.04 2.54 9 1 -1 44.21 2.11 9 1 -1 39.92 2.55 -9 1 1 45.93 2.23 -7 -1 1 0.86 0.15 7 -1 -1 0.64 0.15 7 -1 -1 0.62 0.10 7 1 -1 0.45 0.13 -7 1 1 0.76 0.12 -5 -1 1 53.67 2.56 5 -1 -1 51.84 2.42 5 -1 -1 51.10 2.88 5 1 -1 50.73 2.43 -5 1 1 52.05 2.52 5 1 -1 45.14 2.89 -3 -1 1 397.16 19.06 -3 -1 1 412.80 19.90 3 -1 -1 388.85 22.44 3 -1 -1 413.61 18.98 3 1 -1 383.21 22.52 3 1 -1 414.83 19.09 -3 1 1 425.28 19.81 -1 -1 1 45.16 2.52 -1 -1 1 43.09 2.22 1 -1 -1 47.41 2.13 1 -1 -1 46.69 2.19 -1 -1 1 43.75 2.12 1 1 -1 42.15 2.52 1 -1 1 738.84 35.50 1 -1 1 744.23 42.12 -1 -1 -1 773.94 35.60 -1 -1 -1 780.00 37.22 1 1 1 762.00 42.04 -3 -1 -1 27.57 1.24 3 -1 1 25.93 1.20 -3 -1 -1 28.50 1.33 3 -1 1 25.02 1.49 -3 1 -1 23.44 1.30 3 1 1 23.00 1.48 -5 -1 -1 89.09 4.46 5 -1 1 83.60 5.04 -5 -1 -1 88.80 4.21 5 1 1 87.89 5.04 -5 1 -1 97.90 4.45 7 -1 1 208.37 12.29 -7 -1 -1 231.88 10.32 -7 -1 -1 222.23 10.87 -7 1 -1 230.24 10.85 7 1 1 209.06 12.29 -9 -1 -1 33.53 1.73 9 -1 1 31.13 1.94 9 1 1 29.28 1.93 9 1 1 31.63 1.55 -9 1 -1 32.64 1.70 11 -1 1 74.15 4.52 -11 -1 -1 74.46 4.00 11 1 1 76.22 4.52 11 1 1 82.36 3.70 -11 1 -1 80.92 3.99 -13 -1 -1 21.52 1.35 13 -1 1 21.60 1.52 13 1 1 23.86 1.55 -13 1 -1 22.85 1.33 15 -1 1 35.04 2.23 -15 -1 -1 31.61 1.94 -15 1 -1 34.37 1.94 15 1 1 34.95 2.24 17 -1 1 4.05 0.55 -17 -1 -1 3.23 0.50 17 1 1 4.04 0.56 -17 1 -1 3.21 0.44 -19 -1 -1 9.18 0.82 19 -1 1 9.58 0.92 -19 1 -1 8.39 0.77 19 1 1 9.06 0.92 -21 -1 -1 14.93 1.15 21 -1 1 15.62 1.30 21 1 1 14.67 1.29 -21 1 -1 13.11 1.09 -22 -2 1 1.29 0.39 22 -2 -1 1.49 0.44 -20 -2 1 27.77 1.77 20 -2 -1 28.16 1.97 20 2 -1 28.34 2.00 -18 -2 1 14.89 1.07 18 -2 -1 15.69 1.21 18 2 -1 15.74 1.24 -18 2 1 14.52 1.01 16 -2 -1 38.25 2.33 -16 -2 1 34.02 2.04 16 2 -1 37.11 2.35 -16 2 1 34.25 1.98 -14 -2 1 19.82 1.26 14 -2 -1 20.51 1.42 14 2 -1 20.82 1.45 14 2 -1 21.70 1.14 -14 2 1 21.18 1.22 12 -2 -1 8.62 0.49 -12 -2 1 7.98 0.62 12 -2 -1 8.09 0.68 -12 2 1 8.97 0.58 12 2 -1 8.40 0.54 12 2 -1 8.10 0.70 -10 -2 1 51.76 2.65 10 -2 -1 53.05 2.44 10 -2 -1 48.87 2.96 10 2 -1 46.72 2.98 -10 2 1 51.49 2.58 -8 -2 1 22.84 1.22 8 -2 -1 20.66 1.34 8 -2 -1 23.07 1.10 -8 2 1 22.17 1.15 8 2 -1 19.58 1.36 8 2 -1 22.53 1.14 6 -2 -1 31.69 1.89 -6 -2 1 33.17 1.60 6 -2 -1 34.37 1.58 -6 -2 1 34.95 1.71 6 2 -1 27.73 1.90 -6 2 1 31.62 1.63 4 -2 -1 257.69 13.47 -4 -2 1 233.24 11.40 -4 -2 1 249.23 11.94 4 -2 -1 255.24 11.40 -4 2 1 246.28 11.89 4 2 -1 217.54 13.50 2 -2 -1 43.05 2.38 -2 -2 1 43.90 2.06 2 -2 -1 40.57 2.09 2 -2 -1 44.70 2.05 2 2 -1 41.31 2.43 0 -2 1 28.79 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9.85 0.79 15 -3 -11 7.06 0.72 15 3 -11 7.65 0.73 15 3 -11 7.43 0.80 -13 -3 11 5.68 0.58 13 -3 -11 4.73 0.55 13 3 -11 4.48 0.60 13 3 -11 4.49 0.55 -11 -3 11 4.76 0.56 11 -3 -11 4.85 0.55 11 3 -11 5.84 0.58 11 3 -11 5.78 0.65 -9 -3 11 3.06 0.46 9 -3 -11 2.50 0.42 9 3 -11 2.02 0.43 9 3 -11 2.17 0.40 7 -3 -11 11.34 0.87 7 3 -11 13.09 1.05 7 3 -11 11.87 0.88 7 3 -11 12.77 0.88 5 -3 -11 4.20 0.47 -5 -3 11 4.45 0.52 5 3 -11 3.36 0.43 5 3 -11 3.93 0.48 5 3 -11 5.06 0.60 3 -3 -11 2.85 0.43 -3 -3 11 3.37 0.47 3 3 -11 3.61 0.46 3 3 -11 3.67 0.54 -1 -3 11 1.78 0.40 1 3 -11 2.02 0.40 1 -3 11 2.47 0.48 -1 3 -11 1.45 0.39 3 -3 11 1.77 0.44 -3 3 -11 1.64 0.43 -16 -4 11 24.69 1.62 14 -4 -11 2.06 0.45 -14 -4 11 2.90 0.50 14 4 -11 2.41 0.49 14 4 -11 2.04 0.44 12 -4 -11 3.18 0.52 -12 -4 11 3.43 0.52 12 4 -11 4.14 0.56 12 4 -11 3.26 0.52 10 -4 -11 1.53 0.36 -10 -4 11 1.31 0.35 10 4 -11 0.77 0.31 10 4 -11 0.90 0.31 -8 -4 11 1.13 0.34 8 -4 -11 1.57 0.35 8 4 -11 1.74 0.41 8 4 -11 1.89 0.38 -6 -4 11 5.42 0.62 6 -4 -11 5.40 0.55 6 4 -11 6.01 0.67 6 4 -11 4.60 0.54 6 4 -11 6.02 0.56 -4 -4 11 9.31 0.84 4 -4 -11 8.90 0.72 4 4 -11 9.98 0.92 4 4 -11 8.09 0.75 -2 -4 11 12.97 1.07 2 -4 -11 12.78 0.92 2 4 -11 11.80 0.97 2 4 -11 15.58 1.22 0 -4 11 1.50 0.39 0 4 -11 0.95 0.34 2 -4 11 6.19 0.73 -2 4 -11 6.23 0.71 -13 -5 11 2.94 0.52 13 -5 -11 2.15 0.45 13 5 -11 3.28 0.54 -11 -5 11 1.72 0.41 11 -5 -11 1.27 0.36 11 5 -11 1.94 0.44 11 5 -11 2.40 0.46 -9 -5 11 13.82 1.04 9 -5 -11 12.74 0.95 9 5 -11 11.70 0.93 9 5 -11 12.21 1.08 7 -5 -11 0.14 0.22 -7 -5 11 0.08 0.24 7 5 -11 0.54 0.27 7 5 -11 0.20 0.24 5 -5 -11 3.04 0.46 -5 -5 11 3.29 0.50 5 5 -11 2.78 0.53 5 5 -11 2.46 0.45 3 -5 -11 16.21 1.11 -3 -5 11 17.25 1.30 3 5 -11 18.59 1.40 3 5 -11 14.15 1.14 1 -5 -11 1.73 0.38 -1 -5 11 1.89 0.44 1 5 -11 3.00 0.58 1 5 -11 1.99 0.43 -1 5 -11 3.76 0.60 -10 -6 11 11.63 1.00 10 6 -11 11.34 0.92 8 -6 -11 3.25 0.51 -8 -6 11 3.63 0.59 8 6 -11 3.72 0.54 6 -6 -11 0.18 0.25 6 6 -11 0.59 0.27 4 -6 -11 1.39 0.36 4 6 -11 0.87 0.32 2 -6 -11 10.78 0.86 14 0 -12 10.10 0.84 12 0 -12 0.46 0.26 10 0 -12 4.76 0.53 8 0 -12 0.05 0.19 6 0 -12 10.04 0.76 2 0 -12 4.67 0.54 0 0 -12 2.59 0.45 -2 0 -12 0.38 0.28 13 -1 -12 4.55 0.53 13 1 -12 3.58 0.54 11 -1 -12 1.57 0.35 11 1 -12 1.78 0.39 9 -1 -12 6.44 0.61 9 1 -12 6.51 0.61 7 -1 -12 3.58 0.44 7 1 -12 2.78 0.51 7 1 -12 2.72 0.43 -5 -1 12 3.97 0.50 5 -1 -12 3.94 0.46 5 1 -12 4.56 0.48 5 1 -12 5.13 0.62 5 1 -12 3.68 0.47 -3 -1 12 2.66 0.46 3 1 -12 3.79 0.61 3 1 -12 2.73 0.45 -1 -1 12 5.08 0.59 1 1 -12 5.59 0.72 1 1 -12 4.61 0.57 1 -1 12 2.47 0.47 -1 -1 -12 2.75 0.47 -1 1 -12 4.06 0.58 -3 -1 -12 0.39 0.29 3 -1 12 0.57 0.31 14 2 -12 2.83 0.49 14 2 -12 3.41 0.57 12 -2 -12 3.08 0.49 12 2 -12 3.02 0.49 12 2 -12 2.87 0.52 10 -2 -12 6.22 0.64 10 2 -12 8.65 0.81 10 2 -12 8.37 0.70 8 -2 -12 6.04 0.58 8 2 -12 5.35 0.56 8 2 -12 5.95 0.67 8 2 -12 4.96 0.54 6 -2 -12 6.21 0.59 -6 -2 12 5.57 0.62 6 2 -12 6.55 0.59 6 2 -12 7.10 0.74 6 2 -12 6.25 0.60 4 -2 -12 1.11 0.30 -4 -2 12 0.74 0.28 4 2 -12 0.61 0.28 4 2 -12 0.95 0.36 -2 -2 12 4.57 0.57 2 2 -12 4.14 0.54 2 2 -12 5.59 0.70 0 -2 12 11.34 0.99 0 2 -12 11.52 0.95 -13 -3 12 2.39 0.45 13 3 -12 2.14 0.46 13 3 -12 1.94 0.43 -11 -3 12 1.20 0.35 11 -3 -12 0.58 0.29 11 3 -12 0.77 0.32 11 3 -12 0.31 0.26 9 -3 -12 8.85 0.78 9 3 -12 8.45 0.75 9 3 -12 10.64 0.93 9 3 -12 10.49 0.80 7 -3 -12 8.87 0.73 7 3 -12 8.47 0.84 7 3 -12 7.97 0.69 7 3 -12 7.26 0.69 -5 -3 12 3.04 0.48 5 -3 -12 2.89 0.45 5 3 -12 3.97 0.58 5 3 -12 3.53 0.47 -3 -3 12 0.52 0.27 3 -3 -12 0.29 0.23 3 3 -12 0.21 0.26 3 3 -12 0.29 0.28 -1 -3 12 15.34 1.24 1 3 -12 14.79 1.15 1 3 -12 18.19 1.42 -12 -4 12 1.91 0.43 -10 -4 12 3.41 0.55 10 -4 -12 2.90 0.49 10 4 -12 4.31 0.52 8 -4 -12 8.02 0.72 8 4 -12 8.99 0.74 8 4 -12 8.32 0.85 8 4 -12 7.34 0.70 -6 -4 12 3.54 0.52 6 -4 -12 3.01 0.48 6 4 -12 4.78 0.63 6 4 -12 3.34 0.50 -4 -4 12 3.62 0.53 4 -4 -12 3.74 0.48 4 4 -12 3.56 0.54 2 4 -12 0.47 0.29 9 5 -12 3.28 0.52 5 -5 -12 2.41 0.44 3 -5 -12 0.01 0.23 10 0 -13 0.83 0.31 8 0 -13 0.61 0.27 6 0 -13 1.47 0.35 9 -1 -13 1.53 0.37 9 1 -13 1.46 0.36 7 -1 -13 3.63 0.47 7 1 -13 3.25 0.48 3 1 -13 2.65 0.47 8 -2 -13 4.12 0.55 8 2 -13 6.16 0.71 8 2 -13 4.87 0.56 6 -2 -13 1.39 0.37 6 2 -13 1.09 0.33 6 2 -13 1.99 0.48 4 2 -13 3.35 0.52 9 3 -13 5.94 0.62 7 3 -13 2.98 0.48 5 -3 -13 0.38 0.26 0 0 0 0.00 0.00 ; _shelx_res_checksum 76345 _shelx_res_file ; TITL 61_32co in C2 CELL 0.71073 16.4467 8.3661 9.1549 90 107.642 90 ZERR 2 0.0003 0.0002 0.0002 0 0.001 0 LATT -7 SYMM -X,+Y,-Z SFAC C H Co N O UNIT 48 68 2 4 18 EQIV $1 1-X,+Y,1-Z DFIX 1.554 0.005 Ha H DFIX 0.995 0.005 O4 Ha O4 H DFIX 1.554 0.005 Ha Ha_$1 L.S. 10 PLAN 5 SIZE 0.24 0.256 0.39 TEMP -99.95 HTAB C6 O1 HTAB C6 O5 REM TRY 169 FINAL CC 86.84 TIME 5 SECS REM Fragments: 17 1 BOND $H HTAB CONF fmap 2 acta SHEL 999 0.7 REM Z:/CHE-XRAY-15P/B/B230/work/61_32co.hkl WGHT 0.054400 FVAR 0.17734 C1 1 0.405223 0.490192 0.782969 11.00000 0.01529 0.02000 = 0.02576 0.00040 0.00673 -0.00146 C2 1 0.338830 0.934301 0.862538 11.00000 0.01547 0.03353 = 0.02981 0.00654 0.00668 0.00957 H2A 2 0.301274 0.842930 0.843205 11.00000 -1.20000 H2B 2 0.312649 1.028380 0.805491 11.00000 -1.20000 C3 1 0.447921 0.988060 0.741078 11.00000 0.02031 0.03150 = 0.03222 0.01199 0.01001 0.00740 AFIX 23 H3A 2 0.463407 1.086599 0.803197 11.00000 -1.20000 H3B 2 0.408577 1.016604 0.639179 11.00000 -1.20000 AFIX 0 C4 1 0.526707 0.906826 0.724994 11.00000 0.01836 0.03145 = 0.02357 0.00778 0.00726 0.00474 AFIX 23 H4A 2 0.509731 0.815607 0.653297 11.00000 -1.20000 H4B 2 0.559324 0.983116 0.681797 11.00000 -1.20000 AFIX 0 C5 1 0.627284 0.983828 0.971105 11.00000 0.02247 0.02057 = 0.03317 -0.00263 0.01234 -0.00633 AFIX 23 H5A 2 0.587916 1.075491 0.961288 11.00000 -1.20000 H5B 2 0.675220 1.018162 0.934159 11.00000 -1.20000 AFIX 0 C6 1 0.642184 0.724393 0.851908 11.00000 0.01413 0.01941 = 0.02721 0.00125 0.00890 -0.00124 AFIX 23 H6A 2 0.608684 0.628671 0.806229 11.00000 -1.20000 H6B 2 0.680762 0.692908 0.953561 11.00000 -1.20000 AFIX 0 C7 1 0.696545 0.772080 0.751591 11.00000 0.01185 0.01991 = 0.02232 0.00003 0.00542 -0.00087 C8 1 0.673314 0.721884 0.599370 11.00000 0.01458 0.02410 = 0.02389 -0.00205 0.00330 -0.00306 AFIX 43 H8 2 0.621407 0.665165 0.557528 11.00000 -1.20000 AFIX 0 C9 1 0.725252 0.753869 0.508002 11.00000 0.02239 0.02657 = 0.01985 -0.00454 0.00444 -0.00337 AFIX 43 H9 2 0.709144 0.717746 0.404797 11.00000 -1.20000 AFIX 0 C10 1 0.800359 0.838274 0.567390 11.00000 0.02025 0.02504 = 0.02137 -0.00080 0.00884 -0.00212 AFIX 43 H10 2 0.835664 0.860198 0.504678 11.00000 -1.20000 AFIX 0 C11 1 0.824563 0.891476 0.719270 11.00000 0.01281 0.01912 = 0.02109 -0.00045 0.00551 -0.00098 C12 1 0.772713 0.856500 0.810765 11.00000 0.01285 0.02047 = 0.01937 -0.00097 0.00526 -0.00121 AFIX 43 H12 2 0.789444 0.890554 0.914634 11.00000 -1.20000 AFIX 0 CO1 3 0.500000 0.729940 1.000000 10.50000 0.00956 0.01699 = 0.02051 0.00000 0.00464 0.00000 N1 4 0.581473 0.848623 0.875857 11.00000 0.01332 0.01938 = 0.02379 0.00183 0.00570 0.00042 O1 5 0.457412 0.499416 0.709506 11.00000 0.02244 0.04307 = 0.03364 -0.00886 0.01582 -0.01151 O2 5 0.411696 0.560763 0.907857 11.00000 0.01727 0.02576 = 0.02913 -0.00825 0.00897 -0.00610 O3 5 0.409071 0.874784 0.815814 11.00000 0.01583 0.02690 = 0.02660 0.00542 0.00776 0.00602 AFIX 6 O4 5 0.500000 0.301146 0.500000 10.50000 0.03747 0.05621 = 0.04553 0.00000 0.02277 0.00000 PART -1 H 2 0.456199 0.288376 0.414872 10.50000 -1.50000 HA 2 0.535932 0.342509 0.461197 10.50000 -1.50000 AFIX 0 PART 0 O5 5 0.624699 0.316272 0.800375 11.00000 0.07596 0.05755 = 0.08380 0.01521 0.00569 0.00715 HKLF 4 REM 61_32co in C2 REM R1 = 0.0342 for 3360 Fo > 4sig(Fo) and 0.0346 for all 3413 data REM 173 parameters refined using 5 restraints END WGHT 0.0537 0.0000 REM Instructions for potential hydrogen bonds HTAB C6 O1 HTAB C6 O5 REM Highest difference peak 0.844, deepest hole -0.384, 1-sigma level 0.086 Q1 1 0.5083 0.7893 1.0672 11.00000 0.05 0.84 Q2 1 0.5092 0.6662 1.0591 11.00000 0.05 0.83 Q3 1 0.5312 0.7295 0.9807 11.00000 0.05 0.53 Q4 1 0.6889 0.7473 0.6828 11.00000 0.05 0.47 Q5 1 0.7028 0.7276 0.5655 11.00000 0.05 0.44 ; _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. ; _shelxl_version_number 2012-4