# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_wk _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H48 Co2 N16 O44 Si W12' _chemical_formula_sum 'C48 H48 Co2 N16 O44 Si W12' _chemical_formula_weight 3905.14 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' 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' Si Si 0.0817 0.0704 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_H-M_alt 'P 1' _space_group_name_Hall 'P 1' _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' _cell_length_a 12.401(5) _cell_length_b 13.345(5) _cell_length_c 13.370(5) _cell_angle_alpha 62.968(4) _cell_angle_beta 89.294(5) _cell_angle_gamma 70.227(4) _cell_volume 1828.1(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 3.540 _exptl_crystal_F_000 1748.0 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_absorpt_coefficient_mu 19.356 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.006 _exptl_absorpt_correction_T_max 0.014 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14930 _diffrn_reflns_av_unetI/netI 0.0760 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.254 _diffrn_reflns_theta_max 28.335 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.682 _diffrn_reflns_point_group_measured_fraction_full 0.726 _reflns_number_total 18274 _reflns_number_gt 11969 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.417 _reflns_Friedel_fraction_max 0.401 _reflns_Friedel_fraction_full 0.463 _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-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems. These atoms are as follows: O12 O25 O33 N7 C40 C43 O6 O28 N12 C10 C14 C15 C47 O17 Si1 O42 N8 C17 O39 C18 and O25. This refinement led to the relative high restraint value 123. However, the number cannot be dramatically decreased in oder to fit for the reasonable Ueq values of these non-H atoms. ; _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^)+(0.0780P)^2^+21.3801P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3397 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.495(12) _chemical_absolute_configuration ? _refine_ls_number_reflns 18274 _refine_ls_number_parameters 1103 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 W1 W 0.64802(8) -0.34553(7) 0.60085(7) 0.0176(2) Uani 1 1 d . . . . . W2 W 0.36881(8) -0.54636(7) 0.66468(7) 0.01514(19) Uani 1 1 d . . . . . W3 W 0.37923(7) 0.00561(7) 0.23611(6) 0.01183(17) Uani 1 1 d . . . . . W4 W 0.14454(9) 0.00160(8) 0.40437(9) 0.0229(2) Uani 1 1 d . . . . . W5 W 0.60186(8) -0.25839(8) 0.29470(8) 0.0180(2) Uani 1 1 d . . . . . W6 W 0.33609(8) -0.19623(8) 0.16600(7) 0.0179(2) Uani 1 1 d . . . . . W7 W 0.13082(9) -0.26043(9) 0.60085(8) 0.0204(2) Uani 1 1 d . . . . . W8 W 0.31664(8) -0.47576(8) 0.38771(8) 0.0186(2) Uani 1 1 d . . . . . W9 W 0.43716(8) -0.07465(7) 0.53613(8) 0.0172(2) Uani 1 1 d . . . . . W10 W 0.08829(7) -0.18054(8) 0.31847(7) 0.0171(2) Uani 1 1 d . . . . . W11 W 0.41929(8) -0.33177(8) 0.74071(7) 0.0183(2) Uani 1 1 d . . . . . W12 W 0.58795(9) -0.54456(8) 0.50910(8) 0.0218(2) Uani 1 1 d . . . . . Si1 Si 0.3695(5) -0.2659(5) 0.4552(5) 0.0066(8) Uani 1 1 d . U . . . Co1 Co 0.2681(3) 0.3493(3) 0.1115(3) 0.0200(6) Uani 1 1 d . . . . . Co2 Co 0.4830(3) 1.1017(3) -0.2133(3) 0.0265(8) Uani 1 1 d . . . . . C1 C -0.296(3) 0.005(3) 0.276(3) 0.040(7) Uani 1 1 d . . . . . H1A H -0.3406 0.0090 0.2179 0.048 Uiso 1 1 calc R U . . . C2 C 0.938(3) 1.528(3) -0.530(2) 0.034(7) Uani 1 1 d . . . . . H2A H 0.9096 1.5735 -0.6083 0.041 Uiso 1 1 calc R U . . . C3 C 1.090(2) 1.125(2) -0.063(2) 0.027(6) Uani 1 1 d . . . . . H3A H 1.1561 1.0855 -0.0076 0.033 Uiso 1 1 calc R U . . . C4 C 1.034(3) 1.464(3) -0.364(3) 0.036(7) Uani 1 1 d . . . . . H4A H 1.0810 1.4592 -0.3072 0.043 Uiso 1 1 calc R U . . . C5 C -0.146(2) 0.212(3) 0.133(2) 0.034(7) Uani 1 1 d . . . . . H5A H -0.0782 0.1685 0.1873 0.041 Uiso 1 1 calc R U . . . C6 C -0.187(2) 0.048(2) 0.362(2) 0.031(6) Uani 1 1 d . . . . . H6A H -0.1417 0.0851 0.3764 0.037 Uiso 1 1 calc R U . . . C7 C 1.0822(19) 1.2208(19) -0.161(2) 0.024(5) Uani 1 1 d . . . . . H7A H 1.1453 1.2451 -0.1746 0.029 Uiso 1 1 calc R U . . . C8 C 0.911(2) 1.432(2) -0.454(2) 0.025(5) Uani 1 1 d . . . . . H8A H 0.8594 1.4015 -0.4686 0.030 Uiso 1 1 calc R U . . . C9 C -0.250(2) 0.376(2) -0.053(2) 0.028(6) Uani 1 1 d . . . . . H9A H -0.2555 0.4450 -0.1207 0.033 Uiso 1 1 calc R U . . . C10 C 0.059(2) 0.446(2) -0.074(2) 0.025(5) Uani 1 1 d . U . . . H10A H 0.0868 0.5023 -0.1261 0.030 Uiso 1 1 calc R U . . . C11 C -0.344(2) 0.239(2) 0.0732(19) 0.024(5) Uani 1 1 d . . . . . H11A H -0.4077 0.2155 0.0886 0.028 Uiso 1 1 calc R U . . . C12 C -0.275(3) -0.073(3) 0.388(3) 0.036(7) Uani 1 1 d . . . . . H12A H -0.3022 -0.1357 0.4215 0.043 Uiso 1 1 calc R U . . . C13 C -0.341(3) 0.335(3) -0.033(3) 0.043(8) Uani 1 1 d . . . . . H13A H -0.4041 0.3722 -0.0911 0.051 Uiso 1 1 calc R U . . . C14 C 0.995(2) 1.085(2) -0.044(2) 0.025(5) Uani 1 1 d . U . . . H14A H 1.0010 1.0137 0.0212 0.030 Uiso 1 1 calc R U . . . C15 C 0.785(2) 1.021(2) -0.002(2) 0.025(5) Uani 1 1 d . U . . . H15A H 0.8364 0.9738 0.0667 0.030 Uiso 1 1 calc R U . . . C16 C -0.1517(19) 0.3116(18) 0.0303(19) 0.019(5) Uani 1 1 d . . . . . C17 C -0.047(2) 0.441(2) -0.091(2) 0.024(5) Uani 1 1 d . U . . . H17A H -0.1029 0.4900 -0.1565 0.028 Uiso 1 1 calc R U . . . C18 C 0.8892(19) 1.2542(18) -0.2249(18) 0.015(4) Uani 1 1 d . U . . . H18A H 0.8221 1.2998 -0.2796 0.018 Uiso 1 1 calc R U . . . C19 C 0.8915(18) 1.1551(19) -0.1258(19) 0.017(4) Uani 1 1 d . . . . . C20 C -0.239(2) 0.181(2) 0.153(2) 0.024(5) Uani 1 1 d . . . . . C21 C 0.9824(18) 1.2866(18) -0.2445(19) 0.016(4) Uani 1 1 d . . . . . C22 C -0.067(2) 0.909(2) -0.204(3) 0.033(6) Uani 1 1 d . . . . . H22A H -0.1210 0.8745 -0.1756 0.039 Uiso 1 1 calc R U . . . C23 C -0.098(2) 1.022(2) -0.305(2) 0.027(6) Uani 1 1 d . . . . . H23A H -0.1743 1.0612 -0.3445 0.033 Uiso 1 1 calc R U . . . C24 C 0.045(2) 0.854(2) -0.151(2) 0.021(5) Uani 1 1 d . . . . . C25 C -0.014(2) 1.075(2) -0.346(2) 0.028(6) Uani 1 1 d . . . . . H25A H -0.0328 1.1475 -0.4129 0.034 Uiso 1 1 calc R U . . . C26 C 0.0949(19) 1.0163(17) -0.285(2) 0.018(5) Uani 1 1 d . . . . . C27 C 0.125(2) 0.902(2) -0.185(2) 0.023(5) Uani 1 1 d . . . . . H27A H 0.2007 0.8612 -0.1445 0.028 Uiso 1 1 calc R U . . . C28 C 0.2739(19) 1.047(2) -0.2435(19) 0.022(5) Uani 1 1 d . . . . . H28A H 0.3011 0.9810 -0.1708 0.026 Uiso 1 1 calc R U . . . C29 C 0.167(2) 1.1754(19) -0.407(2) 0.022(5) Uani 1 1 d . . . . . H29A H 0.1075 1.2180 -0.4698 0.026 Uiso 1 1 calc R U . . . C30 C 0.682(2) 1.019(2) -0.0244(19) 0.026(5) Uani 1 1 d . . . . . H30A H 0.6488 0.9693 0.0287 0.031 Uiso 1 1 calc R U . . . C31 C 0.259(2) 1.207(2) -0.395(2) 0.024(5) Uani 1 1 d . . . . . H31A H 0.2749 1.2719 -0.4495 0.029 Uiso 1 1 calc R U . . . C32 C 0.697(2) 1.155(2) -0.179(2) 0.026(5) Uani 1 1 d . . . . . H32A H 0.6796 1.2192 -0.2528 0.032 Uiso 1 1 calc R U . . . C33 C 0.712(3) 0.751(3) -0.141(3) 0.042(7) Uani 1 1 d . . . . . H33A H 0.7742 0.6983 -0.1538 0.050 Uiso 1 1 calc R U . . . C34 C 0.164(3) 0.634(2) -0.037(2) 0.028(6) Uani 1 1 d . . . . . H34A H 0.2116 0.6303 -0.0905 0.034 Uiso 1 1 calc R U . . . C35 C 0.045(2) 0.301(2) 0.081(2) 0.026(6) Uani 1 1 d . . . . . H35A H 0.0597 0.2392 0.1560 0.031 Uiso 1 1 calc R U . . . C36 C 0.462(2) 0.4233(19) 0.1498(18) 0.018(5) Uani 1 1 d . . . . . H36A H 0.4325 0.4938 0.0802 0.022 Uiso 1 1 calc R U . . . C37 C 0.638(2) 0.454(2) 0.1883(19) 0.021(5) Uani 1 1 d . . . . . C38 C 0.614(2) 0.558(2) 0.095(2) 0.021(5) Uani 1 1 d . . . . . H38A H 0.5391 0.5968 0.0526 0.026 Uiso 1 1 calc R U . . . C39 C 0.094(3) 0.583(2) 0.115(2) 0.035(7) Uani 1 1 d . . . . . H39A H 0.0797 0.5364 0.1866 0.042 Uiso 1 1 calc R U . . . C40 C 0.748(2) 0.396(2) 0.255(2) 0.024(5) Uani 1 1 d . U . . . H40A H 0.7665 0.3244 0.3233 0.028 Uiso 1 1 calc R U . . . C41 C 0.832(3) 0.451(3) 0.217(3) 0.040(7) Uani 1 1 d . . . . . H41A H 0.9055 0.4134 0.2604 0.048 Uiso 1 1 calc R U . . . C42 C 0.693(3) 0.612(2) 0.057(2) 0.027(6) Uani 1 1 d . . . . . C43 C 0.483(2) 0.253(2) 0.298(2) 0.024(5) Uani 1 1 d . U . . . H43A H 0.4685 0.1847 0.3469 0.029 Uiso 1 1 calc R U . . . C44 C 0.808(2) 0.549(3) 0.125(3) 0.042(8) Uani 1 1 d . . . . . H44A H 0.8654 0.5811 0.1007 0.051 Uiso 1 1 calc R U . . . C45 C 0.033(3) 0.709(3) 0.047(3) 0.037(7) Uani 1 1 d . . . . . H45A H -0.0245 0.7620 0.0647 0.045 Uiso 1 1 calc R U . . . C46 C 0.571(2) 0.281(2) 0.320(2) 0.027(6) Uani 1 1 d . . . . . H46A H 0.6282 0.2367 0.3846 0.032 Uiso 1 1 calc R U . . . C47 C 0.575(2) 0.828(2) -0.064(2) 0.028(5) Uani 1 1 d . U . . . H47A H 0.5257 0.8330 -0.0122 0.034 Uiso 1 1 calc R U . . . C48 C 0.656(3) 0.866(3) -0.211(2) 0.032(6) Uani 1 1 d . . . . . H48A H 0.6723 0.9074 -0.2827 0.039 Uiso 1 1 calc R U . . . O1 O 0.3363(19) 0.4001(19) -0.0444(18) 0.038(5) Uani 1 1 d . . . . . O2 O 0.5180(14) -0.6233(15) 0.6443(15) 0.025(4) Uani 1 1 d . . . . . O3 O 0.2312(12) -0.1987(13) 0.4505(12) 0.016(3) Uani 1 1 d . . . . . O4 O 0.4499(16) 0.0438(14) 0.5479(13) 0.024(4) Uani 1 1 d . . . . . O5 O 0.6031(14) -0.4170(13) 0.3790(12) 0.021(3) Uani 1 1 d . . . . . O6 O 0.3510(14) -0.3551(13) 0.2582(12) 0.019(3) Uani 1 1 d . U . . . O7 O 0.4424(13) -0.2536(12) 0.5504(12) 0.014(3) Uani 1 1 d . . . . . O8 O 0.4259(13) -0.4734(14) 0.7345(14) 0.021(3) Uani 1 1 d . . . . . O9 O 0.3980(12) -0.4038(12) 0.4917(12) 0.015(3) Uani 1 1 d . . . . . O10 O 0.2352(14) 0.0323(13) 0.2858(13) 0.019(3) Uani 1 1 d . . . . . O11 O 0.4051(13) -0.1979(12) 0.3315(12) 0.015(3) Uani 1 1 d . . . . . O12 O 0.4437(15) -0.0238(15) 0.3822(13) 0.021(3) Uani 1 1 d . U . . . O13 O 0.4992(14) -0.2396(14) 0.1758(14) 0.023(4) Uani 1 1 d . . . . . O14 O 0.2190(14) -0.4179(15) 0.6331(14) 0.022(3) Uani 1 1 d . . . . . O15 O 0.0392(18) -0.2351(15) 0.4709(14) 0.031(5) Uani 1 1 d . . . . . O16 O 0.1887(13) -0.1445(13) 0.2112(13) 0.020(3) Uani 1 1 d . . . . . O17 O 0.3295(13) -0.0312(13) 0.1279(13) 0.018(3) Uani 1 1 d . U . . . O18 O 0.0332(16) -0.2803(17) 0.6929(15) 0.026(4) Uani 1 1 d . . . . . O19 O 0.4194(13) -0.1731(13) 0.6932(13) 0.018(3) Uani 1 1 d . . . . . O20 O 0.1775(13) -0.3492(13) 0.3701(13) 0.019(3) Uani 1 1 d . . . . . O21 O 0.4812(14) -0.5647(16) 0.4269(14) 0.023(4) Uani 1 1 d . . . . . O22 O 0.5836(14) -0.3829(12) 0.7386(13) 0.021(3) Uani 1 1 d . . . . . O23 O 0.3073(15) -0.5648(17) 0.5462(16) 0.028(4) Uani 1 1 d . . . . . O24 O 0.6460(17) -0.2701(13) 0.4376(14) 0.024(4) Uani 1 1 d . . . . . O25 O 0.7267(17) -0.2699(17) 0.2402(16) 0.031(4) Uani 1 1 d . U . . . O26 O 0.3025(18) -0.1689(15) 0.0319(14) 0.027(4) Uani 1 1 d . . . . . O27 O 0.2713(14) -0.0215(14) 0.4980(13) 0.021(3) Uani 1 1 d . . . . . O28 O 0.0526(15) 0.1489(14) 0.3671(14) 0.025(4) Uani 1 1 d . U . . . O29 O 0.7080(15) -0.6698(14) 0.5394(15) 0.025(4) Uani 1 1 d . . . . . O30 O 0.7920(15) -0.3938(15) 0.6573(14) 0.023(4) Uani 1 1 d . . . . . O31 O 0.4240(17) -0.3830(16) 0.8845(13) 0.026(4) Uani 1 1 d . . . . . O32 O 0.0784(14) -0.0819(13) 0.5294(13) 0.021(3) Uani 1 1 d . . . . . O33 O 0.3652(15) 0.1545(13) 0.1505(14) 0.023(3) Uani 1 1 d . U . . . O34 O 0.5356(14) -0.0818(13) 0.2280(13) 0.020(3) Uani 1 1 d . . . . . O35 O 0.0497(15) -0.0222(14) 0.3102(14) 0.023(4) Uani 1 1 d . . . . . O36 O 0.6384(16) -0.4782(15) 0.5952(14) 0.026(4) Uani 1 1 d . . . . . O37 O 0.5988(15) -0.1789(13) 0.5789(13) 0.020(3) Uani 1 1 d . . . . . O38 O -0.0332(14) -0.1549(14) 0.2410(13) 0.020(3) Uani 1 1 d . . . . . O39 O 0.2744(15) -0.5579(15) 0.3421(15) 0.024(3) Uani 1 1 d . U . . . O40 O 0.2095(18) 0.2951(19) 0.2755(15) 0.030(4) Uani 1 1 d . . . . . O41 O 0.5356(17) 1.1643(16) -0.3741(16) 0.026(4) Uani 1 1 d . . . . . O42 O 0.3535(17) -0.6659(17) 0.7846(17) 0.032(4) Uani 1 1 d . U . . . O43 O 0.4106(19) 1.0858(18) -0.0643(16) 0.035(5) Uani 1 1 d . . . . . O44 O 0.2560(14) -0.2672(14) 0.6878(14) 0.023(3) Uiso 1 1 d . . . . . N1 N 0.566(2) 0.9198(19) -0.1640(19) 0.026(5) Uani 1 1 d . . . . . N2 N 0.3215(18) 1.1234(19) -0.2888(18) 0.023(4) Uani 1 1 d . . . . . N3 N 0.1781(18) 1.0727(17) -0.3130(16) 0.019(4) Uani 1 1 d . . . . . N4 N 0.0801(18) 0.7343(18) -0.0518(18) 0.022(4) Uani 1 1 d . . . . . N5 N 0.9784(17) 1.3894(18) -0.3480(19) 0.023(4) Uani 1 1 d . . . . . N6 N -0.2360(17) 0.0794(17) 0.2649(18) 0.020(4) Uani 1 1 d . . . . . N7 N 0.7993(16) 1.1121(16) -0.1047(14) 0.015(4) Uani 1 1 d . U . . . N8 N -0.0544(16) 0.3500(15) 0.0068(15) 0.014(3) Uani 1 1 d . U . . . N9 N 1.013(2) 1.545(2) -0.472(2) 0.040(6) Uani 1 1 d . . . . . N10 N 0.1181(17) 0.3548(16) 0.0320(17) 0.019(4) Uani 1 1 d . . . . . N11 N -0.209(3) -0.046(3) 0.443(3) 0.066(11) Uani 1 1 d . . . . . N12 N 0.5591(16) 0.3927(16) 0.2208(15) 0.015(4) Uani 1 1 d . U . . . N13 N 0.4151(18) 0.3400(16) 0.1925(16) 0.020(4) Uani 1 1 d . . . . . N14 N 0.6628(19) 0.7240(19) -0.0452(18) 0.027(5) Uani 1 1 d . . . . . N15 N 0.173(2) 0.5405(19) 0.0621(17) 0.027(5) Uani 1 1 d . . . . . N16 N 0.631(2) 1.0993(17) -0.1367(16) 0.023(5) 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 W1 0.0133(4) 0.0160(4) 0.0131(4) 0.0021(3) -0.0076(3) -0.0063(3) W2 0.0201(4) 0.0106(3) 0.0097(4) 0.0003(3) -0.0037(3) -0.0071(3) W3 0.0172(4) 0.0082(3) 0.0056(4) 0.0009(3) -0.0027(3) -0.0054(3) W4 0.0245(5) 0.0162(4) 0.0208(5) -0.0061(4) -0.0055(4) -0.0029(4) W5 0.0180(4) 0.0244(4) 0.0123(4) -0.0084(4) 0.0013(3) -0.0093(3) W6 0.0233(5) 0.0187(4) 0.0057(4) -0.0026(3) -0.0027(3) -0.0055(3) W7 0.0214(5) 0.0293(5) 0.0133(4) -0.0089(4) 0.0033(3) -0.0146(4) W8 0.0206(4) 0.0139(4) 0.0227(5) -0.0090(3) -0.0012(3) -0.0075(3) W9 0.0217(5) 0.0141(4) 0.0193(5) -0.0084(3) 0.0016(3) -0.0098(3) W10 0.0133(4) 0.0161(4) 0.0119(4) 0.0021(3) -0.0074(3) -0.0062(3) W11 0.0221(4) 0.0196(4) 0.0062(4) -0.0007(3) -0.0016(3) -0.0073(3) W12 0.0220(5) 0.0123(4) 0.0234(5) -0.0057(4) -0.0081(4) -0.0012(3) Si1 0.0069(12) 0.0059(12) 0.0063(12) -0.0019(9) -0.0016(9) -0.0029(9) Co1 0.0232(15) 0.0210(14) 0.0110(14) 0.0004(12) -0.0016(11) -0.0141(12) Co2 0.0264(17) 0.0305(16) 0.0174(16) 0.0002(13) -0.0041(13) -0.0210(14) C1 0.042(17) 0.038(15) 0.06(2) -0.025(15) 0.021(15) -0.035(14) C2 0.053(18) 0.040(14) 0.022(13) -0.007(11) 0.008(12) -0.044(14) C3 0.007(10) 0.036(13) 0.033(14) -0.013(11) 0.003(9) -0.006(9) C4 0.032(15) 0.048(16) 0.038(16) -0.016(14) -0.003(12) -0.032(13) C5 0.017(11) 0.043(15) 0.023(13) -0.007(11) -0.011(9) -0.002(10) C6 0.015(11) 0.025(11) 0.038(15) 0.002(11) 0.003(10) -0.013(9) C7 0.005(9) 0.011(9) 0.035(14) 0.001(9) -0.003(9) 0.003(7) C8 0.016(11) 0.027(12) 0.027(13) -0.014(10) -0.006(9) -0.002(9) C9 0.016(11) 0.020(10) 0.034(14) -0.010(10) -0.011(10) 0.005(9) C10 0.027(9) 0.022(8) 0.020(9) 0.000(7) 0.001(7) -0.016(7) C11 0.031(13) 0.032(12) 0.011(10) -0.006(9) -0.002(9) -0.023(10) C12 0.030(15) 0.035(14) 0.044(17) -0.011(13) 0.007(12) -0.024(12) C13 0.028(14) 0.039(15) 0.029(15) -0.001(13) -0.023(12) 0.003(12) C14 0.017(9) 0.023(9) 0.021(9) -0.003(7) -0.004(7) -0.002(7) C15 0.024(9) 0.023(8) 0.017(9) 0.002(7) 0.002(7) -0.013(7) C16 0.016(10) 0.011(8) 0.014(10) 0.005(8) -0.007(8) -0.002(8) C17 0.024(5) 0.024(5) 0.024(5) -0.011(3) 0.0038(15) -0.009(2) C18 0.015(4) 0.015(4) 0.015(4) -0.007(2) 0.0021(14) -0.0057(19) C19 0.011(9) 0.016(9) 0.019(11) -0.006(8) -0.005(8) -0.002(8) C20 0.026(12) 0.026(11) 0.028(13) -0.016(10) 0.004(10) -0.016(10) C21 0.011(9) 0.011(8) 0.018(11) -0.002(8) 0.004(8) 0.000(7) C22 0.029(14) 0.018(11) 0.038(16) -0.003(11) 0.010(11) -0.009(10) C23 0.018(11) 0.026(11) 0.038(15) -0.018(11) -0.006(10) -0.004(9) C24 0.018(11) 0.029(11) 0.023(12) -0.019(10) 0.008(9) -0.007(9) C25 0.021(12) 0.025(11) 0.034(14) -0.004(10) 0.002(10) -0.018(10) C26 0.015(10) 0.004(8) 0.033(13) -0.006(8) 0.007(9) -0.005(7) C27 0.034(13) 0.013(9) 0.016(11) 0.001(9) -0.004(9) -0.012(9) C28 0.012(10) 0.031(12) 0.011(10) 0.000(9) -0.005(8) -0.008(9) C29 0.030(13) 0.009(8) 0.015(11) 0.005(8) -0.004(9) -0.009(9) C30 0.037(14) 0.034(13) 0.002(9) 0.000(9) 0.000(9) -0.018(11) C31 0.028(13) 0.014(9) 0.020(12) 0.000(9) -0.006(10) -0.008(9) C32 0.032(13) 0.019(10) 0.011(11) 0.005(9) -0.003(9) -0.009(10) C33 0.042(18) 0.041(16) 0.039(17) -0.016(14) 0.020(14) -0.017(14) C34 0.036(14) 0.015(10) 0.020(12) 0.003(9) -0.009(10) -0.010(10) C35 0.022(11) 0.021(10) 0.022(12) 0.004(9) -0.010(9) -0.014(9) C36 0.027(12) 0.013(9) 0.008(9) 0.004(8) -0.003(8) -0.012(8) C37 0.015(10) 0.037(12) 0.012(10) -0.011(10) -0.005(8) -0.009(9) C38 0.019(11) 0.028(11) 0.014(11) -0.007(9) 0.002(8) -0.010(9) C39 0.034(15) 0.027(13) 0.023(13) 0.002(11) 0.007(11) -0.008(11) C40 0.023(9) 0.020(8) 0.020(9) -0.005(7) -0.011(7) -0.005(7) C41 0.032(15) 0.033(14) 0.042(18) -0.010(13) 0.012(13) -0.011(12) C42 0.041(15) 0.013(9) 0.019(12) -0.002(9) -0.005(10) -0.010(10) C43 0.024(9) 0.015(8) 0.019(9) -0.002(7) -0.001(7) -0.002(7) C44 0.012(12) 0.052(18) 0.06(2) -0.029(17) -0.005(12) -0.010(12) C45 0.046(18) 0.037(14) 0.030(15) -0.013(13) 0.010(12) -0.021(13) C46 0.027(13) 0.020(11) 0.029(13) -0.012(10) -0.003(10) -0.002(9) C47 0.022(9) 0.028(9) 0.031(10) -0.010(8) 0.019(8) -0.011(7) C48 0.032(14) 0.034(13) 0.028(14) -0.003(11) 0.010(11) -0.025(11) O1 0.039(12) 0.041(11) 0.034(11) -0.016(9) 0.012(9) -0.020(9) O2 0.014(8) 0.023(8) 0.026(9) -0.005(7) -0.004(6) 0.000(6) O3 0.010(7) 0.018(7) 0.016(7) -0.009(6) 0.006(5) -0.001(5) O4 0.040(10) 0.022(7) 0.012(8) -0.007(6) -0.004(7) -0.016(7) O5 0.027(8) 0.014(6) 0.010(7) -0.001(6) -0.007(6) -0.002(6) O6 0.022(7) 0.016(6) 0.008(6) 0.002(5) -0.003(5) -0.004(5) O7 0.018(7) 0.014(6) 0.008(6) -0.004(5) -0.006(5) -0.004(5) O8 0.016(7) 0.021(7) 0.022(8) -0.005(6) -0.005(6) -0.012(6) O9 0.013(7) 0.015(6) 0.015(7) -0.005(6) -0.003(5) -0.008(5) O10 0.020(8) 0.018(7) 0.013(7) -0.005(6) -0.003(6) -0.002(6) O11 0.015(7) 0.008(6) 0.007(6) 0.004(5) -0.003(5) 0.001(5) O12 0.028(7) 0.030(7) 0.008(6) -0.012(6) 0.000(5) -0.009(6) O13 0.022(8) 0.024(8) 0.024(9) -0.013(7) -0.006(7) -0.008(6) O14 0.018(8) 0.030(8) 0.026(9) -0.017(7) 0.000(6) -0.012(6) O15 0.059(13) 0.024(8) 0.014(8) -0.003(7) -0.005(8) -0.029(9) O16 0.014(7) 0.021(7) 0.020(8) -0.008(6) -0.006(6) 0.000(6) O17 0.018(3) 0.018(3) 0.018(3) -0.0090(18) 0.0022(13) -0.0069(16) O18 0.029(9) 0.036(9) 0.021(8) -0.014(7) 0.012(7) -0.022(8) O19 0.017(7) 0.019(7) 0.019(8) -0.005(6) -0.001(6) -0.013(6) O20 0.014(7) 0.013(6) 0.022(8) -0.006(6) -0.004(6) 0.000(5) O21 0.016(7) 0.047(10) 0.025(9) -0.031(8) 0.008(6) -0.014(7) O22 0.027(8) 0.008(6) 0.015(7) 0.005(6) -0.003(6) -0.008(6) O23 0.020(8) 0.037(9) 0.031(9) -0.021(8) -0.004(7) -0.009(7) O24 0.046(11) 0.013(7) 0.012(7) 0.000(6) -0.001(7) -0.017(7) O25 0.030(5) 0.031(4) 0.030(5) -0.015(3) 0.008(2) -0.011(3) O26 0.043(11) 0.020(7) 0.013(8) -0.009(7) -0.003(7) -0.003(7) O27 0.026(8) 0.027(8) 0.012(7) -0.012(6) 0.000(6) -0.009(7) O28 0.027(8) 0.012(6) 0.017(7) -0.006(6) -0.002(6) 0.014(6) O29 0.017(8) 0.013(7) 0.025(9) 0.000(6) -0.006(6) 0.004(6) O30 0.022(8) 0.022(8) 0.019(8) -0.004(7) -0.007(6) -0.008(6) O31 0.037(10) 0.029(8) 0.004(7) -0.002(6) 0.002(6) -0.011(7) O32 0.022(8) 0.014(7) 0.014(7) 0.001(6) -0.003(6) -0.004(6) O33 0.028(7) 0.013(6) 0.015(7) 0.006(5) 0.002(5) -0.012(5) O34 0.024(8) 0.015(7) 0.016(8) -0.008(6) 0.001(6) -0.004(6) O35 0.026(9) 0.022(7) 0.015(8) -0.004(6) -0.005(6) -0.011(7) O36 0.038(10) 0.023(8) 0.015(8) -0.006(7) -0.006(7) -0.015(7) O37 0.033(9) 0.018(7) 0.016(7) -0.011(6) -0.005(6) -0.012(6) O38 0.021(8) 0.017(7) 0.013(7) -0.002(6) -0.004(6) -0.005(6) O39 0.024(4) 0.024(4) 0.025(4) -0.012(3) 0.001(2) -0.011(3) O40 0.041(11) 0.050(11) 0.022(9) -0.023(9) 0.013(8) -0.036(9) O41 0.029(9) 0.026(8) 0.027(9) -0.008(7) 0.009(7) -0.020(7) O42 0.032(5) 0.031(5) 0.033(5) -0.013(3) 0.004(2) -0.014(3) O43 0.037(11) 0.036(10) 0.020(9) -0.006(8) 0.007(8) -0.010(8) N1 0.027(11) 0.022(9) 0.024(11) -0.004(9) 0.008(8) -0.013(8) N2 0.020(10) 0.030(10) 0.026(11) -0.016(9) 0.001(8) -0.014(8) N3 0.023(10) 0.017(8) 0.014(9) -0.006(7) -0.003(7) -0.007(7) N4 0.025(10) 0.021(9) 0.022(10) -0.005(8) 0.004(8) -0.020(8) N5 0.017(9) 0.020(9) 0.028(11) -0.007(8) -0.007(8) -0.009(7) N6 0.015(9) 0.018(8) 0.028(10) -0.011(8) 0.008(8) -0.007(7) N7 0.014(7) 0.016(7) 0.006(7) 0.005(5) -0.001(5) -0.009(6) N8 0.014(4) 0.014(3) 0.014(3) -0.0065(19) 0.0017(13) -0.0054(17) N9 0.043(15) 0.035(12) 0.041(15) -0.002(11) 0.005(11) -0.036(12) N10 0.019(9) 0.015(8) 0.025(10) -0.008(8) 0.002(7) -0.013(7) N11 0.039(16) 0.052(17) 0.051(19) 0.014(15) 0.016(14) -0.010(14) N12 0.019(7) 0.016(7) 0.009(7) -0.001(6) 0.005(6) -0.012(6) N13 0.028(10) 0.014(8) 0.015(9) 0.000(7) -0.001(8) -0.015(7) N14 0.029(11) 0.024(10) 0.021(10) -0.013(9) -0.003(8) 0.000(8) N15 0.038(12) 0.026(10) 0.006(9) 0.004(8) -0.004(8) -0.017(9) N16 0.036(12) 0.018(9) 0.007(9) 0.000(7) -0.007(8) -0.008(8) _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 W1 O30 1.728(16) . ? W1 O36 1.849(16) . ? W1 O22 1.918(18) . ? W1 O24 1.940(17) . ? W1 O37 1.974(14) . ? W1 O7 2.373(14) . ? W2 O42 1.74(2) . ? W2 O2 1.873(17) . ? W2 O8 1.905(15) . ? W2 O23 1.914(17) . ? W2 O14 1.943(16) . ? W2 O9 2.355(15) . ? W3 O33 1.729(14) . ? W3 O10 1.875(17) . ? W3 O17 1.894(15) . ? W3 O34 1.926(16) . ? W3 O12 1.933(14) . ? W3 O11 2.319(14) . ? W4 O28 1.738(14) . ? W4 O27 1.871(15) . ? W4 O10 1.903(17) . ? W4 O32 1.897(17) . ? W4 O35 1.930(15) . ? W4 O3 2.293(14) . ? W5 O25 1.69(2) . ? W5 O5 1.887(15) . ? W5 O13 1.918(14) . ? W5 O24 1.916(16) . ? W5 O34 1.955(14) . ? W5 O11 2.418(15) . ? W6 O26 1.686(16) . ? W6 O6 1.847(15) . ? W6 O13 1.895(17) . ? W6 O16 1.918(17) . ? W6 O17 1.994(15) . ? W6 O11 2.370(14) . ? W7 O18 1.713(18) . ? W7 O14 1.852(16) . ? W7 O44 1.904(17) . ? W7 O15 1.918(16) . ? W7 O32 1.977(15) . ? W7 O3 2.322(15) . ? W8 O39 1.688(17) . ? W8 O20 1.887(15) . ? W8 O21 1.916(16) . ? W8 O6 1.920(16) . ? W8 O23 1.93(2) . ? W8 O9 2.403(14) . ? W9 O4 1.715(15) . ? W9 O12 1.862(15) . ? W9 O27 1.925(17) . ? W9 O37 1.923(17) . ? W9 O19 1.965(16) . ? W9 O7 2.285(14) . ? W10 O38 1.682(16) . ? W10 O16 1.891(18) . ? W10 O20 1.921(14) . ? W10 O35 1.952(16) . ? W10 O15 1.99(2) . ? W10 O3 2.390(15) . ? W11 O31 1.717(16) . ? W11 O8 1.904(15) . ? W11 O44 1.909(16) . ? W11 O22 1.922(17) . ? W11 O19 1.914(14) . ? W11 O7 2.327(15) . ? W12 O29 1.700(16) . ? W12 O5 1.864(16) . ? W12 O21 1.892(15) . ? W12 O36 1.954(16) . ? W12 O2 1.994(19) . ? W12 O9 2.399(15) . ? Si1 O9 1.581(15) . ? Si1 O11 1.625(17) . ? Si1 O3 1.632(15) . ? Si1 O7 1.669(14) . ? Co1 N13 2.071(19) . ? Co1 N10 2.117(18) . ? Co1 O1 2.14(2) . ? Co1 O40 2.176(19) . ? Co1 N15 2.19(2) . ? Co1 O33 2.269(16) . ? Co2 N1 2.06(2) . ? Co2 N16 2.10(2) . ? Co2 O41 2.11(2) . ? Co2 N2 2.12(2) . ? Co2 O43 2.13(2) . ? C1 C12 1.35(5) . ? C1 N6 1.38(3) . ? C2 N9 1.36(3) . ? C2 C8 1.37(4) . ? C3 C7 1.32(4) . ? C3 C14 1.43(4) . ? C4 N9 1.31(4) . ? C4 N5 1.33(3) . ? C5 C20 1.34(4) . ? C5 C16 1.39(4) . ? C6 N6 1.26(4) . ? C6 N11 1.35(4) . ? C7 C21 1.40(3) . ? C8 N5 1.41(3) . ? C9 C16 1.39(3) . ? C9 C13 1.39(4) . ? C10 C17 1.37(4) . ? C10 N10 1.37(3) . ? C11 C13 1.42(4) . ? C11 C20 1.42(3) . ? C12 N11 1.34(5) . ? C14 C19 1.42(3) . ? C15 C30 1.33(4) . ? C15 N7 1.42(3) . ? C16 N8 1.44(3) . ? C17 N8 1.35(3) . ? C18 C21 1.35(3) . ? C18 C19 1.37(3) . ? C19 N7 1.42(3) . ? C20 N6 1.49(3) . ? C21 N5 1.42(3) . ? C22 C24 1.34(4) . ? C22 C23 1.41(4) . ? C23 C25 1.43(4) . ? C24 C27 1.34(4) . ? C24 N4 1.46(3) . ? C25 C26 1.35(3) . ? C26 C27 1.42(3) . ? C26 N3 1.42(3) . ? C28 N2 1.26(3) . ? C28 N3 1.36(3) . ? C29 N3 1.34(3) . ? C29 C31 1.37(4) . ? C30 N16 1.38(3) . ? C31 N2 1.37(3) . ? C32 N16 1.25(4) . ? C32 N7 1.39(3) . ? C33 C48 1.30(4) . ? C33 N14 1.36(4) . ? C34 N4 1.32(4) . ? C34 N15 1.32(3) . ? C35 N10 1.33(3) . ? C35 N8 1.35(3) . ? C36 N13 1.32(3) . ? C36 N12 1.36(3) . ? C37 C38 1.31(3) . ? C37 C40 1.40(3) . ? C37 N12 1.42(3) . ? C38 C42 1.37(4) . ? C39 N15 1.33(4) . ? C39 C45 1.41(4) . ? C40 C41 1.42(4) . ? C41 C44 1.26(5) . ? C42 N14 1.42(3) . ? C42 C44 1.45(3) . ? C43 C46 1.34(4) . ? C43 N13 1.38(3) . ? C45 N4 1.38(4) . ? C46 N12 1.44(3) . ? C47 N1 1.32(3) . ? C47 N14 1.35(3) . ? C48 N1 1.41(4) . ? 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 O30 W1 O36 103.8(8) . . ? O30 W1 O22 99.0(8) . . ? O36 W1 O22 92.1(7) . . ? O30 W1 O24 103.7(8) . . ? O36 W1 O24 88.6(7) . . ? O22 W1 O24 156.5(7) . . ? O30 W1 O37 97.3(7) . . ? O36 W1 O37 158.9(7) . . ? O22 W1 O37 86.1(7) . . ? O24 W1 O37 84.9(7) . . ? O30 W1 O7 165.7(7) . . ? O36 W1 O7 87.9(7) . . ? O22 W1 O7 72.0(6) . . ? O24 W1 O7 84.6(7) . . ? O37 W1 O7 71.6(6) . . ? O42 W2 O2 100.6(8) . . ? O42 W2 O8 100.3(8) . . ? O2 W2 O8 91.9(7) . . ? O42 W2 O23 100.7(9) . . ? O2 W2 O23 88.1(8) . . ? O8 W2 O23 158.7(8) . . ? O42 W2 O14 101.0(8) . . ? O2 W2 O14 158.4(8) . . ? O8 W2 O14 85.8(7) . . ? O23 W2 O14 86.4(7) . . ? O42 W2 O9 171.8(8) . . ? O2 W2 O9 74.2(6) . . ? O8 W2 O9 86.3(6) . . ? O23 W2 O9 73.2(7) . . ? O14 W2 O9 84.2(6) . . ? O33 W3 O10 99.3(8) . . ? O33 W3 O17 101.2(7) . . ? O10 W3 O17 92.7(7) . . ? O33 W3 O34 101.7(8) . . ? O10 W3 O34 158.7(6) . . ? O17 W3 O34 86.7(7) . . ? O33 W3 O12 101.1(8) . . ? O10 W3 O12 86.5(7) . . ? O17 W3 O12 157.5(7) . . ? O34 W3 O12 86.1(7) . . ? O33 W3 O11 172.7(7) . . ? O10 W3 O11 85.4(6) . . ? O17 W3 O11 72.9(6) . . ? O34 W3 O11 74.0(6) . . ? O12 W3 O11 84.6(6) . . ? O28 W4 O27 102.4(8) . . ? O28 W4 O10 100.3(8) . . ? O27 W4 O10 86.8(7) . . ? O28 W4 O32 98.3(8) . . ? O27 W4 O32 93.4(7) . . ? O10 W4 O32 160.9(6) . . ? O28 W4 O35 95.9(8) . . ? O27 W4 O35 161.3(7) . . ? O10 W4 O35 85.9(7) . . ? O32 W4 O35 88.0(7) . . ? O28 W4 O3 168.3(8) . . ? O27 W4 O3 87.7(6) . . ? O10 W4 O3 86.1(6) . . ? O32 W4 O3 74.8(6) . . ? O35 W4 O3 74.6(6) . . ? O25 W5 O5 107.1(8) . . ? O25 W5 O13 101.5(9) . . ? O5 W5 O13 86.7(7) . . ? O25 W5 O24 102.1(9) . . ? O5 W5 O24 87.0(6) . . ? O13 W5 O24 156.4(8) . . ? O25 W5 O34 97.6(8) . . ? O5 W5 O34 155.3(7) . . ? O13 W5 O34 87.0(6) . . ? O24 W5 O34 89.3(6) . . ? O25 W5 O11 166.6(7) . . ? O5 W5 O11 84.1(6) . . ? O13 W5 O11 71.3(6) . . ? O24 W5 O11 85.4(7) . . ? O34 W5 O11 71.2(6) . . ? O26 W6 O6 105.2(8) . . ? O26 W6 O13 99.2(9) . . ? O6 W6 O13 92.4(7) . . ? O26 W6 O16 104.7(8) . . ? O6 W6 O16 88.8(7) . . ? O13 W6 O16 154.9(7) . . ? O26 W6 O17 97.6(7) . . ? O6 W6 O17 157.1(7) . . ? O13 W6 O17 85.9(6) . . ? O16 W6 O17 83.4(7) . . ? O26 W6 O11 165.5(8) . . ? O6 W6 O11 87.5(6) . . ? O13 W6 O11 72.8(6) . . ? O16 W6 O11 82.2(6) . . ? O17 W6 O11 70.2(5) . . ? O18 W7 O14 102.6(8) . . ? O18 W7 O44 102.6(8) . . ? O14 W7 O44 87.6(7) . . ? O18 W7 O15 98.4(9) . . ? O14 W7 O15 91.2(7) . . ? O44 W7 O15 158.7(8) . . ? O18 W7 O32 98.2(8) . . ? O14 W7 O32 159.2(8) . . ? O44 W7 O32 86.8(7) . . ? O15 W7 O32 86.8(7) . . ? O18 W7 O3 168.3(7) . . ? O14 W7 O3 86.7(7) . . ? O44 W7 O3 84.7(7) . . ? O15 W7 O3 74.0(7) . . ? O32 W7 O3 72.7(6) . . ? O39 W8 O20 104.5(7) . . ? O39 W8 O21 100.4(8) . . ? O20 W8 O21 155.1(7) . . ? O39 W8 O6 107.1(8) . . ? O20 W8 O6 86.4(7) . . ? O21 W8 O6 85.8(7) . . ? O39 W8 O23 97.3(8) . . ? O20 W8 O23 89.5(7) . . ? O21 W8 O23 87.9(7) . . ? O6 W8 O23 155.5(7) . . ? O39 W8 O9 166.6(7) . . ? O20 W8 O9 83.7(6) . . ? O21 W8 O9 72.0(6) . . ? O6 W8 O9 83.7(6) . . ? O23 W8 O9 71.8(6) . . ? O4 W9 O12 100.7(8) . . ? O4 W9 O27 101.6(8) . . ? O12 W9 O27 87.7(7) . . ? O4 W9 O37 98.4(7) . . ? O12 W9 O37 91.7(7) . . ? O27 W9 O37 159.7(6) . . ? O4 W9 O19 99.4(7) . . ? O12 W9 O19 159.8(7) . . ? O27 W9 O19 86.3(7) . . ? O37 W9 O19 87.2(7) . . ? O4 W9 O7 169.9(6) . . ? O12 W9 O7 86.9(6) . . ? O27 W9 O7 85.3(6) . . ? O37 W9 O7 74.5(6) . . ? O19 W9 O7 73.4(6) . . ? O38 W10 O16 104.0(7) . . ? O38 W10 O20 103.2(7) . . ? O16 W10 O20 87.7(7) . . ? O38 W10 O35 100.1(7) . . ? O16 W10 O35 90.0(7) . . ? O20 W10 O35 156.4(6) . . ? O38 W10 O15 98.8(8) . . ? O16 W10 O15 157.2(7) . . ? O20 W10 O15 85.9(7) . . ? O35 W10 O15 87.2(7) . . ? O38 W10 O3 167.2(7) . . ? O16 W10 O3 86.4(6) . . ? O20 W10 O3 84.5(6) . . ? O35 W10 O3 72.0(5) . . ? O15 W10 O3 71.2(6) . . ? O31 W11 O8 99.6(8) . . ? O31 W11 O44 101.6(8) . . ? O8 W11 O44 87.5(7) . . ? O31 W11 O22 98.6(8) . . ? O8 W11 O22 87.1(7) . . ? O44 W11 O22 159.7(7) . . ? O31 W11 O19 100.1(8) . . ? O8 W11 O19 160.0(7) . . ? O44 W11 O19 91.5(7) . . ? O22 W11 O19 87.1(6) . . ? O31 W11 O7 169.3(8) . . ? O8 W11 O7 86.7(6) . . ? O44 W11 O7 87.2(6) . . ? O22 W11 O7 73.0(6) . . ? O19 W11 O7 73.3(6) . . ? O29 W12 O5 106.8(8) . . ? O29 W12 O21 100.7(8) . . ? O5 W12 O21 93.1(7) . . ? O29 W12 O36 101.8(8) . . ? O5 W12 O36 86.5(7) . . ? O21 W12 O36 156.7(7) . . ? O29 W12 O2 96.4(8) . . ? O5 W12 O2 156.5(7) . . ? O21 W12 O2 85.7(7) . . ? O36 W12 O2 85.5(8) . . ? O29 W12 O9 166.0(7) . . ? O5 W12 O9 86.1(6) . . ? O21 W12 O9 72.4(6) . . ? O36 W12 O9 84.3(6) . . ? O2 W12 O9 71.2(6) . . ? O9 Si1 O11 110.7(9) . . ? O9 Si1 O3 109.7(9) . . ? O11 Si1 O3 109.8(8) . . ? O9 Si1 O7 110.5(7) . . ? O11 Si1 O7 108.6(9) . . ? O3 Si1 O7 107.5(8) . . ? N13 Co1 N10 178.6(8) . . ? N13 Co1 O1 90.0(9) . . ? N10 Co1 O1 90.9(8) . . ? N13 Co1 O40 86.4(8) . . ? N10 Co1 O40 92.6(8) . . ? O1 Co1 O40 176.4(8) . . ? N13 Co1 N15 93.7(8) . . ? N10 Co1 N15 87.3(8) . . ? O1 Co1 N15 90.3(9) . . ? O40 Co1 N15 90.5(8) . . ? N13 Co1 O33 88.2(7) . . ? N10 Co1 O33 90.9(7) . . ? O1 Co1 O33 86.5(7) . . ? O40 Co1 O33 92.8(7) . . ? N15 Co1 O33 176.3(7) . . ? N1 Co2 N16 89.6(8) . . ? N1 Co2 O41 95.4(8) . . ? N16 Co2 O41 91.7(8) . . ? N1 Co2 N2 96.9(9) . . ? N16 Co2 N2 172.9(8) . . ? O41 Co2 N2 90.3(8) . . ? N1 Co2 O43 98.9(9) . . ? N16 Co2 O43 87.7(9) . . ? O41 Co2 O43 165.6(8) . . ? N2 Co2 O43 88.7(9) . . ? C12 C1 N6 105(3) . . ? N9 C2 C8 108(2) . . ? C7 C3 C14 119(2) . . ? N9 C4 N5 110(2) . . ? C20 C5 C16 119(2) . . ? N6 C6 N11 110(3) . . ? C3 C7 C21 122(2) . . ? C2 C8 N5 105(2) . . ? C16 C9 C13 117(3) . . ? C17 C10 N10 109(2) . . ? C13 C11 C20 113(2) . . ? N11 C12 C1 110(3) . . ? C9 C13 C11 124(2) . . ? C19 C14 C3 119(2) . . ? C30 C15 N7 105.6(19) . . ? C9 C16 C5 122(2) . . ? C9 C16 N8 118(2) . . ? C5 C16 N8 120.5(19) . . ? N8 C17 C10 106(2) . . ? C21 C18 C19 121.3(19) . . ? C18 C19 C14 119(2) . . ? C18 C19 N7 123.5(17) . . ? C14 C19 N7 117(2) . . ? C5 C20 C11 125(2) . . ? C5 C20 N6 119(2) . . ? C11 C20 N6 116(2) . . ? C18 C21 C7 120(2) . . ? C18 C21 N5 120.4(18) . . ? C7 C21 N5 120(2) . . ? C24 C22 C23 118(3) . . ? C22 C23 C25 120(2) . . ? C27 C24 C22 124(2) . . ? C27 C24 N4 118(2) . . ? C22 C24 N4 119(2) . . ? C26 C25 C23 119(2) . . ? C25 C26 C27 121(2) . . ? C25 C26 N3 121(2) . . ? C27 C26 N3 118(2) . . ? C24 C27 C26 119(2) . . ? N2 C28 N3 112(2) . . ? N3 C29 C31 108(2) . . ? C15 C30 N16 111(2) . . ? N2 C31 C29 107(2) . . ? N16 C32 N7 113(2) . . ? C48 C33 N14 107(3) . . ? N4 C34 N15 112(3) . . ? N10 C35 N8 110(2) . . ? N13 C36 N12 111.5(18) . . ? C38 C37 C40 119(2) . . ? C38 C37 N12 122.7(19) . . ? C40 C37 N12 118(2) . . ? C37 C38 C42 123(2) . . ? N15 C39 C45 111(3) . . ? C37 C40 C41 118(2) . . ? C44 C41 C40 122(3) . . ? C38 C42 N14 121(2) . . ? C38 C42 C44 117(2) . . ? N14 C42 C44 122(3) . . ? C46 C43 N13 112(2) . . ? C41 C44 C42 121(3) . . ? N4 C45 C39 103(3) . . ? C43 C46 N12 105(2) . . ? N1 C47 N14 113(2) . . ? C33 C48 N1 112(3) . . ? W2 O2 W12 123.2(8) . . ? Si1 O3 W4 123.9(9) . . ? Si1 O3 W7 125.0(8) . . ? W4 O3 W7 93.0(5) . . ? Si1 O3 W10 120.9(8) . . ? W4 O3 W10 92.4(5) . . ? W7 O3 W10 93.0(5) . . ? W12 O5 W5 153.2(9) . . ? W6 O6 W8 151.0(10) . . ? Si1 O7 W9 124.9(7) . . ? Si1 O7 W11 122.4(8) . . ? W9 O7 W11 93.4(5) . . ? Si1 O7 W1 122.3(8) . . ? W9 O7 W1 93.3(5) . . ? W11 O7 W1 91.8(4) . . ? W2 O8 W11 149.5(8) . . ? Si1 O9 W2 125.3(9) . . ? Si1 O9 W12 123.9(8) . . ? W2 O9 W12 91.4(5) . . ? Si1 O9 W8 125.1(7) . . ? W2 O9 W8 90.9(5) . . ? W12 O9 W8 89.8(5) . . ? W3 O10 W4 150.8(8) . . ? Si1 O11 W3 125.2(8) . . ? Si1 O11 W6 123.4(8) . . ? W3 O11 W6 93.7(5) . . ? Si1 O11 W5 122.9(7) . . ? W3 O11 W5 92.0(6) . . ? W6 O11 W5 90.2(5) . . ? W9 O12 W3 149.4(10) . . ? W6 O13 W5 125.6(10) . . ? W7 O14 W2 150.6(9) . . ? W7 O15 W10 121.8(10) . . ? W10 O16 W6 148.5(8) . . ? W3 O17 W6 123.2(8) . . ? W11 O19 W9 119.8(8) . . ? W8 O20 W10 151.1(10) . . ? W12 O21 W8 125.8(8) . . ? W11 O22 W1 123.2(8) . . ? W2 O23 W8 123.9(10) . . ? W5 O24 W1 147.6(9) . . ? W4 O27 W9 148.3(9) . . ? W4 O32 W7 119.5(9) . . ? W3 O33 Co1 144.8(10) . . ? W3 O34 W5 122.8(9) . . ? W4 O35 W10 121.1(8) . . ? W1 O36 W12 149.0(9) . . ? W9 O37 W1 120.7(8) . . ? W7 O44 W11 148.2(10) . . ? C47 N1 C48 102(2) . . ? C47 N1 Co2 127(2) . . ? C48 N1 Co2 128.0(18) . . ? C28 N2 C31 107(2) . . ? C28 N2 Co2 122.7(16) . . ? C31 N2 Co2 129.3(18) . . ? C29 N3 C28 105(2) . . ? C29 N3 C26 126.2(19) . . ? C28 N3 C26 128(2) . . ? C34 N4 C45 108(2) . . ? C34 N4 C24 127(2) . . ? C45 N4 C24 124(2) . . ? C4 N5 C21 128(2) . . ? C4 N5 C8 107(2) . . ? C21 N5 C8 125(2) . . ? C6 N6 C1 109(2) . . ? C6 N6 C20 129(2) . . ? C1 N6 C20 122(2) . . ? C32 N7 C19 127.7(18) . . ? C32 N7 C15 103.5(19) . . ? C19 N7 C15 128.8(18) . . ? C17 N8 C35 109(2) . . ? C17 N8 C16 126.4(18) . . ? C35 N8 C16 125.1(19) . . ? C4 N9 C2 109(2) . . ? C35 N10 C10 105.9(19) . . ? C35 N10 Co1 127.9(16) . . ? C10 N10 Co1 123.1(16) . . ? C6 N11 C12 106(3) . . ? C36 N12 C37 123.4(18) . . ? C36 N12 C46 106.4(18) . . ? C37 N12 C46 129.5(19) . . ? C36 N13 C43 105.8(19) . . ? C36 N13 Co1 124.2(14) . . ? C43 N13 Co1 130.0(17) . . ? C33 N14 C47 106(2) . . ? C33 N14 C42 130(2) . . ? C47 N14 C42 124(2) . . ? C34 N15 C39 106(2) . . ? C34 N15 Co1 127(2) . . ? C39 N15 Co1 126.2(18) . . ? C32 N16 C30 106(2) . . ? C32 N16 Co2 130.6(16) . . ? C30 N16 Co2 123.0(18) . . ? _refine_diff_density_max 5.845 _refine_diff_density_min -6.812 _refine_diff_density_rms 0.451 _shelxl_version_number 2013-2 _shelx_res_file ; TITL wk in P1 CELL 0.71069 12.401 13.345 13.370 62.968 89.294 70.227 ZERR 1 0.005 0.005 0.005 0.005 0.005 0.005 LATT -1 SFAC C H N O Si Co W UNIT 13 13 13 13 13 13 13 MERG 2 acta 50 L.S. 10 BOND FMAP 2 isor 0.01 O12 O25 O33 N7 C40 C43 O6 O28 N12 C10 C14 C15 C47 isor 0.001 O17 Si1 O42 N8 C17 O39 C18 O25 PLAN 20 LIST 1 WGHT 0.078000 21.380098 FVAR 0.04887 W1 7 0.648020 -0.345528 0.600845 11.00000 0.01327 0.01605 = 0.01310 0.00210 -0.00764 -0.00629 W2 7 0.368806 -0.546360 0.664678 11.00000 0.02008 0.01061 = 0.00969 0.00026 -0.00375 -0.00706 W3 7 0.379233 0.005609 0.236106 11.00000 0.01716 0.00817 = 0.00565 0.00088 -0.00271 -0.00541 W4 7 0.144536 0.001601 0.404372 11.00000 0.02448 0.01616 = 0.02077 -0.00610 -0.00545 -0.00291 W5 7 0.601860 -0.258391 0.294696 11.00000 0.01797 0.02444 = 0.01228 -0.00839 0.00129 -0.00928 W6 7 0.336091 -0.196226 0.165995 11.00000 0.02328 0.01868 = 0.00573 -0.00261 -0.00272 -0.00545 W7 7 0.130819 -0.260430 0.600849 11.00000 0.02142 0.02932 = 0.01328 -0.00889 0.00330 -0.01460 W8 7 0.316640 -0.475760 0.387712 11.00000 0.02061 0.01387 = 0.02275 -0.00898 -0.00122 -0.00745 W9 7 0.437157 -0.074646 0.536132 11.00000 0.02167 0.01407 = 0.01928 -0.00835 0.00156 -0.00984 W10 7 0.088290 -0.180543 0.318471 11.00000 0.01325 0.01607 = 0.01188 0.00209 -0.00744 -0.00617 W11 7 0.419289 -0.331766 0.740710 11.00000 0.02208 0.01956 = 0.00618 -0.00072 -0.00165 -0.00730 W12 7 0.587947 -0.544555 0.509100 11.00000 0.02196 0.01225 = 0.02335 -0.00574 -0.00810 -0.00119 SI1 5 0.369541 -0.265924 0.455195 11.00000 0.00691 0.00590 = 0.00634 -0.00187 -0.00155 -0.00291 CO1 6 0.268091 0.349349 0.111460 11.00000 0.02324 0.02100 = 0.01098 0.00039 -0.00162 -0.01413 CO2 6 0.482957 1.101717 -0.213320 11.00000 0.02636 0.03046 = 0.01743 0.00016 -0.00410 -0.02099 C1 1 -0.295837 0.005459 0.275580 11.00000 0.04171 0.03786 = 0.05946 -0.02536 0.02132 -0.03460 AFIX 43 H1A 2 -0.340620 0.009017 0.217895 11.00000 -1.20000 AFIX 0 C2 1 0.937669 1.528153 -0.530399 11.00000 0.05284 0.04043 = 0.02228 -0.00684 0.00793 -0.04372 AFIX 43 H2A 2 0.909598 1.573512 -0.608262 11.00000 -1.20000 AFIX 0 C3 1 1.089978 1.125455 -0.062970 11.00000 0.00749 0.03621 = 0.03264 -0.01332 0.00291 -0.00627 AFIX 43 H3A 2 1.156073 1.085494 -0.007578 11.00000 -1.20000 AFIX 0 C4 1 1.033930 1.464058 -0.364199 11.00000 0.03221 0.04785 = 0.03759 -0.01606 -0.00289 -0.03215 AFIX 43 H4A 2 1.080984 1.459168 -0.307230 11.00000 -1.20000 AFIX 0 C5 1 -0.145642 0.212460 0.133153 11.00000 0.01749 0.04298 = 0.02327 -0.00730 -0.01107 -0.00177 AFIX 43 H5A 2 -0.078194 0.168459 0.187315 11.00000 -1.20000 AFIX 0 C6 1 -0.186913 0.048238 0.362304 11.00000 0.01460 0.02481 = 0.03773 0.00157 0.00262 -0.01265 AFIX 43 H6A 2 -0.141732 0.085103 0.376407 11.00000 -1.20000 AFIX 0 C7 1 1.082183 1.220803 -0.160798 11.00000 0.00497 0.01145 = 0.03511 0.00078 -0.00293 0.00291 AFIX 43 H7A 2 1.145294 1.245059 -0.174568 11.00000 -1.20000 AFIX 0 C8 1 0.910942 1.432050 -0.453916 11.00000 0.01606 0.02746 = 0.02710 -0.01380 -0.00631 -0.00209 AFIX 43 H8A 2 0.859442 1.401501 -0.468629 11.00000 -1.20000 AFIX 0 C9 1 -0.250481 0.376478 -0.053423 11.00000 0.01568 0.01989 = 0.03431 -0.00954 -0.01128 0.00470 AFIX 43 H9A 2 -0.255458 0.445001 -0.120721 11.00000 -1.20000 AFIX 0 C10 1 0.059041 0.445825 -0.073854 11.00000 0.02669 0.02161 = 0.02040 -0.00027 0.00055 -0.01571 AFIX 43 H10A 2 0.086781 0.502295 -0.126069 11.00000 -1.20000 AFIX 0 C11 1 -0.343979 0.238658 0.073169 11.00000 0.03124 0.03221 = 0.01125 -0.00582 -0.00191 -0.02262 AFIX 43 H11A 2 -0.407670 0.215515 0.088603 11.00000 -1.20000 AFIX 0 C12 1 -0.275059 -0.072808 0.387712 11.00000 0.02983 0.03476 = 0.04403 -0.01136 0.00729 -0.02437 AFIX 43 H12A 2 -0.302249 -0.135684 0.421479 11.00000 -1.20000 AFIX 0 C13 1 -0.341289 0.334950 -0.032550 11.00000 0.02813 0.03931 = 0.02895 -0.00142 -0.02256 0.00307 AFIX 43 H13A 2 -0.404067 0.372222 -0.091069 11.00000 -1.20000 AFIX 0 C14 1 0.995026 1.084765 -0.043732 11.00000 0.01679 0.02271 = 0.02110 -0.00281 -0.00388 -0.00182 AFIX 43 H14A 2 1.000968 1.013671 0.021206 11.00000 -1.20000 AFIX 0 C15 1 0.784784 1.021434 -0.001973 11.00000 0.02369 0.02310 = 0.01692 0.00219 0.00170 -0.01315 AFIX 43 H15A 2 0.836405 0.973770 0.066662 11.00000 -1.20000 AFIX 0 C16 1 -0.151658 0.311597 0.030270 11.00000 0.01598 0.01063 = 0.01375 0.00512 -0.00672 -0.00237 C17 1 -0.047096 0.440738 -0.090795 11.00000 0.02374 0.02359 = 0.02364 -0.01115 0.00383 -0.00897 AFIX 43 H17A 2 -0.102929 0.489978 -0.156471 11.00000 -1.20000 AFIX 0 C18 1 0.889246 1.254216 -0.224907 11.00000 0.01507 0.01503 = 0.01503 -0.00723 0.00206 -0.00572 AFIX 43 H18A 2 0.822145 1.299812 -0.279563 11.00000 -1.20000 AFIX 0 C19 1 0.891517 1.155112 -0.125784 11.00000 0.01098 0.01573 = 0.01906 -0.00648 -0.00481 -0.00188 C20 1 -0.239254 0.181348 0.152912 11.00000 0.02574 0.02633 = 0.02846 -0.01560 0.00402 -0.01563 C21 1 0.982401 1.286624 -0.244453 11.00000 0.01079 0.01069 = 0.01765 -0.00203 0.00356 -0.00050 C22 1 -0.066520 0.909378 -0.204376 11.00000 0.02934 0.01760 = 0.03800 -0.00268 0.01013 -0.00857 AFIX 43 H22A 2 -0.120996 0.874477 -0.175606 11.00000 -1.20000 AFIX 0 C23 1 -0.098499 1.021807 -0.305035 11.00000 0.01833 0.02584 = 0.03768 -0.01795 -0.00568 -0.00398 AFIX 43 H23A 2 -0.174330 1.061219 -0.344526 11.00000 -1.20000 AFIX 0 C24 1 0.044528 0.854034 -0.151162 11.00000 0.01801 0.02931 = 0.02324 -0.01922 0.00785 -0.00692 C25 1 -0.013683 1.074505 -0.345720 11.00000 0.02121 0.02534 = 0.03396 -0.00385 0.00187 -0.01804 AFIX 43 H25A 2 -0.032789 1.147494 -0.412852 11.00000 -1.20000 AFIX 0 C26 1 0.094914 1.016296 -0.284811 11.00000 0.01536 0.00368 = 0.03272 -0.00555 0.00724 -0.00515 C27 1 0.125398 0.902043 -0.185313 11.00000 0.03369 0.01332 = 0.01573 0.00071 -0.00449 -0.01175 AFIX 43 H27A 2 0.200700 0.861196 -0.144476 11.00000 -1.20000 AFIX 0 C28 1 0.273949 1.047221 -0.243484 11.00000 0.01170 0.03063 = 0.01097 -0.00045 -0.00528 -0.00758 AFIX 43 H28A 2 0.301148 0.981022 -0.170787 11.00000 -1.20000 AFIX 0 C29 1 0.166959 1.175387 -0.407320 11.00000 0.02954 0.00891 = 0.01475 0.00485 -0.00423 -0.00850 AFIX 43 H29A 2 0.107509 1.217960 -0.469825 11.00000 -1.20000 AFIX 0 C30 1 0.682246 1.018884 -0.024377 11.00000 0.03665 0.03378 = 0.00199 -0.00023 0.00044 -0.01782 AFIX 43 H30A 2 0.648825 0.969310 0.028731 11.00000 -1.20000 AFIX 0 C31 1 0.258542 1.206651 -0.395471 11.00000 0.02806 0.01418 = 0.02006 0.00029 -0.00578 -0.00771 AFIX 43 H31A 2 0.274908 1.271879 -0.449481 11.00000 -1.20000 AFIX 0 C32 1 0.697108 1.155133 -0.178936 11.00000 0.03244 0.01936 = 0.01123 0.00485 -0.00276 -0.00889 AFIX 43 H32A 2 0.679610 1.219189 -0.252761 11.00000 -1.20000 AFIX 0 C33 1 0.712058 0.751337 -0.140788 11.00000 0.04194 0.04124 = 0.03912 -0.01626 0.02037 -0.01672 AFIX 43 H33A 2 0.774206 0.698298 -0.153812 11.00000 -1.20000 AFIX 0 C34 1 0.164088 0.634304 -0.037006 11.00000 0.03635 0.01487 = 0.02038 0.00297 -0.00855 -0.00967 AFIX 43 H34A 2 0.211608 0.630291 -0.090508 11.00000 -1.20000 AFIX 0 C35 1 0.044877 0.301122 0.081348 11.00000 0.02178 0.02061 = 0.02249 0.00427 -0.00966 -0.01355 AFIX 43 H35A 2 0.059722 0.239176 0.155992 11.00000 -1.20000 AFIX 0 C36 1 0.462056 0.423291 0.149819 11.00000 0.02708 0.01335 = 0.00790 0.00383 -0.00276 -0.01199 AFIX 43 H36A 2 0.432540 0.493785 0.080196 11.00000 -1.20000 AFIX 0 C37 1 0.637727 0.454215 0.188319 11.00000 0.01453 0.03657 = 0.01189 -0.01106 -0.00501 -0.00866 C38 1 0.613570 0.558106 0.094957 11.00000 0.01897 0.02838 = 0.01414 -0.00703 0.00183 -0.01002 AFIX 43 H38A 2 0.539098 0.596823 0.052573 11.00000 -1.20000 AFIX 0 C39 1 0.093568 0.583210 0.114854 11.00000 0.03447 0.02744 = 0.02290 0.00207 0.00722 -0.00787 AFIX 43 H39A 2 0.079687 0.536393 0.186647 11.00000 -1.20000 AFIX 0 C40 1 0.748248 0.396438 0.255414 11.00000 0.02327 0.01959 = 0.02005 -0.00463 -0.01128 -0.00499 AFIX 43 H40A 2 0.766505 0.324364 0.323341 11.00000 -1.20000 AFIX 0 C41 1 0.831737 0.450958 0.216862 11.00000 0.03204 0.03345 = 0.04233 -0.00987 0.01207 -0.01062 AFIX 43 H41A 2 0.905525 0.413443 0.260382 11.00000 -1.20000 AFIX 0 C42 1 0.692661 0.612176 0.056997 11.00000 0.04133 0.01273 = 0.01947 -0.00164 -0.00529 -0.01010 C43 1 0.482674 0.253444 0.297519 11.00000 0.02394 0.01535 = 0.01901 -0.00152 -0.00136 -0.00174 AFIX 43 H43A 2 0.468465 0.184685 0.346920 11.00000 -1.20000 AFIX 0 C44 1 0.808231 0.549038 0.125016 11.00000 0.01222 0.05217 = 0.06245 -0.02874 -0.00499 -0.00968 AFIX 43 H44A 2 0.865427 0.581097 0.100738 11.00000 -1.20000 AFIX 0 C45 1 0.032864 0.709150 0.047211 11.00000 0.04644 0.03667 = 0.02962 -0.01276 0.01023 -0.02141 AFIX 43 H45A 2 -0.024491 0.762031 0.064702 11.00000 -1.20000 AFIX 0 C46 1 0.571437 0.280639 0.319670 11.00000 0.02685 0.02018 = 0.02908 -0.01230 -0.00293 -0.00246 AFIX 43 H46A 2 0.628174 0.236685 0.384552 11.00000 -1.20000 AFIX 0 C47 1 0.574900 0.827570 -0.064164 11.00000 0.02166 0.02831 = 0.03054 -0.01004 0.01927 -0.01091 AFIX 43 H47A 2 0.525748 0.832967 -0.012191 11.00000 -1.20000 AFIX 0 C48 1 0.655620 0.866051 -0.210660 11.00000 0.03171 0.03449 = 0.02753 -0.00341 0.00998 -0.02453 AFIX 43 H48A 2 0.672251 0.907447 -0.282750 11.00000 -1.20000 AFIX 0 O1 4 0.336251 0.400126 -0.044441 11.00000 0.03908 0.04145 = 0.03448 -0.01557 0.01215 -0.02020 O2 4 0.518036 -0.623257 0.644317 11.00000 0.01385 0.02301 = 0.02601 -0.00549 -0.00355 -0.00040 O3 4 0.231173 -0.198744 0.450533 11.00000 0.00995 0.01821 = 0.01641 -0.00929 0.00619 -0.00087 O4 4 0.449859 0.043774 0.547924 11.00000 0.04047 0.02185 = 0.01209 -0.00740 -0.00351 -0.01559 O5 4 0.603142 -0.416976 0.379033 11.00000 0.02698 0.01409 = 0.00986 -0.00073 -0.00719 -0.00205 O6 4 0.350997 -0.355066 0.258174 11.00000 0.02188 0.01584 = 0.00849 0.00194 -0.00330 -0.00403 O7 4 0.442442 -0.253555 0.550393 11.00000 0.01773 0.01433 = 0.00760 -0.00438 -0.00618 -0.00442 O8 4 0.425913 -0.473407 0.734459 11.00000 0.01592 0.02146 = 0.02245 -0.00481 -0.00460 -0.01164 O9 4 0.397970 -0.403836 0.491693 11.00000 0.01345 0.01542 = 0.01479 -0.00477 -0.00305 -0.00762 O10 4 0.235162 0.032327 0.285798 11.00000 0.01981 0.01805 = 0.01252 -0.00510 -0.00283 -0.00171 O11 4 0.405101 -0.197917 0.331502 11.00000 0.01458 0.00843 = 0.00699 0.00395 -0.00285 0.00069 O12 4 0.443732 -0.023815 0.382177 11.00000 0.02769 0.03009 = 0.00803 -0.01190 -0.00038 -0.00867 O13 4 0.499223 -0.239561 0.175833 11.00000 0.02238 0.02378 = 0.02423 -0.01292 -0.00609 -0.00818 O14 4 0.218960 -0.417910 0.633084 11.00000 0.01836 0.02960 = 0.02600 -0.01683 0.00044 -0.01155 O15 4 0.039182 -0.235053 0.470892 11.00000 0.05934 0.02361 = 0.01408 -0.00276 -0.00484 -0.02878 O16 4 0.188749 -0.144457 0.211166 11.00000 0.01388 0.02067 = 0.01981 -0.00839 -0.00620 -0.00040 O17 4 0.329470 -0.031177 0.127909 11.00000 0.01791 0.01789 = 0.01784 -0.00896 0.00216 -0.00693 O18 4 0.033205 -0.280284 0.692890 11.00000 0.02865 0.03645 = 0.02107 -0.01444 0.01163 -0.02220 O19 4 0.419387 -0.173123 0.693233 11.00000 0.01726 0.01912 = 0.01860 -0.00479 -0.00062 -0.01340 O20 4 0.177516 -0.349222 0.370097 11.00000 0.01392 0.01266 = 0.02238 -0.00554 -0.00426 -0.00032 O21 4 0.481179 -0.564739 0.426942 11.00000 0.01575 0.04740 = 0.02475 -0.03061 0.00777 -0.01357 O22 4 0.583575 -0.382868 0.738612 11.00000 0.02678 0.00832 = 0.01467 0.00525 -0.00331 -0.00787 O23 4 0.307280 -0.564829 0.546248 11.00000 0.01957 0.03733 = 0.03070 -0.02082 -0.00378 -0.00865 O24 4 0.645970 -0.270112 0.437647 11.00000 0.04576 0.01340 = 0.01227 -0.00023 -0.00126 -0.01728 O25 4 0.726654 -0.269900 0.240220 11.00000 0.02955 0.03140 = 0.03031 -0.01480 0.00777 -0.01102 O26 4 0.302548 -0.168857 0.031898 11.00000 0.04323 0.01986 = 0.01264 -0.00944 -0.00285 -0.00342 O27 4 0.271254 -0.021493 0.498005 11.00000 0.02610 0.02684 = 0.01242 -0.01228 -0.00001 -0.00916 O28 4 0.052556 0.148916 0.367080 11.00000 0.02737 0.01158 = 0.01728 -0.00629 -0.00241 0.01426 O29 4 0.708033 -0.669794 0.539378 11.00000 0.01693 0.01328 = 0.02523 -0.00044 -0.00557 0.00357 O30 4 0.792018 -0.393764 0.657319 11.00000 0.02200 0.02207 = 0.01859 -0.00421 -0.00652 -0.00760 O31 4 0.423975 -0.382953 0.884518 11.00000 0.03659 0.02894 = 0.00403 -0.00236 0.00191 -0.01140 O32 4 0.078442 -0.081933 0.529408 11.00000 0.02204 0.01445 = 0.01358 0.00125 -0.00330 -0.00389 O33 4 0.365227 0.154459 0.150533 11.00000 0.02819 0.01282 = 0.01544 0.00566 0.00194 -0.01172 O34 4 0.535586 -0.081784 0.228035 11.00000 0.02435 0.01537 = 0.01626 -0.00756 0.00080 -0.00406 O35 4 0.049736 -0.022210 0.310153 11.00000 0.02604 0.02220 = 0.01519 -0.00374 -0.00535 -0.01099 O36 4 0.638369 -0.478179 0.595187 11.00000 0.03835 0.02328 = 0.01550 -0.00598 -0.00586 -0.01465 O37 4 0.598755 -0.178906 0.578929 11.00000 0.03258 0.01837 = 0.01594 -0.01150 -0.00485 -0.01152 O38 4 -0.033239 -0.154865 0.240992 11.00000 0.02102 0.01727 = 0.01265 -0.00230 -0.00414 -0.00518 O39 4 0.274374 -0.557884 0.342129 11.00000 0.02371 0.02381 = 0.02503 -0.01164 0.00106 -0.01059 O40 4 0.209469 0.295133 0.275492 11.00000 0.04111 0.05035 = 0.02162 -0.02264 0.01295 -0.03646 O41 4 0.535637 1.164269 -0.374081 11.00000 0.02906 0.02559 = 0.02664 -0.00810 0.00949 -0.02017 O42 4 0.353497 -0.665888 0.784609 11.00000 0.03204 0.03128 = 0.03273 -0.01297 0.00388 -0.01438 O43 4 0.410585 1.085837 -0.064291 11.00000 0.03672 0.03625 = 0.01994 -0.00632 0.00709 -0.00959 O44 4 0.256012 -0.267207 0.687829 11.00000 0.02271 N1 3 0.566495 0.919787 -0.163963 11.00000 0.02660 0.02230 = 0.02436 -0.00385 0.00847 -0.01303 N2 3 0.321493 1.123436 -0.288790 11.00000 0.02050 0.03029 = 0.02640 -0.01600 0.00120 -0.01448 N3 3 0.178110 1.072681 -0.313010 11.00000 0.02282 0.01709 = 0.01429 -0.00602 -0.00272 -0.00678 N4 3 0.080064 0.734325 -0.051763 11.00000 0.02457 0.02143 = 0.02229 -0.00517 0.00429 -0.01960 N5 3 0.978355 1.389394 -0.348030 11.00000 0.01680 0.01974 = 0.02801 -0.00685 -0.00663 -0.00934 N6 3 -0.236028 0.079420 0.264915 11.00000 0.01536 0.01808 = 0.02832 -0.01122 0.00832 -0.00715 N7 3 0.799315 1.112139 -0.104661 11.00000 0.01365 0.01584 = 0.00559 0.00490 -0.00112 -0.00940 N8 3 -0.054408 0.350036 0.006826 11.00000 0.01384 0.01394 = 0.01366 -0.00647 0.00175 -0.00540 N9 3 1.012694 1.544988 -0.471586 11.00000 0.04272 0.03467 = 0.04076 -0.00228 0.00540 -0.03565 N10 3 0.118115 0.354811 0.031978 11.00000 0.01898 0.01501 = 0.02495 -0.00778 0.00191 -0.01265 N11 3 -0.209319 -0.046334 0.443165 11.00000 0.03919 0.05224 = 0.05128 0.01355 0.01580 -0.00971 N12 3 0.559051 0.392719 0.220757 11.00000 0.01866 0.01633 = 0.00888 -0.00074 0.00455 -0.01209 N13 3 0.415148 0.339996 0.192508 11.00000 0.02763 0.01417 = 0.01479 -0.00005 -0.00084 -0.01517 N14 3 0.662752 0.723985 -0.045219 11.00000 0.02864 0.02401 = 0.02109 -0.01254 -0.00339 0.00035 N15 3 0.173317 0.540450 0.062134 11.00000 0.03760 0.02627 = 0.00644 0.00446 -0.00384 -0.01729 N16 3 0.631458 1.099272 -0.136669 11.00000 0.03590 0.01828 = 0.00709 -0.00044 -0.00718 -0.00763 HKLF 4 REM wk in P1 REM R1 = 0.0510 for 11969 Fo > 4sig(Fo) and 0.0527 for all 12469 data REM 1103 parameters refined using 123 restraints END WGHT 0.0755 24.9415 REM Highest difference peak 5.845, deepest hole -6.812, 1-sigma level 0.451 Q1 1 0.3982 0.0191 0.2807 11.00000 0.05 5.85 Q2 1 0.0760 -0.1993 0.2827 11.00000 0.05 5.31 Q3 1 0.2938 -0.4831 0.3381 11.00000 0.05 5.18 Q4 1 0.4644 -0.0634 0.5862 11.00000 0.05 4.95 Q5 1 0.4179 -0.0840 0.4865 11.00000 0.05 4.91 Q6 1 0.3531 -0.0039 0.1820 11.00000 0.05 4.91 Q7 1 0.6352 -0.3632 0.5594 11.00000 0.05 4.75 Q8 1 0.3401 -0.4609 0.4370 11.00000 0.05 4.58 Q9 1 0.6221 -0.2424 0.3391 11.00000 0.05 4.57 Q10 1 0.3941 -0.5377 0.7197 11.00000 0.05 4.55 Q11 1 0.3159 -0.2163 0.1271 11.00000 0.05 4.39 Q12 1 0.4417 -0.3164 0.7929 11.00000 0.05 4.32 Q13 1 0.3439 -0.5592 0.6147 11.00000 0.05 4.14 Q14 1 0.3606 -0.1803 0.2156 11.00000 0.05 4.03 Q15 1 0.5744 -0.2630 0.2393 11.00000 0.05 3.91 Q16 1 0.6789 -0.3391 0.6579 11.00000 0.05 3.84 Q17 1 0.1164 -0.0111 0.3574 11.00000 0.05 3.77 Q18 1 0.1038 -0.2715 0.5512 11.00000 0.05 3.74 Q19 1 0.1146 -0.1646 0.3678 11.00000 0.05 3.68 Q20 1 0.3920 -0.3422 0.6910 11.00000 0.05 3.67 ; _shelx_res_checksum 32269 _shelx_hkl_file ; -2 0 0 10.23 0.69 2 0 0 10.81 0.99 -3 0 0 254.71 14.55 3 0 0 233.64 20.51 -4 0 0 496.93 28.85 -4 0 0 488.21 38.91 4 0 0 469.71 40.68 -5 0 0 27.01 2.27 -5 0 0 28.31 1.69 5 0 0 27.78 2.44 -6 0 0 65.82 3.93 -6 0 0 64.42 5.27 -7 0 0 4.15 0.43 -7 0 0 4.27 0.32 -8 0 0 7.12 0.52 -8 0 0 7.81 0.71 -9 0 0 3.70 0.45 -9 0 0 4.18 0.33 -10 0 0 1.57 0.22 -10 0 0 1.83 0.32 -11 0 0 8.54 0.86 -12 0 0 6.71 0.75 -13 0 0 7.34 0.85 -14 0 0 16.68 1.62 -15 0 0 1.68 0.50 -14 1 0 0.35 0.33 -13 1 0 9.40 1.02 -12 1 0 12.93 1.25 -11 1 0 37.90 3.20 -10 1 0 60.91 3.66 -10 1 0 58.98 4.93 -9 1 0 38.07 3.20 -9 1 0 38.89 2.38 8 -1 0 4.80 0.67 -8 1 0 5.44 0.54 -8 1 0 5.25 0.40 7 -1 0 4.99 0.63 -7 1 0 5.41 0.39 -7 1 0 5.33 0.52 6 -1 0 38.91 3.43 -6 1 0 39.11 3.19 -6 1 0 38.62 2.37 5 -1 0 18.86 1.75 -5 1 0 20.50 1.61 -5 1 0 18.40 1.20 4 -1 0 302.27 26.89 -4 1 0 326.81 25.63 -4 1 0 330.65 19.06 3 -1 0 452.56 39.64 -3 1 0 483.72 37.92 -3 1 0 482.04 28.21 -2 1 0 27.68 1.67 1 -1 0 0.69 0.13 -1 1 0 0.58 0.06 -3 -1 0 47.46 2.80 3 1 0 45.50 2.80 -4 -1 0 48.23 2.92 -5 -1 0 2.46 0.21 -5 -1 0 2.91 0.28 -6 -1 0 68.25 5.56 -6 -1 0 69.18 4.14 -7 -1 0 19.80 1.20 -7 -1 0 18.19 1.60 -8 -1 0 7.26 0.49 -8 -1 0 6.68 0.65 -9 -1 0 18.81 1.22 -9 -1 0 19.58 1.65 -10 -1 0 16.56 1.47 -10 -1 0 16.90 1.09 -11 -1 0 0.65 0.22 -12 -1 0 6.51 0.72 -13 -1 0 11.56 1.15 -14 -1 0 1.78 0.41 -15 -1 0 0.74 0.37 -14 2 0 11.57 1.23 -13 2 0 25.78 2.30 -12 2 0 43.15 3.66 -11 2 0 19.37 1.73 -10 2 0 14.76 1.01 -10 2 0 15.45 1.37 9 -2 0 35.99 3.54 -9 2 0 40.87 2.42 -9 2 0 39.56 3.25 8 -2 0 28.29 2.73 -8 2 0 30.69 1.85 -8 2 0 29.67 2.48 7 -2 0 4.54 0.67 -7 2 0 5.62 0.41 -7 2 0 5.83 0.54 6 -2 0 3.20 0.49 -6 2 0 3.67 0.38 -6 2 0 4.04 0.30 5 -2 0 113.93 10.15 -5 2 0 122.58 9.62 -5 2 0 121.46 7.15 4 -2 0 32.91 3.02 -4 2 0 35.02 2.10 -4 2 0 35.45 2.81 3 -2 0 3.42 0.43 -3 2 0 3.93 0.34 -3 2 0 3.63 0.26 2 -2 0 70.10 6.27 -2 2 0 75.83 5.93 -2 2 0 75.09 4.41 1 -2 0 143.99 13.02 -1 2 0 162.38 12.37 -1 2 0 156.62 9.21 0 -2 0 19.63 1.92 0 2 0 23.28 1.32 -1 -2 0 10.74 1.01 1 2 0 11.26 0.68 2 2 0 214.69 12.81 3 2 0 0.77 0.09 -4 -2 0 58.08 3.36 4 2 0 52.92 3.35 -5 -2 0 3.18 0.27 -5 -2 0 3.90 0.34 5 2 0 3.41 0.27 -6 -2 0 62.68 4.19 -6 -2 0 75.83 5.62 -7 -2 0 3.37 0.32 -7 -2 0 2.34 0.24 -8 -2 0 102.85 8.17 -8 -2 0 99.25 6.08 -9 -2 0 9.50 0.89 -9 -2 0 10.06 0.68 -10 -2 0 21.15 1.82 -11 -2 0 2.02 0.34 -12 -2 0 10.82 1.05 -13 -2 0 11.48 1.13 -14 -2 0 25.03 2.24 -15 -2 0 12.61 1.31 -13 3 0 13.38 1.34 -12 3 0 6.44 0.77 -11 3 0 7.48 0.82 10 -3 0 36.09 3.55 -10 3 0 39.31 2.39 -10 3 0 38.58 3.22 9 -3 0 33.40 3.12 -9 3 0 33.30 2.09 -9 3 0 33.39 2.81 8 -3 0 13.26 1.47 -8 3 0 14.37 0.94 -8 3 0 14.35 1.25 7 -3 0 36.13 3.30 -7 3 0 36.30 2.25 -7 3 0 36.64 3.01 6 -3 0 0.98 0.30 -6 3 0 0.39 0.11 -6 3 0 0.48 0.14 5 -3 0 6.75 0.76 -5 3 0 6.50 0.47 -5 3 0 7.10 0.62 4 -3 0 66.12 5.86 -4 3 0 68.40 4.10 -4 3 0 69.27 5.49 -3 3 0 25.73 2.09 -3 3 0 25.43 1.57 2 -3 0 10.56 1.07 -2 3 0 11.05 0.91 -2 3 0 10.93 0.69 1 -3 0 0.99 0.25 -1 3 0 0.37 0.06 -1 3 0 0.32 0.06 0 -3 0 147.06 13.92 0 3 0 181.17 9.82 1 3 0 52.45 3.15 2 3 0 53.19 3.19 3 3 0 71.14 4.26 -4 -3 0 533.13 42.21 4 3 0 519.85 31.35 -5 -3 0 242.60 19.04 5 3 0 232.51 14.18 -6 -3 0 4.56 0.37 -6 -3 0 5.77 0.48 6 3 0 4.43 0.37 -7 -3 0 94.33 7.11 -7 -3 0 81.21 5.31 -8 -3 0 563.56 42.16 -8 -3 0 488.56 31.36 -9 -3 0 135.80 10.94 -9 -3 0 135.27 8.15 -10 -3 0 17.89 1.55 -11 -3 0 2.57 0.39 -12 -3 0 25.53 2.21 -13 -3 0 7.39 0.81 -14 -3 0 19.68 1.80 -15 -3 0 3.17 0.56 -16 -3 0 1.66 0.48 -13 4 0 86.14 7.15 -12 4 0 18.32 1.71 11 -4 0 22.54 2.22 -11 4 0 19.26 1.83 10 -4 0 8.35 1.10 -10 4 0 7.60 0.61 -10 4 0 7.34 0.80 9 -4 0 56.14 5.24 -9 4 0 58.87 4.81 -9 4 0 59.40 3.59 8 -4 0 3.13 0.59 -8 4 0 2.51 0.36 -8 4 0 2.40 0.29 7 -4 0 44.93 4.24 -7 4 0 48.51 3.89 -7 4 0 47.87 2.91 6 -4 0 20.82 1.97 -6 4 0 20.27 1.30 -6 4 0 20.37 1.72 5 -4 0 4.17 0.55 -5 4 0 2.90 0.28 -5 4 0 3.37 0.35 4 -4 0 7.51 0.83 -4 4 0 7.30 0.65 -4 4 0 6.94 0.51 3 -4 0 1.08 0.31 -3 4 0 1.30 0.16 -3 4 0 1.08 0.14 2 -4 0 54.12 4.77 -2 4 0 54.79 3.30 -2 4 0 54.86 4.40 1 -4 0 27.67 2.55 -1 4 0 28.18 1.72 -1 4 0 28.36 2.28 0 -4 0 88.81 8.44 0 4 0 107.53 5.91 -1 -4 0 235.92 23.24 1 4 0 312.46 16.40 -2 -4 0 16.08 1.66 2 4 0 18.56 1.09 -3 -4 0 16.07 1.49 -3 -4 0 15.46 1.31 3 4 0 16.97 1.00 -4 -4 0 431.72 32.92 4 4 0 390.74 24.48 -5 -4 0 318.82 25.01 5 4 0 305.49 18.61 -6 -4 0 19.31 1.63 6 4 0 20.10 1.25 -7 -4 0 13.19 0.90 -7 -4 0 14.95 1.17 7 4 0 12.59 0.90 -8 -4 0 113.02 7.09 -8 -4 0 132.15 9.50 8 4 0 107.18 7.08 -9 -4 0 110.02 8.18 -9 -4 0 91.53 6.12 -10 -4 0 26.68 2.25 -11 -4 0 19.24 1.68 -12 -4 0 5.99 0.66 -13 -4 0 4.24 0.56 -14 -4 0 2.16 0.43 -15 -4 0 -0.40 0.24 -16 -4 0 0.72 0.38 12 -5 0 11.77 1.61 11 -5 0 18.55 2.09 -11 5 0 18.85 1.32 10 -5 0 31.29 3.06 -10 5 0 30.97 2.65 -10 5 0 30.35 1.98 9 -5 0 11.83 1.37 -9 5 0 11.32 1.08 -9 5 0 11.20 0.82 8 -5 0 14.99 1.67 -8 5 0 15.42 1.37 -8 5 0 15.78 1.05 7 -5 0 46.42 4.32 -7 5 0 48.37 2.95 -7 5 0 47.96 3.92 6 -5 0 39.65 3.67 -6 5 0 40.43 3.32 -6 5 0 40.81 2.50 5 -5 0 95.05 8.30 -5 5 0 95.91 7.73 -5 5 0 96.41 5.78 4 -5 0 83.16 7.28 -4 5 0 85.43 5.07 -4 5 0 83.30 6.77 3 -5 0 2.52 0.50 -3 5 0 2.11 0.23 -3 5 0 2.28 0.22 2 -5 0 15.64 1.54 -2 5 0 15.04 1.26 -2 5 0 15.47 0.97 1 -5 0 63.52 5.70 -1 5 0 67.53 5.25 -1 5 0 64.46 3.94 0 -5 0 10.38 1.12 0 5 0 9.99 0.65 1 5 0 46.86 2.83 -2 -5 0 7.52 0.98 2 5 0 8.48 0.54 -3 -5 0 40.31 3.56 -3 -5 0 39.06 3.22 3 5 0 40.91 2.43 -4 -5 0 10.24 0.88 -4 -5 0 11.66 1.07 4 5 0 10.63 0.69 -5 -5 0 16.88 1.34 5 5 0 15.59 1.03 -6 -5 0 40.70 3.29 6 5 0 40.41 2.48 -7 -5 0 113.90 9.24 7 5 0 115.73 6.92 -8 -5 0 11.44 0.79 -8 -5 0 12.06 1.01 8 5 0 11.04 0.79 -9 -5 0 5.53 0.48 -9 -5 0 6.28 0.58 -10 -5 0 59.51 4.87 -11 -5 0 14.81 1.32 -12 -5 0 13.25 1.22 -13 -5 0 1.62 0.35 -14 -5 0 25.30 2.23 -15 -5 0 2.82 0.51 -16 -5 0 7.55 0.92 11 -6 0 5.00 1.06 -11 6 0 4.97 0.54 10 -6 0 3.27 0.80 -10 6 0 3.16 0.40 9 -6 0 10.51 1.31 -9 6 0 9.50 0.75 8 -6 0 20.73 2.14 -8 6 0 20.06 1.35 7 -6 0 46.97 4.29 -7 6 0 46.30 2.89 6 -6 0 1.24 0.50 -6 6 0 1.57 0.24 5 -6 0 4.28 0.73 -5 6 0 4.27 0.37 4 -6 0 61.15 5.54 -4 6 0 64.76 3.81 -4 6 0 61.46 5.06 3 -6 0 54.18 4.92 -3 6 0 55.79 3.36 -3 6 0 55.39 4.46 2 -6 0 13.13 1.37 -2 6 0 12.29 0.81 -2 6 0 11.97 1.02 1 -6 0 2.63 0.56 -1 6 0 2.36 0.23 -1 6 0 2.63 0.24 0 -6 0 63.02 5.71 0 6 0 65.92 3.91 -1 -6 0 110.66 11.06 1 6 0 144.61 7.72 -2 -6 0 84.81 7.39 2 6 0 83.51 5.05 -3 -6 0 89.88 6.97 -3 -6 0 78.98 7.56 3 6 0 90.10 5.23 -4 -6 0 37.54 3.38 -4 -6 0 36.73 3.03 4 6 0 38.49 2.29 -5 -6 0 24.51 2.05 -5 -6 0 26.43 2.33 5 6 0 25.30 1.57 -6 -6 0 56.95 4.59 6 6 0 56.67 3.45 -7 -6 0 10.46 0.89 7 6 0 10.25 0.71 -8 -6 0 71.11 5.80 8 6 0 72.22 4.38 -9 -6 0 55.43 4.52 -10 -6 0 23.32 1.97 -11 -6 0 3.36 0.42 -12 -6 0 66.82 5.49 -13 -6 0 60.75 5.03 -14 -6 0 9.17 0.95 -15 -6 0 5.07 0.68 -16 -6 0 27.00 2.43 11 -7 0 5.32 1.15 -11 7 0 4.94 0.56 10 -7 0 12.72 1.69 -10 7 0 13.67 1.01 9 -7 0 110.88 9.62 -9 7 0 106.77 6.62 8 -7 0 42.06 3.89 -8 7 0 39.55 2.56 7 -7 0 20.34 1.97 -7 7 0 16.52 1.20 6 -7 0 38.72 3.51 -6 7 0 35.64 2.32 5 -7 0 154.22 12.86 -5 7 0 144.71 8.97 4 -7 0 41.40 3.82 -4 7 0 41.01 2.55 3 -7 0 38.38 3.60 -3 7 0 38.66 2.39 2 -7 0 31.02 2.97 -2 7 0 31.04 1.93 1 -7 0 9.11 1.15 -1 7 0 8.86 0.62 0 -7 0 2.56 0.62 0 7 0 1.58 0.20 -1 -7 0 48.89 4.89 1 7 0 58.53 3.31 -2 -7 0 39.22 3.75 2 7 0 40.56 2.46 -3 -7 0 6.82 1.02 3 7 0 8.27 0.54 -4 -7 0 23.44 2.38 -4 -7 0 24.87 1.99 4 7 0 24.64 1.53 -5 -7 0 65.68 5.37 -5 -7 0 67.09 5.86 5 7 0 67.70 4.05 -6 -7 0 10.35 0.85 -6 -7 0 9.87 1.09 6 7 0 9.58 0.68 -7 -7 0 3.15 0.33 7 7 0 3.56 0.30 -8 -7 0 117.84 9.50 8 7 0 118.07 7.13 -9 -7 0 383.82 30.77 -10 -7 0 69.38 5.65 -11 -7 0 16.18 1.42 -12 -7 0 145.73 11.79 -13 -7 0 198.31 16.01 -14 -7 0 12.22 1.19 -15 -7 0 13.55 1.34 -16 -7 0 3.99 0.63 10 -8 0 16.97 1.98 -10 8 0 13.65 1.11 9 -8 0 59.90 5.36 -9 8 0 54.63 3.56 8 -8 0 110.06 9.57 -8 8 0 106.08 6.58 7 -8 0 7.07 1.13 -7 8 0 5.47 0.55 6 -8 0 24.93 2.50 -6 8 0 23.33 1.58 5 -8 0 8.43 1.13 -5 8 0 8.02 0.63 4 -8 0 34.76 3.13 -4 8 0 30.14 2.02 3 -8 0 17.96 1.97 -3 8 0 18.32 1.20 2 -8 0 84.34 7.30 -2 8 0 80.64 4.99 1 -8 0 16.68 1.86 -1 8 0 17.20 1.11 0 -8 0 1.58 0.61 0 8 0 1.65 0.21 -1 -8 0 12.59 1.57 1 8 0 13.96 0.89 -2 -8 0 22.83 2.52 2 8 0 26.24 1.57 -3 -8 0 16.42 1.87 3 8 0 16.77 1.07 -4 -8 0 4.12 0.82 4 8 0 4.66 0.36 -5 -8 0 46.85 4.38 5 8 0 48.83 2.94 -6 -8 0 40.87 3.73 6 8 0 40.67 2.52 -7 -8 0 0.80 0.33 -7 -8 0 0.61 0.13 7 8 0 0.58 0.14 -8 -8 0 8.64 0.96 -8 -8 0 7.69 0.68 8 8 0 6.69 0.56 -9 -8 0 137.19 11.05 -10 -8 0 44.36 3.65 -11 -8 0 16.57 1.45 -12 -8 0 9.31 0.89 -13 -8 0 10.32 1.01 -14 -8 0 2.53 0.44 -15 -8 0 32.23 2.80 -16 -8 0 4.63 0.69 9 -9 0 3.91 1.04 -9 9 0 3.64 0.50 8 -9 0 13.34 1.70 -8 9 0 11.82 0.96 7 -9 0 6.21 1.09 -7 9 0 4.00 0.50 6 -9 0 45.74 4.19 -6 9 0 42.22 2.76 5 -9 0 19.46 2.03 -5 9 0 17.36 1.24 4 -9 0 24.79 2.44 -4 9 0 21.92 1.50 3 -9 0 38.01 3.56 -3 9 0 35.56 2.29 2 -9 0 43.81 4.09 -2 9 0 42.63 2.68 1 -9 0 17.29 1.98 -1 9 0 17.92 1.17 0 -9 0 41.68 3.98 0 9 0 42.32 2.60 -1 -9 0 60.82 6.03 1 9 0 71.10 4.08 -2 -9 0 15.40 1.85 2 9 0 16.26 1.05 -3 -9 0 2.61 0.76 3 9 0 3.59 0.31 -4 -9 0 52.56 4.86 4 9 0 51.58 3.18 -5 -9 0 21.65 2.42 5 9 0 24.36 1.50 -6 -9 0 17.22 1.81 6 9 0 15.74 1.07 -7 -9 0 14.75 1.58 7 9 0 14.49 0.99 -8 -9 0 56.45 4.96 8 9 0 54.12 3.41 -9 -9 0 50.95 4.59 -10 -9 0 12.35 1.37 -12 -9 0 21.19 1.84 -13 -9 0 3.03 0.44 -14 -9 0 6.07 0.69 -15 -9 0 19.01 1.75 -16 -9 0 1.23 0.38 8 -10 0 8.63 1.43 -8 10 0 7.48 0.75 7 -10 0 0.11 0.57 -7 10 0 0.39 0.26 6 -10 0 3.39 0.88 -6 10 0 2.41 0.37 5 -10 0 11.45 1.56 -5 10 0 11.43 0.89 4 -10 0 21.66 2.31 -4 10 0 19.92 1.39 3 -10 0 9.29 1.40 -3 10 0 8.84 0.69 2 -10 0 12.74 1.56 -2 10 0 10.34 0.80 1 -10 0 77.49 6.65 -1 10 0 69.92 4.46 0 -10 0 55.64 5.26 0 10 0 58.06 3.52 -1 -10 0 16.78 2.04 1 10 0 18.27 1.18 -2 -10 0 17.65 2.13 2 10 0 20.82 1.29 -3 -10 0 57.00 5.12 3 10 0 53.17 3.35 -4 -10 0 9.53 1.43 4 10 0 7.41 0.57 -5 -10 0 70.94 6.69 5 10 0 75.10 4.48 -6 -10 0 44.94 4.64 6 10 0 53.24 3.09 -7 -10 0 6.51 1.12 7 10 0 8.17 0.60 -8 -10 0 14.44 1.64 -9 -10 0 3.70 0.75 -10 -10 0 3.24 0.67 -11 -10 0 0.74 0.42 -12 -10 0 7.90 1.09 6 -11 0 12.17 1.68 -6 11 0 11.91 0.98 5 -11 0 81.52 7.25 -5 11 0 77.14 4.89 4 -11 0 160.04 13.34 -4 11 0 145.53 9.21 3 -11 0 39.65 3.78 -3 11 0 36.34 2.40 2 -11 0 18.55 2.12 -2 11 0 18.06 1.25 1 -11 0 77.42 6.80 -1 11 0 71.75 4.55 0 -11 0 178.67 15.67 0 11 0 182.30 10.88 -1 -11 0 3.57 0.87 1 11 0 3.66 0.39 -2 -11 0 44.84 4.79 2 11 0 55.29 3.18 -3 -11 0 1.26 0.68 3 11 0 1.37 0.22 -4 -11 0 15.34 1.74 4 11 0 12.14 0.89 -5 -11 0 6.82 1.25 5 11 0 6.60 0.53 -6 -11 0 25.74 2.83 6 11 0 26.93 1.71 -7 -11 0 2.78 0.78 7 11 0 2.62 0.33 -8 -11 0 8.24 1.31 -9 -11 0 20.92 2.25 -10 -11 0 18.25 2.00 -11 -11 0 3.55 0.79 -12 -11 0 3.23 0.72 -13 -11 0 48.51 4.52 -14 -11 0 48.35 4.53 -15 -11 0 3.72 0.88 5 -12 0 1.05 0.77 -5 12 0 0.76 0.32 4 -12 0 61.87 5.44 -4 12 0 53.22 3.56 3 -12 0 31.92 3.10 -3 12 0 25.94 1.86 2 -12 0 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18.46 1.93 5 6 -3 70.97 4.31 -5 -6 3 75.30 5.80 -5 -6 3 67.10 6.29 4 6 -3 21.95 1.29 -4 -6 3 18.78 1.74 -4 -6 3 20.34 2.12 3 6 -3 168.84 9.44 -3 -6 3 144.16 13.60 2 6 -3 4.32 0.35 -2 -6 3 5.05 0.95 1 6 -3 48.14 3.01 -1 -6 3 50.99 4.58 0 6 -3 35.34 2.12 0 -6 3 31.50 3.29 -1 6 -3 72.73 4.06 1 -6 3 57.69 5.96 -2 6 -3 4.97 0.42 2 -6 3 4.74 0.94 -3 6 -3 45.62 2.84 3 -6 3 45.92 4.33 -4 6 -3 6.25 0.53 4 -6 3 6.22 1.12 -5 6 -3 21.97 1.48 5 -6 3 23.36 2.43 -6 6 -3 31.05 2.03 6 -6 3 32.04 3.19 -7 6 -3 22.35 1.55 7 -6 3 24.30 2.54 -8 6 -3 44.88 3.00 8 -6 3 51.75 4.64 -9 6 -3 27.38 1.94 9 -6 3 32.67 3.18 -10 6 -3 4.80 0.59 10 -6 3 6.54 1.28 -16 -5 3 2.70 0.59 -15 -5 3 1.50 0.43 -14 -5 3 1.13 0.36 -13 -5 3 21.88 1.94 -12 -5 3 8.00 0.84 -11 -5 3 29.58 2.51 -10 -5 3 61.90 5.07 -9 -5 3 15.34 1.33 -8 -5 3 6.03 0.59 -7 -5 3 338.81 27.16 6 5 -3 322.27 20.20 -6 -5 3 359.72 27.18 -6 -5 3 334.82 28.61 5 5 -3 5.97 0.44 -5 -5 3 5.69 0.77 -5 -5 3 7.04 0.60 4 5 -3 43.94 2.71 -4 -5 3 47.22 3.66 -4 -5 3 42.03 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8 -4 38.15 2.52 -3 -8 4 44.91 3.99 2 8 -4 6.94 0.56 -2 -8 4 7.14 1.28 1 8 -4 60.93 3.85 -1 -8 4 64.83 5.80 0 8 -4 1.70 0.27 0 -8 4 1.65 0.79 -1 8 -4 32.02 2.09 1 -8 4 33.01 3.37 -2 8 -4 57.73 3.44 2 -8 4 50.34 5.20 -3 8 -4 178.98 10.45 3 -8 4 164.71 15.12 -4 8 -4 21.27 1.45 4 -8 4 19.75 2.44 -5 8 -4 18.56 1.39 5 -8 4 22.51 2.50 -6 8 -4 83.38 5.27 6 -8 4 86.95 7.87 -7 8 -4 105.56 6.70 7 -8 4 113.35 9.96 -15 -7 4 84.65 7.01 -14 -7 4 81.13 6.70 -13 -7 4 5.33 0.68 -12 -7 4 3.97 0.55 -11 -7 4 29.20 2.84 -10 -7 4 23.94 2.37 -9 -7 4 0.92 0.42 -8 -7 4 11.09 1.30 -7 -7 4 1.67 0.51 -6 -7 4 12.40 1.48 5 7 -4 1.55 0.20 -5 -7 4 0.68 0.52 4 7 -4 3.92 0.33 -4 -7 4 2.73 0.78 3 7 -4 93.76 5.67 2 7 -4 50.32 3.27 -2 -7 4 58.59 5.01 1 7 -4 50.04 3.19 -1 -7 4 54.61 4.88 0 7 -4 36.16 2.32 0 -7 4 38.26 3.66 -1 7 -4 41.71 2.55 1 -7 4 38.66 3.93 -2 7 -4 2.05 0.30 2 -7 4 1.84 0.78 -3 7 -4 115.11 6.78 3 -7 4 106.09 9.91 -4 7 -4 41.37 2.64 4 -7 4 41.54 4.14 -5 7 -4 12.39 0.94 5 -7 4 12.03 1.85 -6 7 -4 1.30 0.31 6 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34.58 -6 -4 4 430.51 32.91 5 4 -4 33.80 1.97 -5 -4 4 29.63 2.93 -5 -4 4 32.70 2.68 4 4 -4 32.97 2.01 -4 -4 4 31.94 3.03 -4 -4 4 34.10 2.76 3 4 -4 4.97 0.35 -3 -4 4 5.02 0.57 -3 -4 4 4.05 0.74 2 4 -4 9.70 0.65 -2 -4 4 10.16 1.24 -2 -4 4 10.01 0.95 1 4 -4 2.48 0.22 -1 -4 4 2.71 0.62 -1 -4 4 2.12 0.33 0 4 -4 2.20 0.22 0 -4 4 1.77 0.58 0 -4 4 1.99 0.27 -1 4 -4 88.18 4.88 1 -4 4 66.89 7.06 1 -4 4 83.35 6.51 -2 4 -4 24.61 1.58 2 -4 4 20.84 2.42 2 -4 4 26.93 2.06 -3 4 -4 38.93 2.41 3 -4 4 37.73 3.63 -4 4 -4 23.86 1.52 4 -4 4 22.55 2.38 -5 4 -4 61.72 3.67 5 -4 4 56.17 5.40 -6 4 -4 5.18 0.47 6 -4 4 5.06 0.95 -7 4 -4 109.49 6.75 7 -4 4 112.74 9.79 -8 4 -4 95.63 5.91 8 -4 4 97.64 8.62 -9 4 -4 15.15 1.12 9 -4 4 15.55 1.88 -10 4 -4 6.83 0.66 10 -4 4 6.58 1.22 -11 4 -4 70.75 4.31 11 -4 4 65.14 6.40 -16 -3 4 21.20 2.02 -15 -3 4 0.47 0.37 -14 -3 4 57.76 4.85 -13 -3 4 19.95 1.81 -12 -3 4 20.17 1.80 -11 -3 4 30.35 2.58 -10 -3 4 222.12 17.89 -9 -3 4 32.78 2.74 -8 -3 4 22.24 1.88 -7 -3 4 2.69 0.33 -6 -3 4 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3.10 0.97 -7 9 15 1.28 0.58 -6 9 15 4.24 0.81 -5 9 15 10.40 1.27 -4 9 15 10.09 1.25 -3 9 15 5.49 0.92 -2 9 15 2.19 0.61 -1 9 15 9.27 1.24 0 9 15 7.56 1.15 -1 -9 -15 1.32 0.33 1 9 15 1.89 0.37 1 9 15 2.01 0.66 -2 -9 -15 42.25 2.78 2 9 15 40.64 2.77 2 9 15 45.07 3.94 -3 -9 -15 18.04 1.34 3 9 15 16.52 1.33 3 9 15 17.83 2.00 -4 -9 -15 0.25 0.28 4 9 15 0.10 0.54 4 9 15 0.80 0.34 -5 -9 -15 7.86 0.88 5 9 15 7.97 1.33 5 9 15 7.50 0.86 -6 -9 -15 18.60 1.53 6 9 15 16.95 2.15 6 9 15 21.44 1.55 -7 -9 -15 0.77 0.42 7 9 15 -0.24 0.55 -8 -9 -15 1.76 0.56 8 9 15 1.49 0.83 -9 -9 -15 3.04 0.69 9 9 15 2.88 1.06 -6 10 15 9.83 1.32 -5 10 15 5.58 0.92 -4 10 15 4.17 0.79 -3 10 15 2.91 0.68 -2 10 15 12.27 1.48 -1 10 15 20.58 2.11 0 10 15 2.77 0.68 0 10 15 2.84 0.42 -1 -10 -15 1.89 0.37 1 10 15 2.25 0.40 1 10 15 2.18 0.66 -2 -10 -15 16.78 1.27 2 10 15 15.62 1.26 2 10 15 19.64 1.98 -3 -10 -15 25.49 1.85 3 10 15 31.13 2.74 3 10 15 24.40 1.84 -4 -10 -15 10.78 0.98 4 10 15 11.42 1.54 4 10 15 11.68 1.00 -5 -10 -15 0.96 0.35 5 10 15 -0.08 0.53 5 10 15 0.83 0.35 -6 -10 -15 8.81 0.86 6 10 15 7.94 0.87 6 10 15 7.14 1.29 -7 -10 -15 33.39 2.28 7 10 15 28.31 3.14 7 10 15 32.24 2.27 -8 -10 -15 17.31 1.38 8 10 15 12.06 1.88 -9 -10 -15 11.49 1.13 9 10 15 9.91 1.66 -5 11 15 0.61 0.47 -4 11 15 6.19 0.99 -3 11 15 9.11 1.23 -2 11 15 5.54 0.95 -1 11 15 22.69 2.28 0 11 15 4.90 0.56 0 11 15 4.73 0.90 1 11 15 11.89 1.00 1 11 15 13.21 1.53 2 11 15 3.64 0.83 2 11 15 3.09 0.47 -3 -11 -15 29.96 2.15 3 11 15 39.02 3.20 3 11 15 29.48 2.15 -4 -11 -15 14.19 1.20 4 11 15 18.56 1.91 4 11 15 14.44 1.20 -5 -11 -15 27.20 1.94 5 11 15 25.97 1.92 5 11 15 29.15 2.85 -6 -11 -15 40.36 2.68 6 11 15 38.97 2.67 6 11 15 38.92 3.77 7 11 15 2.11 0.81 7 11 15 4.56 0.66 -8 -11 -15 2.02 0.55 8 11 15 1.44 0.50 8 11 15 0.50 0.62 9 11 15 27.88 3.00 -4 12 15 0.34 0.42 -3 12 15 3.38 0.74 -2 12 15 6.35 1.03 -1 12 15 20.88 2.16 0 12 15 25.21 2.35 0 12 15 21.26 1.58 1 12 15 13.29 1.06 1 12 15 14.28 1.63 2 12 15 9.12 0.83 2 12 15 9.21 1.33 3 12 15 0.35 0.51 3 12 15 0.88 0.33 -4 -12 -15 4.13 0.56 4 12 15 3.79 0.53 4 12 15 5.02 0.97 -5 -12 -15 10.93 0.96 5 12 15 10.74 1.55 5 12 15 9.92 0.95 6 12 15 40.25 3.96 6 12 15 43.59 2.84 -7 -12 -15 32.92 2.20 7 12 15 31.11 2.17 7 12 15 26.05 3.02 -8 -12 -15 3.39 0.63 8 12 15 4.05 0.65 8 12 15 2.08 0.84 -3 13 15 9.34 1.31 -2 13 15 10.92 1.41 -1 13 15 8.99 1.28 0 13 15 12.03 1.37 0 13 15 7.62 0.76 1 13 15 6.84 0.72 1 13 15 8.93 1.24 2 13 15 10.34 0.91 2 13 15 11.53 1.44 3 13 15 2.31 0.45 3 13 15 4.39 0.90 4 13 15 1.93 0.39 4 13 15 1.62 0.68 5 13 15 -0.13 0.26 5 13 15 -0.27 0.45 -6 -13 -15 2.39 0.53 6 13 15 2.81 0.86 6 13 15 4.26 0.61 -7 -13 -15 14.00 1.15 7 13 15 11.83 1.12 7 13 15 12.11 1.67 -8 -13 -15 0.90 0.42 8 13 15 0.96 0.69 8 13 15 0.67 0.43 0 14 15 5.84 0.63 1 14 15 4.87 0.60 1 14 15 8.54 1.31 2 14 15 4.95 0.95 2 14 15 3.94 0.55 3 14 15 21.36 2.07 3 14 15 15.93 1.32 4 14 15 1.45 0.37 4 14 15 1.29 0.67 5 14 15 4.39 0.95 5 14 15 4.17 0.59 6 14 15 6.90 0.77 6 14 15 7.38 1.23 -7 -14 -15 22.19 1.72 7 14 15 21.93 2.42 7 14 15 23.02 1.70 1 15 15 24.97 1.74 2 15 15 13.04 1.06 3 15 15 17.31 1.31 4 15 15 8.86 0.85 5 15 15 9.99 0.93 -5 1 16 3.16 0.79 -4 1 16 7.12 1.11 -3 1 16 1.12 0.59 -2 1 16 2.63 0.74 -1 1 16 5.97 1.12 -6 2 16 11.50 1.49 -5 2 16 -0.11 0.47 -4 2 16 1.52 0.65 -3 2 16 6.47 1.07 -2 2 16 14.12 1.67 -1 2 16 0.78 0.57 0 2 16 9.78 1.37 1 2 16 29.55 2.89 2 2 16 7.64 1.24 -6 3 16 2.02 0.66 -5 3 16 4.81 0.94 -4 3 16 5.15 0.96 -3 3 16 4.05 0.85 -2 3 16 30.55 2.96 -1 3 16 25.26 2.55 0 3 16 33.21 3.18 1 3 16 23.79 2.45 2 3 16 31.72 3.09 -3 -3 -16 16.77 1.39 3 3 16 21.08 2.13 -7 4 16 5.78 1.00 -6 4 16 2.13 0.65 -5 4 16 8.62 1.23 -4 4 16 4.12 0.86 -3 4 16 16.69 1.87 -2 4 16 1.83 0.65 -1 4 16 20.47 2.17 0 4 16 18.18 2.01 1 4 16 4.86 0.99 2 4 16 3.92 0.92 -3 -4 -16 20.87 1.68 3 4 16 26.70 2.53 -4 -4 -16 31.89 2.48 4 4 16 43.38 3.63 -7 5 16 30.52 2.90 -6 5 16 30.99 2.94 -5 5 16 4.61 0.89 -4 5 16 6.12 1.02 -3 5 16 79.82 6.82 -2 5 16 87.26 7.43 -1 5 16 7.96 1.22 0 5 16 0.07 0.55 1 5 16 2.70 0.77 2 5 16 20.64 2.24 -3 -5 -16 5.46 0.69 3 5 16 6.49 1.13 -4 -5 -16 11.36 1.03 4 5 16 11.31 1.62 -5 -5 -16 17.06 1.49 5 5 16 22.56 2.28 -6 6 16 39.66 3.61 -5 6 16 11.12 1.41 -4 6 16 2.15 0.63 -3 6 16 16.65 1.82 -2 6 16 21.14 2.18 -1 6 16 0.95 0.57 0 6 16 3.40 0.85 1 6 16 0.44 0.56 -2 -6 -16 15.41 1.26 2 6 16 15.64 1.86 -3 -6 -16 10.40 0.99 3 6 16 10.99 1.53 -4 -6 -16 0.90 0.40 4 6 16 1.49 0.76 -5 -6 -16 7.16 0.88 5 6 16 10.08 1.47 -6 -6 -16 22.86 1.86 6 6 16 29.31 2.79 -6 7 16 4.14 0.79 -5 7 16 2.89 0.69 -4 7 16 1.62 0.55 -3 7 16 2.40 0.65 -2 7 16 0.99 0.53 -1 7 16 19.43 2.04 0 7 16 12.88 1.57 1 7 16 8.41 1.27 -2 -7 -16 0.21 0.36 2 7 16 0.16 0.56 -3 -7 -16 40.06 2.86 3 7 16 45.88 4.02 -4 -7 -16 23.78 1.81 4 7 16 24.66 2.62 -5 -7 -16 11.74 1.13 5 7 16 13.13 1.74 -6 -7 -16 2.56 0.57 6 7 16 2.31 0.89 -6 8 16 0.66 0.46 -5 8 16 7.49 1.10 -4 8 16 7.02 1.06 -3 8 16 15.15 1.68 -2 8 16 26.05 2.54 -1 8 16 2.10 0.66 0 8 16 2.71 0.74 1 8 16 56.05 4.98 -2 -8 -16 92.89 6.34 2 8 16 112.93 8.73 -3 -8 -16 1.74 0.46 3 8 16 1.68 0.75 -4 -8 -16 3.19 0.57 4 8 16 3.40 0.93 -5 -8 -16 27.46 2.01 5 8 16 26.60 2.83 -6 -8 -16 37.92 2.76 6 8 16 41.40 3.88 -7 -8 -16 5.42 0.83 7 8 16 5.44 1.17 -5 9 16 0.09 0.42 -4 9 16 4.14 0.82 -3 9 16 20.52 2.10 -2 9 16 89.80 7.61 -1 9 16 43.35 3.92 0 9 16 9.34 1.34 1 9 16 58.22 4.96 1 9 16 53.25 3.57 -2 -9 -16 125.90 8.26 2 9 16 152.20 11.34 2 9 16 128.20 8.27 -3 -9 -16 39.61 2.75 3 9 16 42.85 3.90 3 9 16 41.58 2.77 -4 -9 -16 1.16 0.37 4 9 16 1.24 0.67 4 9 16 0.68 0.35 -5 -9 -16 2.52 0.55 5 9 16 2.39 0.85 -6 -9 -16 18.42 1.56 6 9 16 18.81 2.20 -7 -9 -16 16.61 1.49 7 9 16 15.85 2.03 -5 10 16 6.07 1.00 -4 10 16 0.82 0.51 -3 10 16 1.13 0.53 -2 10 16 17.96 1.91 -1 10 16 17.26 1.87 0 10 16 0.98 0.53 1 10 16 2.41 0.72 1 10 16 1.77 0.39 -2 -10 -16 11.54 1.01 2 10 16 11.78 1.02 2 10 16 13.21 1.57 -3 -10 -16 1.19 0.37 3 10 16 2.01 0.75 3 10 16 0.76 0.35 -4 -10 -16 5.66 0.68 4 10 16 4.23 0.62 4 10 16 4.42 1.01 -5 -10 -16 1.54 0.46 5 10 16 0.83 0.41 5 10 16 0.79 0.71 -6 -10 -16 -0.37 0.39 6 10 16 -0.03 0.62 6 10 16 0.21 0.44 -7 -10 -16 12.15 1.17 7 10 16 10.98 1.71 -4 11 16 1.92 0.62 -3 11 16 0.29 0.48 -2 11 16 2.74 0.71 -1 11 16 25.59 2.51 0 11 16 14.52 1.66 -1 -11 -16 0.39 0.29 1 11 16 0.15 0.48 1 11 16 0.03 0.27 -2 -11 -16 5.59 0.66 2 11 16 5.39 0.65 2 11 16 6.94 1.11 -3 -11 -16 5.74 0.73 3 11 16 6.88 0.76 3 11 16 9.74 1.32 -4 -11 -16 10.13 0.96 4 11 16 10.28 0.96 4 11 16 14.10 1.62 -5 -11 -16 7.51 0.88 5 11 16 8.21 0.89 5 11 16 9.93 1.46 6 11 16 30.24 3.05 6 11 16 28.30 2.11 -7 -11 -16 1.30 0.52 7 11 16 0.96 0.77 7 11 16 0.56 0.47 -2 12 16 3.85 0.82 -1 12 16 1.99 0.64 0 12 16 16.78 1.84 1 12 16 14.81 1.65 1 12 16 11.28 1.00 -2 -12 -16 52.77 3.50 2 12 16 49.69 3.47 2 12 16 63.17 4.95 -3 -12 -16 23.12 1.69 3 12 16 28.60 2.56 3 12 16 20.70 1.66 -4 -12 -16 0.14 0.30 4 12 16 0.11 0.30 4 12 16 -0.12 0.54 -5 -12 -16 17.18 1.38 5 12 16 18.90 2.16 5 12 16 16.41 1.35 -6 -12 -16 112.76 7.16 6 12 16 111.24 7.14 6 12 16 120.34 9.83 -7 -12 -16 62.22 4.04 7 12 16 58.64 5.56 7 12 16 62.60 4.03 -1 13 16 1.63 0.66 0 13 16 0.94 0.57 1 13 16 2.74 0.45 1 13 16 3.01 0.78 2 13 16 29.67 2.17 2 13 16 35.84 3.16 3 13 16 44.15 3.23 3 13 16 58.93 4.65 4 13 16 13.88 1.63 4 13 16 9.57 0.98 -5 -13 -16 5.60 0.72 5 13 16 5.25 0.67 5 13 16 6.06 1.17 -6 -13 -16 39.33 2.58 6 13 16 33.57 2.52 6 13 16 38.57 3.64 1 14 16 0.81 0.33 1 14 16 0.43 0.53 2 14 16 2.26 0.45 2 14 16 1.59 0.73 3 14 16 8.88 0.89 3 14 16 10.81 1.49 4 14 16 3.62 0.54 4 14 16 4.06 0.97 -2 3 17 6.25 1.08 -1 3 17 12.48 1.60 -4 4 17 25.89 2.58 -3 4 17 12.26 1.58 -2 4 17 10.14 1.42 -1 4 17 15.98 1.88 0 4 17 36.03 3.43 1 4 17 18.04 2.10 -4 5 17 13.09 1.58 -3 5 17 6.70 1.10 -2 5 17 0.68 0.60 -1 5 17 5.52 1.04 0 5 17 40.70 3.79 1 5 17 26.45 2.73 2 5 17 14.03 1.79 3 5 17 6.57 1.21 -4 6 17 2.30 0.67 -3 6 17 1.73 0.67 -2 6 17 7.60 1.18 -1 6 17 8.56 1.29 0 6 17 6.47 1.11 1 6 17 20.91 2.27 2 6 17 32.32 3.21 3 6 17 17.28 2.05 -4 7 17 5.00 0.93 -3 7 17 4.69 0.90 -2 7 17 7.44 1.15 -1 7 17 18.97 2.04 0 7 17 13.30 1.66 1 7 17 15.17 1.82 2 7 17 15.23 1.90 -3 -7 -17 6.67 0.83 3 7 17 9.40 1.38 -4 -7 -17 6.56 0.84 4 7 17 8.48 1.34 -3 8 17 5.65 0.97 -2 8 17 1.95 0.64 -1 8 17 10.82 1.42 0 8 17 32.20 3.09 1 8 17 15.08 1.80 2 8 17 0.49 0.63 -3 -8 -17 9.95 1.03 3 8 17 12.23 1.59 -4 -8 -17 28.20 2.23 4 8 17 35.23 3.20 5 8 17 18.30 2.33 -3 9 17 7.46 1.14 -2 9 17 53.07 4.70 -1 9 17 22.13 2.27 0 9 17 2.99 0.79 1 9 17 2.19 0.74 2 9 17 10.84 1.12 2 9 17 12.72 1.67 -3 -9 -17 8.87 0.96 3 9 17 10.46 1.47 -4 -9 -17 17.19 1.45 4 9 17 17.83 2.07 -5 -9 -17 19.75 1.71 5 9 17 24.03 2.51 -3 10 17 5.83 1.01 -2 10 17 31.87 3.02 -1 10 17 32.47 3.08 0 10 17 2.27 0.72 1 10 17 2.15 0.73 2 10 17 2.08 0.46 2 10 17 1.43 0.71 -3 -10 -17 18.39 1.49 3 10 17 21.41 2.23 3 10 17 18.71 1.50 -4 -10 -17 11.75 1.14 4 10 17 11.70 1.71 4 10 17 12.96 1.16 -5 -10 -17 5.44 0.79 5 10 17 5.18 1.15 -1 11 17 1.16 0.60 0 11 17 6.95 1.14 1 11 17 3.95 0.88 -2 -11 -17 1.70 0.43 2 11 17 1.68 0.71 2 11 17 2.78 0.48 -3 -11 -17 8.25 0.89 3 11 17 8.15 0.89 3 11 17 10.95 1.51 -4 -11 -17 19.49 1.61 4 11 17 19.35 1.60 4 11 17 25.18 2.43 0 12 17 10.89 1.45 1 12 17 0.27 0.56 -2 -12 -17 27.78 2.06 2 12 17 34.67 3.06 2 12 17 28.80 2.07 -3 -12 -17 5.08 0.71 3 12 17 4.86 0.70 3 12 17 7.97 1.24 -4 -12 -17 8.04 0.90 4 12 17 7.91 1.35 4 12 17 7.75 0.86 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 32604 _database_code_depnum_ccdc_archive 'CCDC 945353' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ytt _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H45 B Co2 N16 O42 W12' _chemical_formula_sum 'C48 H45 B Co2 N16 O42 W12' _chemical_formula_weight 3852.84 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 13.270(5) _cell_length_b 15.060(5) _cell_length_c 21.186(5) _cell_angle_alpha 91.802(5) _cell_angle_beta 103.098(5) _cell_angle_gamma 112.440(5) _cell_volume 3779(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.386 _exptl_crystal_F_000 3430 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 18.706 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.007 _exptl_absorpt_correction_T_max 0.016 _exptl_absorpt_process_details ? _exptl_special_details ; During the refinement, the restraint command 'ISOR' or 'simu' is used to refine the non-H atoms with ADP problems. These atoms are as follows: O15 O20 N7 N11 N16 C2 C4 C28 C47 C48 N10 N15 C1 C12 C14 C16 C23 C37 O6 C5 C9 N5 C7 C26 O21 C22 O13 O41 C31 C40 C41 O27 N10 C2 C4 C6 and N4. The command 'delu' was used to solve the non-H atoms with 'Large Hirshfeld Difference...' problems. These atoms are as follows: C10 C48 N4 C2 C6 C9 N14 C15 C4. These restraint refinement leads to a relatively high restraint value 269. In the final refinement, the water molecule could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced by using the SQUEEZE routine. The SQUEEZE programe indicats that there is at least one solvent water molecule in the crystal structure. This water molecule was directly included in the final molecular formula based on the elemental analysis, TG and SQUEEZE analysis. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19648 _diffrn_reflns_av_unetI/netI 0.0913 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.995 _diffrn_reflns_theta_max 25.289 _diffrn_reflns_theta_full 25.240 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_point_group_measured_fraction_full 0.986 _reflns_number_total 13465 _reflns_number_gt 9245 _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-2013 (Sheldrick, 2013)' _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^)+(0.0758P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13465 _refine_ls_number_parameters 1067 _refine_ls_number_restraints 269 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 159.3 26.7 2 0.393 0.343 0.947 9.3 0.7 3 0.607 0.656 0.053 9.3 1.1 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 W1 W 0.17981(7) 0.87030(6) -1.93504(3) 0.0207(2) Uani 1 1 d . . . . . W2 W 0.05527(7) 0.98134(6) -1.83870(3) 0.0195(2) Uani 1 1 d . . . . . W3 W 0.43259(7) 1.00880(6) -1.84119(3) 0.01894(19) Uani 1 1 d . . . . . W4 W 0.40404(7) 0.76127(6) -1.68866(3) 0.0226(2) Uani 1 1 d . . . . . W5 W 0.28921(7) 0.86434(6) -1.60077(3) 0.01869(19) Uani 1 1 d . . . . . W6 W 0.30532(7) 1.11864(6) -1.74239(3) 0.01669(18) Uani 1 1 d . . . . . W7 W 0.48882(7) 1.00109(6) -1.66617(3) 0.01709(19) Uani 1 1 d . . . . . W8 W 0.10196(7) 0.97619(6) -1.67980(3) 0.01874(19) Uani 1 1 d . . . . . W9 W 0.12639(8) 0.61639(6) -1.79587(4) 0.0280(2) Uani 1 1 d . . . . . W10 W 0.01117(7) 0.71352(6) -1.70541(4) 0.0246(2) Uani 1 1 d . . . . . W11 W 0.35220(8) 0.76998(6) -1.86481(4) 0.0256(2) Uani 1 1 d . . . . . W12 W -0.04580(8) 0.71768(6) -1.86539(4) 0.0269(2) Uani 1 1 d . . . . . Co1 Co 0.2936(2) 0.77684(19) -1.43723(11) 0.0163(6) Uani 1 1 d . . . . . Co2 Co 0.8027(2) 1.0299(2) -0.90971(11) 0.0226(6) Uani 1 1 d . . . . . O1 O 0.6489(12) 1.0484(13) -0.9468(6) 0.042(4) Uani 1 1 d . . . . . O2 O -0.0386(12) 1.0199(10) -1.8866(6) 0.027(3) Uani 1 1 d . . . . . O3 O 0.1344(11) 0.8794(9) -2.0173(6) 0.025(3) Uani 1 1 d . . . . . O4 O 0.6157(11) 1.0888(9) -1.6269(5) 0.022(3) Uani 1 1 d . . . . . O5 O 0.1075(13) 0.4982(10) -1.8090(7) 0.039(4) Uani 1 1 d . . . . . O6 O 0.2945(10) 0.8589(9) -1.5186(6) 0.018(3) Uani 1 1 d . U . . . O7 O 0.1298(12) 0.9584(10) -1.8984(6) 0.028(3) Uani 1 1 d . . . . . O8 O 0.0363(11) 1.0063(10) -1.6270(6) 0.027(3) Uani 1 1 d . . . . . O9 O -0.0965(12) 0.6897(11) -1.7897(6) 0.032(4) Uani 1 1 d . . . . . O10 O -0.0035(13) 0.6091(10) -1.8618(6) 0.036(4) Uani 1 1 d . . . . . O11 O 0.2560(12) 0.7890(9) -1.9429(6) 0.024(3) Uani 1 1 d . . . . . O12 O 0.0374(13) 0.6042(10) -1.7341(6) 0.029(4) Uani 1 1 d . . . . . O13 O 0.4586(12) 0.8957(10) -1.8648(6) 0.029(3) Uani 1 1 d . U . . . O14 O 0.3614(11) 0.7776(10) -1.6101(6) 0.022(3) Uani 1 1 d . . . . . O15 O 0.4987(10) 1.0024(9) -1.7532(6) 0.018(3) Uani 1 1 d . U . . . O16 O -0.0783(12) 0.6601(12) -1.6591(6) 0.040(4) Uani 1 1 d . . . . . O17 O 0.3760(12) 1.2409(10) -1.7314(6) 0.027(3) Uani 1 1 d . . . . . O18 O -0.0310(12) 0.8494(10) -1.8505(6) 0.030(3) Uani 1 1 d . . . . . O19 O 0.2162(10) 0.9479(9) -1.6216(5) 0.021(3) Uani 1 1 d . . . . . O20 O 0.4078(11) 1.0798(9) -1.6833(6) 0.024(3) Uani 1 1 d . U . . . O21 O 0.2205(11) 0.6712(9) -1.8519(6) 0.025(3) Uani 1 1 d . U . . . O22 O 0.1759(10) 1.1066(9) -1.8097(5) 0.018(3) Uani 1 1 d . . . . . O23 O 0.4304(12) 0.9671(10) -1.5911(6) 0.026(3) Uani 1 1 d . . . . . O24 O 0.4191(12) 0.7721(9) -1.7751(5) 0.024(3) Uani 1 1 d . . . . . O25 O 0.5464(12) 1.0950(10) -1.8607(6) 0.030(3) Uani 1 1 d . . . . . O26 O 0.1218(11) 0.7708(9) -1.7776(6) 0.025(3) Uani 1 1 d . . . . . O27 O 0.3713(11) 1.0884(9) -1.8083(6) 0.020(3) Uani 1 1 d . U . . . O28 O 0.2759(10) 0.8773(9) -1.8272(5) 0.017(3) Uani 1 1 d . . . . . O29 O 0.0541(12) 0.7688(10) -1.9217(6) 0.030(4) Uani 1 1 d . . . . . O30 O 0.0138(10) 0.9951(9) -1.7589(5) 0.018(3) Uani 1 1 d . . . . . O31 O 0.2584(13) 0.6634(10) -1.7247(6) 0.030(4) Uani 1 1 d . . . . . O32 O 0.3243(10) 0.9773(9) -1.9223(5) 0.016(3) Uani 1 1 d . . . . . O33 O 0.0184(10) 0.8420(9) -1.6969(6) 0.022(3) Uani 1 1 d . . . . . O34 O 0.2160(11) 1.1028(9) -1.6808(6) 0.022(3) Uani 1 1 d . . . . . O35 O 0.5225(11) 0.8870(10) -1.6614(5) 0.022(3) Uani 1 1 d . . . . . O36 O 0.1502(12) 0.7611(9) -1.6398(6) 0.023(3) Uani 1 1 d . . . . . O37 O 0.4054(15) 0.7021(12) -1.9024(6) 0.040(4) Uani 1 1 d . . . . . O38 O -0.1725(12) 0.6676(11) -1.9231(7) 0.042(4) Uani 1 1 d . . . . . O39 O 0.4786(14) 0.6936(12) -1.6620(6) 0.043(4) Uani 1 1 d . . . . . O40 O 0.1871(10) 0.9490(9) -1.7615(5) 0.015(3) Uani 1 1 d . . . . . O41 O 0.3156(10) 0.8735(8) -1.7077(5) 0.013(3) Uani 1 1 d . U . . . C1 C -0.096(2) 0.3115(19) -1.8040(12) 0.049(6) Uani 1 1 d . U . . . H1A H -0.1021 0.3703 -1.7972 0.059 Uiso 1 1 calc R U . . . C3 C -0.2038(15) 0.8007(16) -1.4616(9) 0.026(5) Uani 1 1 d . . . . . H3A H -0.2086 0.7612 -1.4286 0.031 Uiso 1 1 calc R U . . . C5 C 0.662(3) 0.623(2) -0.6792(15) 0.069(8) Uani 1 1 d . U . . . H5A H 0.6850 0.6073 -0.6379 0.083 Uiso 1 1 calc R U . . . C7 C 0.593(3) 0.659(3) -0.8017(19) 0.093(10) Uani 1 1 d . U . . . H7A H 0.5702 0.6683 -0.8450 0.112 Uiso 1 1 calc R U . . . C8 C 0.673(2) 0.738(2) -0.7609(16) 0.068(9) Uani 1 1 d . . . . . C9 C 0.548(4) 0.580(4) -0.789(2) 0.119(9) Uani 1 1 d . U . . . C10 C 0.711(3) 0.717(3) -0.6932(16) 0.082(11) Uani 1 1 d . . . . . H10A H 0.7660 0.7653 -0.6612 0.098 Uiso 1 1 calc R U . . . C11 C 0.711(2) 0.913(2) -0.7405(14) 0.063(8) Uani 1 1 d . . . . . H11A H 0.6954 0.9177 -0.7002 0.076 Uiso 1 1 calc R U . . . C12 C -0.170(2) 0.2322(17) -1.8457(11) 0.040(6) Uani 1 1 d . U . . . H12A H -0.2396 0.2266 -1.8708 0.048 Uiso 1 1 calc R U . . . C13 C 0.736(2) 0.979(2) -0.7787(10) 0.046(7) Uani 1 1 d . . . . . H13A H 0.7427 1.0410 -0.7670 0.056 Uiso 1 1 calc R U . . . C14 C 0.065(3) 0.533(2) -1.5762(14) 0.065(8) Uani 1 1 d . U . . . H14A H -0.0078 0.4905 -1.5982 0.078 Uiso 1 1 calc R U . . . C15 C 0.742(2) 0.864(2) -0.8269(13) 0.050(6) Uani 1 1 d . U . . . H15A H 0.7547 0.8255 -0.8567 0.059 Uiso 1 1 calc R U . . . C16 C 0.420(2) 0.6535(17) -1.0566(12) 0.042(6) Uani 1 1 d . U . . . H16A H 0.4389 0.6579 -1.0112 0.051 Uiso 1 1 calc R U . . . C17 C 0.283(2) 0.399(2) -1.6775(12) 0.063(9) Uani 1 1 d . . . . . H17A H 0.3535 0.3999 -1.6780 0.075 Uiso 1 1 calc R U . . . C18 C 0.625(2) 0.8453(15) -0.9979(10) 0.038(6) Uani 1 1 d . . . . . H18A H 0.5695 0.8475 -0.9782 0.046 Uiso 1 1 calc R U . . . C19 C 0.7031(19) 0.8040(15) -1.0667(9) 0.032(5) Uani 1 1 d . . . . . H19A H 0.7144 0.7748 -1.1023 0.038 Uiso 1 1 calc R U . . . C20 C -0.1903(19) 0.9176(17) -1.5613(10) 0.035(6) Uani 1 1 d . . . . . H20A H -0.1852 0.9549 -1.5955 0.043 Uiso 1 1 calc R U . . . C21 C 0.1123(17) 0.7982(16) -1.3733(9) 0.028(5) Uani 1 1 d . . . . . H21A H 0.1503 0.7913 -1.3323 0.033 Uiso 1 1 calc R U . . . C22 C -0.433(2) 0.6995(17) -1.4478(11) 0.040(6) Uani 1 1 d . U . . . H22A H -0.4021 0.6532 -1.4476 0.047 Uiso 1 1 calc R U . . . C23 C 0.090(2) 0.6015(17) -1.5288(11) 0.038(5) Uani 1 1 d . U . . . H23A H 0.0381 0.6151 -1.5118 0.045 Uiso 1 1 calc R U . . . C24 C -0.526(2) 0.6926(18) -1.4272(11) 0.040(6) Uani 1 1 d . . . . . H24A H -0.5648 0.6433 -1.4055 0.048 Uiso 1 1 calc R U . . . C25 C 0.3435(17) 0.7210(15) -1.2915(8) 0.023(5) Uani 1 1 d . . . . . H25A H 0.3911 0.7843 -1.2732 0.028 Uiso 1 1 calc R U . . . C26 C -0.2853(19) 0.8868(16) -1.5414(10) 0.032(5) Uani 1 1 d . U . . . H26A H -0.3441 0.9046 -1.5600 0.038 Uiso 1 1 calc R U . . . C27 C 0.7818(18) 0.8736(15) -1.0215(9) 0.028(5) Uani 1 1 d . . . . . H27A H 0.8584 0.8995 -1.0198 0.034 Uiso 1 1 calc R U . . . C28 C -0.4736(16) 0.8249(14) -1.4677(9) 0.021(4) Uani 1 1 d . U . . . H28A H -0.4709 0.8829 -1.4828 0.025 Uiso 1 1 calc R U . . . C29 C -0.0963(17) 0.8952(15) -1.5317(9) 0.027(5) Uani 1 1 d . . . . . H29A H -0.0299 0.9198 -1.5450 0.033 Uiso 1 1 calc R U . . . C30 C -0.036(2) 0.1942(15) -1.8007(10) 0.038(6) Uani 1 1 d . . . . . H30A H 0.0072 0.1587 -1.7877 0.046 Uiso 1 1 calc R U . . . C31 C 0.1898(17) 0.3367(15) -1.7197(9) 0.027(5) Uani 1 1 d . U . . . H31A H 0.1936 0.2882 -1.7461 0.032 Uiso 1 1 calc R U . . . C32 C 0.0809(17) 0.4098(15) -1.6808(9) 0.025(5) Uani 1 1 d . . . . . H32A H 0.0117 0.4132 -1.6830 0.030 Uiso 1 1 calc R U . . . C33 C 0.319(2) 0.5872(16) -1.0896(10) 0.045(6) Uani 1 1 d . . . . . H33A H 0.2716 0.5451 -1.0675 0.053 Uiso 1 1 calc R U . . . C34 C 0.2362(18) 0.5980(16) -1.3593(9) 0.031(5) Uani 1 1 d . . . . . H34A H 0.1935 0.5590 -1.3987 0.038 Uiso 1 1 calc R U . . . C35 C 0.0893(18) 0.3431(15) -1.7244(9) 0.024(5) Uani 1 1 d . . . . . C36 C -0.2944(17) 0.8254(15) -1.4905(9) 0.025(5) Uani 1 1 d . . . . . C37 C 0.2413(17) 0.6064(14) -1.5445(9) 0.025(4) Uani 1 1 d . U . . . H37A H 0.3180 0.6241 -1.5404 0.030 Uiso 1 1 calc R U . . . C38 C 0.0679(18) 0.8068(15) -1.4742(9) 0.028(5) Uani 1 1 d . . . . . H38A H 0.0699 0.8095 -1.5177 0.034 Uiso 1 1 calc R U . . . C39 C 0.4622(15) 0.7115(13) -1.1534(9) 0.020(4) Uani 1 1 d . . . . . H39A H 0.5101 0.7536 -1.1752 0.024 Uiso 1 1 calc R U . . . C40 C 0.2743(18) 0.4656(15) -1.6313(10) 0.030(5) Uani 1 1 d . U . . . H40A H 0.3380 0.5053 -1.5990 0.036 Uiso 1 1 calc R U . . . C41 C 0.0203(16) 0.8154(14) -1.3851(9) 0.024(4) Uani 1 1 d . U . . . H41A H -0.0159 0.8243 -1.3541 0.029 Uiso 1 1 calc R U . . . C42 C 0.360(2) 0.6475(15) -1.1871(8) 0.028(5) Uani 1 1 d . . . . . C43 C -0.1058(16) 0.8377(15) -1.4842(9) 0.023(5) Uani 1 1 d . . . . . C44 C 0.4974(19) 0.7152(15) -1.0854(9) 0.027(5) Uani 1 1 d . . . . . C45 C 0.1768(17) 0.4709(14) -1.6341(9) 0.021(4) Uani 1 1 d . . . . . C46 C 0.286(2) 0.5818(14) -1.1558(9) 0.029(5) Uani 1 1 d . . . . . H46A H 0.2162 0.5360 -1.1797 0.035 Uiso 1 1 calc R U . . . C47 C 0.2496(17) 0.5637(15) -1.3013(9) 0.026(5) Uani 1 1 d . U . . . H47A H 0.2187 0.4999 -1.2931 0.031 Uiso 1 1 calc R U . . . C48 C 0.575(3) 0.552(3) -0.7287(16) 0.083(9) Uani 1 1 d . U . . . H48A H 0.5373 0.4891 -0.7205 0.099 Uiso 1 1 calc R U . . . N1 N -0.1299(15) 0.1604(12) -1.8471(7) 0.028(4) Uani 1 1 d . . . . . N2 N 0.2917(14) 0.6953(12) -1.3539(7) 0.022(4) Uani 1 1 d . . . . . N3 N 0.3199(12) 0.6453(11) -1.2567(7) 0.019(4) Uani 1 1 d . . . . . N5 N 0.6016(15) 0.7828(12) -1.0516(8) 0.028(4) Uani 1 1 d . U . . . N6 N 0.7334(15) 0.9033(12) -0.9759(7) 0.029(4) Uani 1 1 d . . . . . N7 N -0.3938(13) 0.7878(11) -1.4685(7) 0.021(4) Uani 1 1 d . U . . . N8 N 0.1445(13) 0.7918(11) -1.4293(7) 0.020(4) Uani 1 1 d . . . . . N9 N -0.0133(14) 0.8178(12) -1.4511(8) 0.027(4) Uani 1 1 d . . . . . N11 N 0.2046(12) 0.6501(11) -1.5079(7) 0.014(3) Uani 1 1 d . U . . . N12 N 0.1632(14) 0.5349(11) -1.5883(7) 0.024(4) Uani 1 1 d . . . . . N13 N 0.7142(18) 0.8360(16) -0.7744(9) 0.045(5) Uani 1 1 d . . . . . N14 N 0.751(2) 0.9544(15) -0.8347(8) 0.052(6) Uani 1 1 d . U . . . N15 N -0.0079(14) 0.2854(12) -1.7732(8) 0.027(4) Uani 1 1 d . U . . . N16 N -0.5531(13) 0.7689(11) -1.4434(7) 0.018(3) Uani 1 1 d . U . . . N4 N 0.446(3) 0.518(2) -0.8356(16) 0.147(6) Uani 1 1 d G U . . . C6 C 0.442(3) 0.490(2) -0.9000(18) 0.149(6) Uani 1 1 d G U . . . H6A H 0.5033 0.5043 -0.9177 0.179 Uiso 1 1 calc R U . . . N10 N 0.329(3) 0.438(2) -0.9331(13) 0.152(6) Uani 1 1 d G U . . . C4 C 0.263(3) 0.434(2) -0.8891(19) 0.149(6) Uani 1 1 d G U . . . H4A H 0.1852 0.4029 -0.8984 0.178 Uiso 1 1 calc R U . . . C2 C 0.336(3) 0.483(2) -0.8289(16) 0.151(6) Uani 1 1 d G U . . . H2A H 0.3147 0.4913 -0.7909 0.181 Uiso 1 1 calc R U . . . B1 B 0.2248(19) 0.8667(16) -1.7690(10) 0.020 Uiso 1 1 d . U . . . 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 W1 0.0309(5) 0.0264(5) 0.0067(3) 0.0014(3) -0.0002(3) 0.0165(4) W2 0.0225(4) 0.0257(5) 0.0122(4) 0.0022(3) -0.0025(3) 0.0156(4) W3 0.0233(4) 0.0291(5) 0.0086(3) 0.0021(3) 0.0030(3) 0.0157(4) W4 0.0356(5) 0.0298(5) 0.0126(4) 0.0047(3) 0.0037(4) 0.0251(4) W5 0.0251(4) 0.0282(5) 0.0069(3) 0.0036(3) 0.0018(3) 0.0162(4) W6 0.0187(4) 0.0190(4) 0.0147(4) 0.0007(3) 0.0016(3) 0.0117(3) W7 0.0189(4) 0.0263(5) 0.0079(3) 0.0005(3) -0.0009(3) 0.0136(4) W8 0.0231(4) 0.0267(5) 0.0120(4) 0.0038(3) 0.0042(3) 0.0160(4) W9 0.0431(6) 0.0204(5) 0.0203(4) 0.0014(3) 0.0029(4) 0.0155(4) W10 0.0274(5) 0.0235(5) 0.0175(4) 0.0023(3) 0.0023(4) 0.0065(4) W11 0.0462(6) 0.0326(5) 0.0126(4) 0.0048(3) 0.0090(4) 0.0304(5) W12 0.0299(5) 0.0241(5) 0.0178(4) 0.0004(3) -0.0039(4) 0.0072(4) Co1 0.0146(13) 0.0270(15) 0.0099(11) 0.0003(10) 0.0007(10) 0.0127(12) Co2 0.0273(15) 0.0282(16) 0.0112(12) -0.0012(11) -0.0010(11) 0.0136(13) O1 0.021(8) 0.090(13) 0.023(8) 0.002(8) 0.009(7) 0.029(9) O2 0.031(8) 0.030(8) 0.019(7) 0.005(6) -0.008(6) 0.018(7) O3 0.029(8) 0.024(8) 0.019(7) 0.000(6) -0.001(6) 0.012(7) O4 0.036(8) 0.026(8) 0.006(6) 0.008(5) 0.010(6) 0.012(7) O5 0.051(10) 0.022(9) 0.032(8) -0.004(7) -0.001(8) 0.008(8) O6 0.018(3) 0.018(3) 0.018(3) 0.0026(11) 0.0045(12) 0.0074(15) O7 0.035(9) 0.030(9) 0.014(6) 0.002(6) -0.003(6) 0.014(7) O8 0.027(8) 0.040(9) 0.014(6) -0.005(6) 0.003(6) 0.014(7) O9 0.033(9) 0.045(10) 0.020(7) 0.010(7) 0.010(7) 0.017(8) O10 0.052(10) 0.025(9) 0.020(7) -0.005(6) -0.011(7) 0.015(8) O11 0.043(9) 0.028(8) 0.015(6) 0.014(6) 0.009(6) 0.027(7) O12 0.058(10) 0.026(8) 0.014(6) 0.005(6) 0.011(7) 0.026(8) O13 0.030(3) 0.029(3) 0.029(3) 0.0033(11) 0.0074(13) 0.0122(16) O14 0.033(8) 0.032(8) 0.015(6) 0.003(6) 0.006(6) 0.028(7) O15 0.018(3) 0.018(3) 0.018(3) 0.0027(11) 0.0041(12) 0.0077(15) O16 0.032(9) 0.060(11) 0.020(7) 0.018(7) 0.001(7) 0.013(8) O17 0.031(8) 0.036(9) 0.021(7) -0.001(6) 0.011(6) 0.017(7) O18 0.029(8) 0.043(9) 0.009(6) 0.003(6) 0.000(6) 0.009(7) O19 0.017(7) 0.036(9) 0.009(6) -0.002(6) -0.004(5) 0.013(6) O20 0.024(3) 0.025(3) 0.024(3) 0.0031(11) 0.0061(13) 0.0098(15) O21 0.025(3) 0.025(3) 0.025(3) 0.0032(11) 0.0063(13) 0.0102(16) O22 0.021(7) 0.019(7) 0.014(6) 0.005(5) -0.003(6) 0.013(6) O23 0.033(8) 0.039(9) 0.011(6) -0.001(6) -0.001(6) 0.025(7) O24 0.047(9) 0.028(8) 0.012(6) 0.007(6) 0.015(6) 0.024(7) O25 0.041(9) 0.033(9) 0.029(8) 0.004(6) 0.011(7) 0.027(8) O26 0.028(8) 0.021(8) 0.018(7) 0.001(6) -0.011(6) 0.012(7) O27 0.021(3) 0.021(3) 0.020(3) 0.0023(11) 0.0055(12) 0.0082(15) O28 0.022(7) 0.020(7) 0.015(6) -0.001(5) 0.004(6) 0.013(6) O29 0.045(9) 0.023(8) 0.021(7) 0.000(6) -0.011(7) 0.022(7) O30 0.018(7) 0.029(8) 0.014(6) 0.006(6) 0.006(6) 0.016(6) O31 0.051(10) 0.033(9) 0.014(7) 0.010(6) 0.002(7) 0.029(8) O32 0.014(7) 0.025(8) 0.010(6) 0.001(5) -0.004(5) 0.015(6) O33 0.011(7) 0.026(8) 0.019(7) 0.001(6) 0.005(6) -0.003(6) O34 0.025(8) 0.014(7) 0.022(7) -0.006(6) 0.002(6) 0.005(6) O35 0.034(8) 0.038(9) 0.010(6) 0.008(6) 0.009(6) 0.030(7) O36 0.040(9) 0.016(8) 0.018(7) 0.008(6) 0.008(6) 0.015(7) O37 0.074(12) 0.062(11) 0.018(7) 0.014(7) 0.025(8) 0.056(10) O38 0.027(9) 0.038(10) 0.035(9) 0.006(7) -0.012(7) -0.004(7) O39 0.068(12) 0.058(11) 0.016(7) 0.002(7) 0.000(8) 0.046(10) O40 0.015(7) 0.020(7) 0.007(6) -0.003(5) 0.005(5) 0.002(6) O41 0.013(3) 0.013(3) 0.013(3) 0.0017(11) 0.0030(12) 0.0053(14) C1 0.049(6) 0.049(6) 0.049(6) 0.0061(13) 0.0125(19) 0.020(3) C3 0.012(10) 0.051(15) 0.022(10) 0.014(10) 0.006(9) 0.020(10) C5 0.069(8) 0.069(8) 0.069(8) 0.0091(15) 0.018(2) 0.028(3) C7 0.093(10) 0.093(10) 0.093(10) 0.0124(17) 0.024(3) 0.037(4) C8 0.043(17) 0.07(2) 0.09(2) 0.008(19) 0.017(17) 0.021(17) C9 0.119(9) 0.119(9) 0.119(9) 0.0158(16) 0.031(3) 0.048(4) C10 0.10(3) 0.08(3) 0.08(2) -0.001(19) 0.03(2) 0.06(2) C11 0.06(2) 0.09(3) 0.056(18) 0.022(18) 0.023(16) 0.05(2) C12 0.040(6) 0.040(6) 0.040(6) 0.0052(13) 0.0100(18) 0.016(2) C13 0.072(19) 0.057(18) 0.015(11) 0.004(11) 0.006(12) 0.033(16) C14 0.064(8) 0.065(8) 0.065(8) 0.0081(14) 0.017(2) 0.026(3) C15 0.037(14) 0.051(13) 0.052(15) 0.006(13) 0.014(13) 0.006(13) C16 0.042(6) 0.042(6) 0.042(6) 0.0056(13) 0.0108(18) 0.017(2) C17 0.040(16) 0.12(3) 0.052(16) -0.001(16) 0.014(14) 0.052(18) C18 0.037(14) 0.024(13) 0.032(12) 0.000(10) -0.013(11) 0.002(11) C19 0.051(15) 0.025(13) 0.010(9) -0.006(9) 0.006(10) 0.006(11) C20 0.046(15) 0.047(16) 0.022(11) 0.014(10) 0.015(11) 0.024(13) C21 0.031(12) 0.059(16) 0.017(10) 0.014(10) 0.012(9) 0.039(12) C22 0.039(6) 0.040(6) 0.040(6) 0.0053(13) 0.0102(17) 0.016(2) C23 0.038(5) 0.038(5) 0.038(5) 0.0043(12) 0.0099(17) 0.015(2) C24 0.041(14) 0.051(16) 0.046(14) 0.022(12) 0.027(12) 0.028(13) C25 0.031(12) 0.027(12) 0.014(9) 0.007(8) 0.006(9) 0.015(10) C26 0.032(5) 0.032(5) 0.032(5) 0.0043(12) 0.0081(16) 0.013(2) C27 0.027(12) 0.033(13) 0.032(12) 0.015(10) 0.010(10) 0.018(11) C28 0.021(4) 0.021(4) 0.021(4) 0.0026(12) 0.0052(15) 0.0086(19) C29 0.024(11) 0.041(14) 0.016(10) 0.001(9) 0.003(9) 0.014(10) C30 0.048(15) 0.025(13) 0.030(12) -0.011(10) -0.009(11) 0.014(12) C31 0.027(5) 0.027(5) 0.027(5) 0.0033(12) 0.0068(15) 0.011(2) C32 0.027(12) 0.030(13) 0.024(10) 0.010(9) 0.006(9) 0.019(10) C33 0.060(17) 0.028(14) 0.027(12) 0.007(10) 0.016(12) -0.005(12) C34 0.033(13) 0.040(15) 0.016(10) 0.006(10) -0.007(9) 0.016(11) C35 0.040(13) 0.030(13) 0.017(9) 0.016(9) 0.013(9) 0.024(11) C36 0.030(12) 0.031(13) 0.021(10) 0.003(9) 0.009(9) 0.020(10) C37 0.025(5) 0.025(5) 0.025(5) 0.0031(12) 0.0065(15) 0.010(2) C38 0.032(12) 0.039(14) 0.020(10) 0.007(9) 0.012(10) 0.017(11) C39 0.012(10) 0.010(10) 0.026(10) 0.007(8) -0.010(9) 0.001(8) C40 0.030(5) 0.030(5) 0.030(5) 0.0036(12) 0.0077(16) 0.012(2) C41 0.024(4) 0.024(4) 0.024(4) 0.0033(12) 0.0060(15) 0.010(2) C42 0.058(15) 0.035(14) 0.009(9) 0.010(9) 0.010(10) 0.037(12) C43 0.011(10) 0.034(13) 0.029(11) 0.016(9) 0.001(9) 0.014(9) C44 0.047(14) 0.023(12) 0.015(9) 0.005(8) 0.010(10) 0.018(11) C45 0.027(11) 0.019(11) 0.030(11) 0.005(9) 0.014(9) 0.018(9) C46 0.047(14) 0.014(11) 0.027(11) 0.004(9) 0.010(11) 0.011(10) C47 0.026(5) 0.026(5) 0.026(5) 0.0034(12) 0.0062(15) 0.010(2) C48 0.083(9) 0.083(9) 0.083(9) 0.0109(16) 0.021(3) 0.033(4) N1 0.042(11) 0.023(10) 0.018(8) -0.009(7) 0.000(8) 0.019(9) N2 0.027(9) 0.035(11) 0.015(8) 0.017(7) 0.010(7) 0.019(9) N3 0.014(8) 0.013(9) 0.021(8) 0.001(7) -0.003(7) 0.003(7) N5 0.028(4) 0.028(4) 0.028(4) 0.0038(11) 0.0072(14) 0.0111(19) N6 0.042(11) 0.022(10) 0.017(8) -0.007(7) -0.005(8) 0.014(9) N7 0.021(4) 0.021(4) 0.021(4) 0.0027(11) 0.0055(13) 0.0087(17) N8 0.017(9) 0.025(10) 0.017(8) 0.005(7) 0.001(7) 0.009(8) N9 0.025(10) 0.039(11) 0.026(9) -0.004(8) 0.009(8) 0.022(9) N11 0.014(3) 0.014(3) 0.014(3) 0.0014(11) 0.0038(13) 0.0057(16) N12 0.026(9) 0.019(9) 0.019(8) -0.011(7) -0.002(7) 0.007(8) N13 0.053(14) 0.052(15) 0.047(12) 0.032(11) 0.031(11) 0.026(12) N14 0.090(18) 0.042(12) 0.020(10) -0.001(9) 0.024(11) 0.016(13) N15 0.027(4) 0.027(4) 0.026(4) 0.0032(11) 0.0068(14) 0.0105(18) N16 0.018(3) 0.018(3) 0.018(3) 0.0020(11) 0.0048(13) 0.0074(16) N4 0.147(6) 0.147(6) 0.147(6) 0.0192(13) 0.0378(19) 0.059(3) C6 0.149(6) 0.149(6) 0.149(6) 0.0196(13) 0.0385(19) 0.060(3) N10 0.152(6) 0.152(6) 0.152(6) 0.0199(13) 0.0391(19) 0.060(3) C4 0.149(6) 0.149(6) 0.149(6) 0.0194(13) 0.0385(19) 0.059(3) C2 0.151(6) 0.151(6) 0.151(6) 0.0198(13) 0.0388(19) 0.060(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 W1 O3 1.739(12) . ? W1 O29 1.869(16) . ? W1 O11 1.886(12) . ? W1 O7 1.909(13) . ? W1 O32 1.930(13) . ? W1 O28 2.328(11) . ? W2 O2 1.713(11) . ? W2 O18 1.850(15) . ? W2 O7 1.870(14) . ? W2 O22 1.917(13) . ? W2 O30 1.922(11) . ? W2 O40 2.319(11) . ? W3 O25 1.720(16) . ? W3 O27 1.879(12) . ? W3 O32 1.885(10) . ? W3 O15 1.894(11) . ? W3 O13 1.935(13) . ? W3 O28 2.346(14) . ? W4 O39 1.700(13) . ? W4 O31 1.891(16) . ? W4 O24 1.892(11) . ? W4 O35 1.907(15) . ? W4 O14 1.914(12) . ? W4 O41 2.396(11) . ? W5 O6 1.731(12) . ? W5 O19 1.869(12) . ? W5 O23 1.882(15) . ? W5 O36 1.882(14) . ? W5 O14 1.920(11) . ? W5 O41 2.370(11) . ? W6 O17 1.697(14) . ? W6 O20 1.908(12) . ? W6 O22 1.912(11) . ? W6 O34 1.915(13) . ? W6 O27 1.935(12) . ? W6 O40 2.395(12) . ? W7 O4 1.694(14) . ? W7 O20 1.874(12) . ? W7 O15 1.879(12) . ? W7 O23 1.923(13) . ? W7 O35 1.934(11) . ? W7 O41 2.314(12) . ? W8 O8 1.711(12) . ? W8 O33 1.873(13) . ? W8 O30 1.911(11) . ? W8 O19 1.917(11) . ? W8 O34 1.934(13) . ? W8 O40 2.374(11) . ? W9 O5 1.705(14) . ? W9 O21 1.896(14) . ? W9 O31 1.906(13) . ? W9 O10 1.920(13) . ? W9 O12 1.922(14) . ? W9 O26 2.371(12) . ? W10 O16 1.693(15) . ? W10 O36 1.901(13) . ? W10 O33 1.901(13) . ? W10 O12 1.916(12) . ? W10 O9 1.943(13) . ? W10 O26 2.319(14) . ? W11 O37 1.711(12) . ? W11 O13 1.880(15) . ? W11 O21 1.897(14) . ? W11 O24 1.901(11) . ? W11 O11 1.950(11) . ? W11 O28 2.409(11) . ? W12 O38 1.713(14) . ? W12 O9 1.874(13) . ? W12 O10 1.920(13) . ? W12 O18 1.926(14) . ? W12 O29 1.942(16) . ? W12 O26 2.392(12) . ? Co1 N16 2.115(15) 1_655 ? Co1 N8 2.118(15) . ? Co1 N11 2.140(14) . ? Co1 O4 2.148(13) 2_672 ? Co1 O6 2.153(12) . ? Co1 N2 2.182(15) . ? Co2 N14 2.07(2) . ? Co2 N6 2.086(16) . ? Co2 N1 2.092(15) 1_666 ? Co2 O2 2.116(13) 1_656 ? Co2 O1 2.141(13) . ? Co2 O3 2.190(14) 2_672 ? O2 Co2 2.116(13) 1_454 ? O3 Co2 2.190(14) 2_672 ? O4 Co1 2.148(13) 2_672 ? O26 B1 1.53(3) . ? O28 B1 1.52(2) . ? O40 B1 1.52(2) . ? O41 B1 1.53(2) . ? C1 C12 1.35(3) . ? C1 N15 1.40(3) . ? C1 H1A 0.9300 . ? C3 C43 1.41(3) . ? C3 C36 1.41(2) . ? C3 H3A 0.9300 . ? C5 C10 1.38(4) . ? C5 C48 1.42(4) . ? C5 H5A 0.9300 . ? C7 C9 1.19(5) . ? C7 C8 1.36(4) . ? C7 H7A 0.9300 . ? C8 N13 1.42(4) . ? C8 C10 1.50(4) . ? C9 C48 1.36(5) . ? C9 N4 1.43(5) . ? C10 H10A 0.9300 . ? C11 C13 1.28(4) . ? C11 N13 1.37(3) . ? C11 H11A 0.9300 . ? C12 N1 1.37(3) . ? C12 H12A 0.9300 . ? C13 N14 1.31(3) . ? C13 C15 2.01(4) . ? C13 H13A 0.9300 . ? C14 C23 1.30(3) . ? C14 N12 1.38(3) . ? C14 H14A 0.9300 . ? C15 N13 1.29(3) . ? C15 N14 1.34(3) . ? C15 H15A 0.9300 . ? C16 C33 1.34(3) . ? C16 C44 1.37(3) . ? C16 H16A 0.9300 . ? C17 C31 1.33(3) . ? C17 C40 1.43(3) . ? C17 H17A 0.9300 . ? C18 N6 1.33(3) . ? C18 N5 1.35(3) . ? C18 H18A 0.9300 . ? C19 C27 1.33(3) . ? C19 N5 1.38(3) . ? C19 H19A 0.9300 . ? C20 C26 1.34(3) . ? C20 C29 1.43(3) . ? C20 H20A 0.9300 . ? C21 C41 1.32(2) . ? C21 N8 1.36(2) . ? C21 H21A 0.9300 . ? C22 N7 1.36(3) . ? C22 C24 1.37(3) . ? C22 H22A 0.9300 . ? C23 N11 1.37(3) . ? C23 H23A 0.9300 . ? C24 N16 1.36(2) . ? C24 H24A 0.9300 . ? C25 N2 1.31(2) . ? C25 N3 1.35(2) . ? C25 H25A 0.9300 . ? C26 C36 1.44(3) . ? C26 H26A 0.9300 . ? C27 N6 1.42(3) . ? C27 H27A 0.9300 . ? C28 N16 1.30(2) . ? C28 N7 1.38(2) . ? C28 H28A 0.9300 . ? C29 C43 1.34(3) . ? C29 H29A 0.9300 . ? C30 N1 1.31(2) . ? C30 N15 1.35(2) . ? C30 H30A 0.9300 . ? C31 C35 1.36(3) . ? C31 H31A 0.9300 . ? C32 C45 1.39(3) . ? C32 C35 1.40(3) . ? C32 H32A 0.9300 . ? C33 C46 1.36(3) . ? C33 H33A 0.9300 . ? C34 C47 1.35(3) . ? C34 N2 1.35(3) . ? C34 H34A 0.9300 . ? C35 N15 1.40(3) . ? C36 N7 1.41(3) . ? C37 N11 1.29(2) . ? C37 N12 1.32(2) . ? C37 H37A 0.9300 . ? C38 N8 1.32(2) . ? C38 N9 1.34(2) . ? C38 H38A 0.9300 . ? C39 C42 1.34(3) . ? C39 C44 1.40(2) . ? C39 H39A 0.9300 . ? C40 C45 1.31(3) . ? C40 H40A 0.9300 . ? C41 N9 1.37(2) . ? C41 H41A 0.9300 . ? C42 C46 1.41(3) . ? C42 N3 1.44(2) . ? C43 N9 1.41(2) . ? C44 N5 1.37(3) . ? C45 N12 1.43(2) . ? C46 H46A 0.9300 . ? C47 N3 1.39(2) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? N1 Co2 2.092(15) 1_444 ? N16 Co1 2.115(15) 1_455 ? N4 C2 1.396(19) . ? N4 C6 1.396(19) . ? C6 N10 1.40(2) . ? C6 H6A 0.9300 . ? N10 C4 1.396(19) . ? C4 C2 1.396(19) . ? C4 H4A 0.9300 . ? C2 H2A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 W1 O29 101.8(6) . . ? O3 W1 O11 98.9(5) . . ? O29 W1 O11 92.9(6) . . ? O3 W1 O7 99.0(5) . . ? O29 W1 O7 88.1(6) . . ? O11 W1 O7 161.4(5) . . ? O3 W1 O32 94.3(6) . . ? O29 W1 O32 163.8(5) . . ? O11 W1 O32 86.4(6) . . ? O7 W1 O32 87.4(6) . . ? O3 W1 O28 168.6(6) . . ? O29 W1 O28 89.3(5) . . ? O11 W1 O28 77.5(4) . . ? O7 W1 O28 83.9(4) . . ? O32 W1 O28 74.7(5) . . ? O2 W2 O18 100.1(6) . . ? O2 W2 O7 101.8(6) . . ? O18 W2 O7 88.1(6) . . ? O2 W2 O22 96.8(6) . . ? O18 W2 O22 163.1(5) . . ? O7 W2 O22 89.1(6) . . ? O2 W2 O30 96.3(6) . . ? O18 W2 O30 90.3(6) . . ? O7 W2 O30 161.9(5) . . ? O22 W2 O30 87.3(5) . . ? O2 W2 O40 170.9(5) . . ? O18 W2 O40 86.1(5) . . ? O7 W2 O40 85.0(5) . . ? O22 W2 O40 77.0(4) . . ? O30 W2 O40 76.9(4) . . ? O25 W3 O27 100.3(6) . . ? O25 W3 O32 100.1(6) . . ? O27 W3 O32 91.7(5) . . ? O25 W3 O15 100.3(6) . . ? O27 W3 O15 87.2(5) . . ? O32 W3 O15 159.4(6) . . ? O25 W3 O13 98.1(6) . . ? O27 W3 O13 161.5(6) . . ? O32 W3 O13 87.3(5) . . ? O15 W3 O13 87.3(5) . . ? O25 W3 O28 172.0(5) . . ? O27 W3 O28 86.5(5) . . ? O32 W3 O28 75.1(5) . . ? O15 W3 O28 84.3(5) . . ? O13 W3 O28 75.4(5) . . ? O39 W4 O31 101.0(7) . . ? O39 W4 O24 101.9(6) . . ? O31 W4 O24 87.5(6) . . ? O39 W4 O35 98.8(7) . . ? O31 W4 O35 160.1(5) . . ? O24 W4 O35 89.1(6) . . ? O39 W4 O14 97.7(6) . . ? O31 W4 O14 89.4(6) . . ? O24 W4 O14 160.4(5) . . ? O35 W4 O14 87.2(6) . . ? O39 W4 O41 169.9(5) . . ? O31 W4 O41 86.0(5) . . ? O24 W4 O41 85.5(4) . . ? O35 W4 O41 74.2(4) . . ? O14 W4 O41 75.0(4) . . ? O6 W5 O19 102.2(5) . . ? O6 W5 O23 97.9(6) . . ? O19 W5 O23 90.6(6) . . ? O6 W5 O36 101.2(6) . . ? O19 W5 O36 87.5(5) . . ? O23 W5 O36 160.7(5) . . ? O6 W5 O14 97.0(5) . . ? O19 W5 O14 160.7(5) . . ? O23 W5 O14 87.5(6) . . ? O36 W5 O14 88.0(6) . . ? O6 W5 O41 169.7(5) . . ? O19 W5 O41 85.5(5) . . ? O23 W5 O41 75.0(5) . . ? O36 W5 O41 85.8(5) . . ? O14 W5 O41 75.5(4) . . ? O17 W6 O20 101.8(6) . . ? O17 W6 O22 99.4(6) . . ? O20 W6 O22 158.7(5) . . ? O17 W6 O34 100.9(6) . . ? O20 W6 O34 90.2(5) . . ? O22 W6 O34 88.4(5) . . ? O17 W6 O27 98.0(6) . . ? O20 W6 O27 85.1(5) . . ? O22 W6 O27 89.3(5) . . ? O34 W6 O27 161.0(5) . . ? O17 W6 O40 173.8(5) . . ? O20 W6 O40 83.8(5) . . ? O22 W6 O40 75.2(5) . . ? O34 W6 O40 76.1(5) . . ? O27 W6 O40 85.0(5) . . ? O4 W7 O20 98.0(6) . . ? O4 W7 O15 101.1(6) . . ? O20 W7 O15 87.8(5) . . ? O4 W7 O23 98.0(6) . . ? O20 W7 O23 89.2(5) . . ? O15 W7 O23 161.0(6) . . ? O4 W7 O35 101.2(6) . . ? O20 W7 O35 160.8(6) . . ? O15 W7 O35 89.9(5) . . ? O23 W7 O35 86.7(5) . . ? O4 W7 O41 172.9(5) . . ? O20 W7 O41 85.1(5) . . ? O15 W7 O41 85.4(5) . . ? O23 W7 O41 75.7(5) . . ? O35 W7 O41 75.7(5) . . ? O8 W8 O33 99.9(6) . . ? O8 W8 O30 97.9(5) . . ? O33 W8 O30 91.2(5) . . ? O8 W8 O19 102.0(5) . . ? O33 W8 O19 86.3(5) . . ? O30 W8 O19 160.1(5) . . ? O8 W8 O34 99.8(6) . . ? O33 W8 O34 160.3(5) . . ? O30 W8 O34 87.4(5) . . ? O19 W8 O34 88.3(6) . . ? O8 W8 O40 172.5(5) . . ? O33 W8 O40 84.3(5) . . ? O30 W8 O40 75.7(4) . . ? O19 W8 O40 84.4(5) . . ? O34 W8 O40 76.4(5) . . ? O5 W9 O21 100.3(7) . . ? O5 W9 O31 100.2(6) . . ? O21 W9 O31 88.0(6) . . ? O5 W9 O10 97.6(6) . . ? O21 W9 O10 90.5(6) . . ? O31 W9 O10 162.2(6) . . ? O5 W9 O12 98.6(7) . . ? O21 W9 O12 161.2(5) . . ? O31 W9 O12 88.7(6) . . ? O10 W9 O12 87.0(6) . . ? O5 W9 O26 170.8(7) . . ? O21 W9 O26 86.8(5) . . ? O31 W9 O26 85.8(5) . . ? O10 W9 O26 76.4(5) . . ? O12 W9 O26 74.4(5) . . ? O16 W10 O36 99.6(6) . . ? O16 W10 O33 101.0(7) . . ? O36 W10 O33 86.3(5) . . ? O16 W10 O12 99.4(7) . . ? O36 W10 O12 91.4(5) . . ? O33 W10 O12 159.6(6) . . ? O16 W10 O9 99.9(6) . . ? O36 W10 O9 160.4(6) . . ? O33 W10 O9 88.1(5) . . ? O12 W10 O9 87.3(6) . . ? O16 W10 O26 173.4(6) . . ? O36 W10 O26 85.2(5) . . ? O33 W10 O26 83.8(5) . . ? O12 W10 O26 75.8(5) . . ? O9 W10 O26 75.5(5) . . ? O37 W11 O13 100.7(7) . . ? O37 W11 O21 100.7(7) . . ? O13 W11 O21 158.6(5) . . ? O37 W11 O24 101.8(6) . . ? O13 W11 O24 91.0(6) . . ? O21 W11 O24 86.3(6) . . ? O37 W11 O11 98.0(6) . . ? O13 W11 O11 87.9(6) . . ? O21 W11 O11 87.5(6) . . ? O24 W11 O11 160.1(5) . . ? O37 W11 O28 171.1(5) . . ? O13 W11 O28 74.8(5) . . ? O21 W11 O28 83.9(5) . . ? O24 W11 O28 86.1(4) . . ? O11 W11 O28 74.4(4) . . ? O38 W12 O9 99.5(7) . . ? O38 W12 O10 99.9(7) . . ? O9 W12 O10 90.1(6) . . ? O38 W12 O18 100.9(6) . . ? O9 W12 O18 90.6(6) . . ? O10 W12 O18 158.7(6) . . ? O38 W12 O29 99.7(7) . . ? O9 W12 O29 160.8(6) . . ? O10 W12 O29 88.1(6) . . ? O18 W12 O29 84.2(6) . . ? O38 W12 O26 172.8(6) . . ? O9 W12 O26 74.9(5) . . ? O10 W12 O26 75.9(5) . . ? O18 W12 O26 83.8(5) . . ? O29 W12 O26 86.1(5) . . ? N16 Co1 N8 177.3(6) 1_655 . ? N16 Co1 N11 88.8(6) 1_655 . ? N8 Co1 N11 93.7(6) . . ? N16 Co1 O4 90.8(5) 1_655 2_672 ? N8 Co1 O4 86.6(6) . 2_672 ? N11 Co1 O4 175.1(5) . 2_672 ? N16 Co1 O6 90.8(5) 1_655 . ? N8 Co1 O6 88.3(5) . . ? N11 Co1 O6 86.6(5) . . ? O4 Co1 O6 88.5(5) 2_672 . ? N16 Co1 N2 89.9(6) 1_655 . ? N8 Co1 N2 90.9(6) . . ? N11 Co1 N2 94.1(6) . . ? O4 Co1 N2 90.8(5) 2_672 . ? O6 Co1 N2 179.0(5) . . ? N14 Co2 N6 92.2(7) . . ? N14 Co2 N1 90.1(7) . 1_666 ? N6 Co2 N1 177.2(6) . 1_666 ? N14 Co2 O2 93.5(8) . 1_656 ? N6 Co2 O2 90.8(6) . 1_656 ? N1 Co2 O2 90.6(6) 1_666 1_656 ? N14 Co2 O1 95.4(8) . . ? N6 Co2 O1 87.3(6) . . ? N1 Co2 O1 90.9(6) 1_666 . ? O2 Co2 O1 171.0(5) 1_656 . ? N14 Co2 O3 175.1(6) . 2_672 ? N6 Co2 O3 92.6(6) . 2_672 ? N1 Co2 O3 85.1(6) 1_666 2_672 ? O2 Co2 O3 85.6(5) 1_656 2_672 ? O1 Co2 O3 85.7(5) . 2_672 ? W2 O2 Co2 150.0(8) . 1_454 ? W1 O3 Co2 138.5(7) . 2_672 ? W7 O4 Co1 147.5(7) . 2_672 ? W5 O6 Co1 148.7(7) . . ? W2 O7 W1 146.9(8) . . ? W12 O9 W10 120.2(7) . . ? W12 O10 W9 119.4(7) . . ? W1 O11 W11 119.4(6) . . ? W10 O12 W9 119.7(7) . . ? W11 O13 W3 121.1(7) . . ? W4 O14 W5 120.8(6) . . ? W7 O15 W3 148.1(7) . . ? W2 O18 W12 150.5(8) . . ? W5 O19 W8 148.9(7) . . ? W7 O20 W6 150.1(7) . . ? W11 O21 W9 149.1(7) . . ? W6 O22 W2 119.0(6) . . ? W5 O23 W7 120.0(6) . . ? W4 O24 W11 149.0(8) . . ? B1 O26 W10 128.0(10) . . ? B1 O26 W9 123.8(11) . . ? W10 O26 W9 90.1(5) . . ? B1 O26 W12 125.6(10) . . ? W10 O26 W12 89.3(5) . . ? W9 O26 W12 88.2(4) . . ? W3 O27 W6 148.6(7) . . ? B1 O28 W1 125.2(10) . . ? B1 O28 W3 127.2(11) . . ? W1 O28 W3 90.0(4) . . ? B1 O28 W11 125.2(10) . . ? W1 O28 W11 88.7(4) . . ? W3 O28 W11 88.6(4) . . ? W1 O29 W12 147.5(7) . . ? W8 O30 W2 118.3(6) . . ? W4 O31 W9 147.0(7) . . ? W3 O32 W1 120.1(6) . . ? W8 O33 W10 150.6(7) . . ? W6 O34 W8 119.2(6) . . ? W4 O35 W7 120.2(6) . . ? W5 O36 W10 148.7(7) . . ? B1 O40 W2 126.2(10) . . ? B1 O40 W8 126.1(11) . . ? W2 O40 W8 89.1(4) . . ? B1 O40 W6 126.3(11) . . ? W2 O40 W6 88.8(4) . . ? W8 O40 W6 88.2(4) . . ? B1 O41 W7 127.2(11) . . ? B1 O41 W5 124.7(10) . . ? W7 O41 W5 89.4(4) . . ? B1 O41 W4 125.2(10) . . ? W7 O41 W4 89.9(4) . . ? W5 O41 W4 88.7(4) . . ? C12 C1 N15 104(2) . . ? C12 C1 H1A 127.8 . . ? N15 C1 H1A 127.8 . . ? C43 C3 C36 117.9(18) . . ? C43 C3 H3A 121.1 . . ? C36 C3 H3A 121.1 . . ? C10 C5 C48 119(3) . . ? C10 C5 H5A 120.5 . . ? C48 C5 H5A 120.5 . . ? C9 C7 C8 128(4) . . ? C9 C7 H7A 116.1 . . ? C8 C7 H7A 116.1 . . ? C7 C8 N13 127(3) . . ? C7 C8 C10 113(3) . . ? N13 C8 C10 119(3) . . ? C7 C9 C48 124(5) . . ? C7 C9 N4 115(4) . . ? C48 C9 N4 119(5) . . ? C5 C10 C8 119(3) . . ? C5 C10 H10A 120.7 . . ? C8 C10 H10A 120.7 . . ? C13 C11 N13 102(2) . . ? C13 C11 H11A 129.0 . . ? N13 C11 H11A 129.0 . . ? C1 C12 N1 112(2) . . ? C1 C12 H12A 123.8 . . ? N1 C12 H12A 123.8 . . ? C11 C13 N14 118(3) . . ? C11 C13 C15 77(2) . . ? N14 C13 C15 41.0(13) . . ? C11 C13 H13A 121.0 . . ? N14 C13 H13A 121.0 . . ? C15 C13 H13A 161.6 . . ? C23 C14 N12 109(3) . . ? C23 C14 H14A 125.6 . . ? N12 C14 H14A 125.6 . . ? N13 C15 N14 114(2) . . ? N13 C15 C13 73.7(18) . . ? N14 C15 C13 40.1(13) . . ? N13 C15 H15A 123.2 . . ? N14 C15 H15A 123.2 . . ? C13 C15 H15A 162.8 . . ? C33 C16 C44 124(2) . . ? C33 C16 H16A 117.9 . . ? C44 C16 H16A 117.9 . . ? C31 C17 C40 119(2) . . ? C31 C17 H17A 120.4 . . ? C40 C17 H17A 120.4 . . ? N6 C18 N5 114(2) . . ? N6 C18 H18A 123.1 . . ? N5 C18 H18A 123.1 . . ? C27 C19 N5 107.7(17) . . ? C27 C19 H19A 126.2 . . ? N5 C19 H19A 126.2 . . ? C26 C20 C29 122(2) . . ? C26 C20 H20A 118.9 . . ? C29 C20 H20A 118.9 . . ? C41 C21 N8 110.6(16) . . ? C41 C21 H21A 124.7 . . ? N8 C21 H21A 124.7 . . ? N7 C22 C24 106(2) . . ? N7 C22 H22A 127.0 . . ? C24 C22 H22A 127.0 . . ? C14 C23 N11 110(2) . . ? C14 C23 H23A 125.1 . . ? N11 C23 H23A 125.1 . . ? N16 C24 C22 110(2) . . ? N16 C24 H24A 125.2 . . ? C22 C24 H24A 125.2 . . ? N2 C25 N3 112.6(18) . . ? N2 C25 H25A 123.7 . . ? N3 C25 H25A 123.7 . . ? C20 C26 C36 118(2) . . ? C20 C26 H26A 120.8 . . ? C36 C26 H26A 120.8 . . ? C19 C27 N6 110.8(19) . . ? C19 C27 H27A 124.6 . . ? N6 C27 H27A 124.6 . . ? N16 C28 N7 111.6(17) . . ? N16 C28 H28A 124.2 . . ? N7 C28 H28A 124.2 . . ? C43 C29 C20 119(2) . . ? C43 C29 H29A 120.6 . . ? C20 C29 H29A 120.6 . . ? N1 C30 N15 113.9(19) . . ? N1 C30 H30A 123.1 . . ? N15 C30 H30A 123.1 . . ? C17 C31 C35 121(2) . . ? C17 C31 H31A 119.7 . . ? C35 C31 H31A 119.7 . . ? C45 C32 C35 119.4(18) . . ? C45 C32 H32A 120.3 . . ? C35 C32 H32A 120.3 . . ? C16 C33 C46 120(2) . . ? C16 C33 H33A 120.2 . . ? C46 C33 H33A 120.2 . . ? C47 C34 N2 112.7(18) . . ? C47 C34 H34A 123.7 . . ? N2 C34 H34A 123.7 . . ? C31 C35 C32 120(2) . . ? C31 C35 N15 121.9(17) . . ? C32 C35 N15 118.2(18) . . ? C3 C36 N7 118.3(17) . . ? C3 C36 C26 120(2) . . ? N7 C36 C26 121.5(17) . . ? N11 C37 N12 115.8(18) . . ? N11 C37 H37A 122.1 . . ? N12 C37 H37A 122.1 . . ? N8 C38 N9 113.5(17) . . ? N8 C38 H38A 123.2 . . ? N9 C38 H38A 123.2 . . ? C42 C39 C44 120(2) . . ? C42 C39 H39A 119.8 . . ? C44 C39 H39A 119.8 . . ? C45 C40 C17 121(2) . . ? C45 C40 H40A 119.7 . . ? C17 C40 H40A 119.7 . . ? C21 C41 N9 108.1(17) . . ? C21 C41 H41A 125.9 . . ? N9 C41 H41A 125.9 . . ? C39 C42 C46 121.3(18) . . ? C39 C42 N3 121(2) . . ? C46 C42 N3 117.3(19) . . ? C29 C43 C3 122.4(17) . . ? C29 C43 N9 120.8(19) . . ? C3 C43 N9 116.7(17) . . ? C16 C44 N5 124.3(19) . . ? C16 C44 C39 116(2) . . ? N5 C44 C39 120(2) . . ? C40 C45 C32 119.9(18) . . ? C40 C45 N12 122.6(19) . . ? C32 C45 N12 117.4(16) . . ? C33 C46 C42 118(2) . . ? C33 C46 H46A 120.9 . . ? C42 C46 H46A 120.9 . . ? C34 C47 N3 104.3(19) . . ? C34 C47 H47A 127.8 . . ? N3 C47 H47A 127.8 . . ? C9 C48 C5 117(4) . . ? C9 C48 H48A 121.4 . . ? C5 C48 H48A 121.4 . . ? C30 N1 C12 103.3(17) . . ? C30 N1 Co2 127.3(13) . 1_444 ? C12 N1 Co2 129.4(14) . 1_444 ? C25 N2 C34 104.1(15) . . ? C25 N2 Co1 132.4(14) . . ? C34 N2 Co1 123.5(12) . . ? C25 N3 C47 106.3(16) . . ? C25 N3 C42 127.4(16) . . ? C47 N3 C42 126.2(17) . . ? C18 N5 C44 126.9(19) . . ? C18 N5 C19 105.6(18) . . ? C44 N5 C19 127.5(17) . . ? C18 N6 C27 102.1(17) . . ? C18 N6 Co2 127.0(16) . . ? C27 N6 Co2 128.6(15) . . ? C22 N7 C28 106.1(18) . . ? C22 N7 C36 123.8(17) . . ? C28 N7 C36 129.9(17) . . ? C38 N8 C21 103.7(15) . . ? C38 N8 Co1 129.6(13) . . ? C21 N8 Co1 126.4(11) . . ? C38 N9 C41 103.9(16) . . ? C38 N9 C43 129.1(17) . . ? C41 N9 C43 126.7(16) . . ? C37 N11 C23 103.4(17) . . ? C37 N11 Co1 130.3(14) . . ? C23 N11 Co1 126.1(13) . . ? C37 N12 C14 102.3(18) . . ? C37 N12 C45 129.1(17) . . ? C14 N12 C45 128.5(19) . . ? C15 N13 C11 107(2) . . ? C15 N13 C8 126(3) . . ? C11 N13 C8 126(2) . . ? C13 N14 C15 99(2) . . ? C13 N14 Co2 134.3(18) . . ? C15 N14 Co2 126.0(16) . . ? C30 N15 C1 105.6(18) . . ? C30 N15 C35 127.7(17) . . ? C1 N15 C35 126.7(18) . . ? C28 N16 C24 106.0(16) . . ? C28 N16 Co1 130.3(13) . 1_455 ? C24 N16 Co1 123.3(14) . 1_455 ? C2 N4 C6 108.0 . . ? C2 N4 C9 128(4) . . ? C6 N4 C9 123(4) . . ? N10 C6 N4 108.0 . . ? N10 C6 H6A 126.0 . . ? N4 C6 H6A 126.0 . . ? C6 N10 C4 108.0 . . ? C2 C4 N10 108.0 . . ? C2 C4 H4A 126.0 . . ? N10 C4 H4A 126.0 . . ? C4 C2 N4 108.0 . . ? C4 C2 H2A 126.0 . . ? N4 C2 H2A 126.0 . . ? O40 B1 O28 108.8(15) . . ? O40 B1 O41 109.3(14) . . ? O28 B1 O41 108.3(15) . . ? O40 B1 O26 108.1(15) . . ? O28 B1 O26 112.2(15) . . ? O41 B1 O26 110.1(15) . . ? _refine_diff_density_max 4.034 _refine_diff_density_min -2.359 _refine_diff_density_rms 0.428 _shelxl_version_number 2013-2 _shelx_res_file ; TITL ytt in P-1 CELL 0.71069 13.270 15.060 21.186 91.802 103.098 112.440 ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005 LATT 1 SFAC C H B N O Co W UNIT 28 28 28 28 28 28 28 MERG 2 L.S. 12 ACTA bond $H FMAP 2 PLAN 50 LIST 1 isor 0.001 O15 O20 N7 N11 N16 C28 C47 C48 N15 C1 C12 C14 C16 C23 C37 isor 0.001 O6 C5 C9 N5 C7 C26 O21 C22 O13 O41 C31 C40 C41 O27 isor 0.001 N10 C2 C4 C6 N4 delu C10 C48 delu N4 C2 delu N4 C6 delu N4 C9 delu N14 C15 delu N10 C4 simu 0.01 0.02 5.12 N10 C2 C4 C6 N4 WGHT 0.075800 FVAR 0.02486 W1 7 0.179805 0.870296 -1.935039 11.00000 0.03089 0.02643 = 0.00671 0.00143 -0.00024 0.01654 W2 7 0.055271 0.981336 -1.838701 11.00000 0.02253 0.02570 = 0.01223 0.00217 -0.00250 0.01556 W3 7 0.432589 1.008795 -1.841189 11.00000 0.02333 0.02914 = 0.00861 0.00208 0.00301 0.01572 W4 7 0.404041 0.761273 -1.688661 11.00000 0.03556 0.02981 = 0.01256 0.00470 0.00375 0.02515 W5 7 0.289213 0.864341 -1.600767 11.00000 0.02513 0.02815 = 0.00688 0.00361 0.00185 0.01622 W6 7 0.305319 1.118639 -1.742393 11.00000 0.01869 0.01901 = 0.01472 0.00071 0.00160 0.01170 W7 7 0.488822 1.001085 -1.666175 11.00000 0.01890 0.02627 = 0.00793 0.00048 -0.00093 0.01358 W8 7 0.101958 0.976187 -1.679797 11.00000 0.02310 0.02669 = 0.01200 0.00382 0.00418 0.01602 W9 7 0.126392 0.616393 -1.795868 11.00000 0.04311 0.02044 = 0.02029 0.00135 0.00295 0.01547 W10 7 0.011166 0.713520 -1.705408 11.00000 0.02742 0.02352 = 0.01752 0.00230 0.00226 0.00645 W11 7 0.352200 0.769979 -1.864806 11.00000 0.04621 0.03261 = 0.01264 0.00485 0.00903 0.03041 W12 7 -0.045802 0.717680 -1.865391 11.00000 0.02995 0.02411 = 0.01775 0.00044 -0.00391 0.00725 CO1 6 0.293647 0.776842 -1.437232 11.00000 0.01457 0.02701 = 0.00987 0.00032 0.00071 0.01273 CO2 6 0.802733 1.029914 -0.909710 11.00000 0.02735 0.02824 = 0.01115 -0.00119 -0.00097 0.01358 O1 5 0.648906 1.048419 -0.946787 11.00000 0.02120 0.08983 = 0.02291 0.00247 0.00898 0.02915 O2 5 -0.038607 1.019882 -1.886551 11.00000 0.03095 0.03013 = 0.01878 0.00463 -0.00795 0.01769 O3 5 0.134434 0.879448 -2.017330 11.00000 0.02904 0.02382 = 0.01884 -0.00011 -0.00053 0.01224 O4 5 0.615661 1.088813 -1.626896 11.00000 0.03573 0.02588 = 0.00627 0.00812 0.00985 0.01238 O5 5 0.107493 0.498160 -1.808955 11.00000 0.05073 0.02183 = 0.03173 -0.00421 -0.00118 0.00777 O6 5 0.294499 0.858913 -1.518629 11.00000 0.01838 0.01824 = 0.01772 0.00257 0.00453 0.00737 O7 5 0.129832 0.958369 -1.898361 11.00000 0.03539 0.02951 = 0.01413 0.00220 -0.00305 0.01429 O8 5 0.036281 1.006257 -1.627007 11.00000 0.02687 0.04011 = 0.01409 -0.00511 0.00346 0.01384 O9 5 -0.096508 0.689708 -1.789750 11.00000 0.03287 0.04518 = 0.02019 0.00990 0.01023 0.01657 O10 5 -0.003516 0.609073 -1.861764 11.00000 0.05203 0.02519 = 0.02023 -0.00538 -0.01093 0.01513 O11 5 0.256034 0.789049 -1.942945 11.00000 0.04251 0.02774 = 0.01485 0.01411 0.00903 0.02650 O12 5 0.037398 0.604206 -1.734079 11.00000 0.05827 0.02565 = 0.01359 0.00538 0.01067 0.02572 O13 5 0.458605 0.895677 -1.864760 11.00000 0.02982 0.02931 = 0.02929 0.00331 0.00737 0.01220 O14 5 0.361367 0.777596 -1.610053 11.00000 0.03301 0.03226 = 0.01543 0.00287 0.00571 0.02757 O15 5 0.498724 1.002431 -1.753240 11.00000 0.01806 0.01822 = 0.01788 0.00271 0.00413 0.00771 O16 5 -0.078282 0.660078 -1.659120 11.00000 0.03172 0.06016 = 0.02034 0.01770 0.00079 0.01316 O17 5 0.376000 1.240895 -1.731392 11.00000 0.03094 0.03587 = 0.02083 -0.00068 0.01060 0.01703 O18 5 -0.030986 0.849430 -1.850501 11.00000 0.02871 0.04278 = 0.00930 0.00297 -0.00015 0.00860 O19 5 0.216168 0.947931 -1.621647 11.00000 0.01662 0.03616 = 0.00880 -0.00242 -0.00410 0.01312 O20 5 0.407848 1.079779 -1.683316 11.00000 0.02437 0.02465 = 0.02391 0.00306 0.00615 0.00982 O21 5 0.220539 0.671247 -1.851855 11.00000 0.02514 0.02455 = 0.02499 0.00323 0.00629 0.01023 O22 5 0.175874 1.106611 -1.809744 11.00000 0.02132 0.01936 = 0.01383 0.00454 -0.00266 0.01279 O23 5 0.430405 0.967142 -1.591127 11.00000 0.03297 0.03931 = 0.01078 -0.00129 -0.00055 0.02495 O24 5 0.419112 0.772089 -1.775085 11.00000 0.04661 0.02754 = 0.01193 0.00692 0.01541 0.02393 O25 5 0.546376 1.094975 -1.860740 11.00000 0.04087 0.03304 = 0.02881 0.00362 0.01080 0.02713 O26 5 0.121836 0.770806 -1.777619 11.00000 0.02815 0.02056 = 0.01760 0.00149 -0.01146 0.01167 O27 5 0.371348 1.088428 -1.808315 11.00000 0.02055 0.02064 = 0.02013 0.00234 0.00548 0.00817 O28 5 0.275937 0.877293 -1.827211 11.00000 0.02153 0.02042 = 0.01472 -0.00108 0.00437 0.01335 O29 5 0.054082 0.768801 -1.921741 11.00000 0.04499 0.02278 = 0.02053 -0.00035 -0.01051 0.02240 O30 5 0.013790 0.995122 -1.758862 11.00000 0.01829 0.02921 = 0.01377 0.00623 0.00635 0.01563 O31 5 0.258395 0.663377 -1.724697 11.00000 0.05063 0.03261 = 0.01439 0.00968 0.00217 0.02931 O32 5 0.324295 0.977273 -1.922328 11.00000 0.01431 0.02546 = 0.00982 0.00058 -0.00357 0.01480 O33 5 0.018353 0.841994 -1.696908 11.00000 0.01087 0.02587 = 0.01890 0.00102 0.00546 -0.00345 O34 5 0.215952 1.102823 -1.680848 11.00000 0.02501 0.01391 = 0.02196 -0.00559 0.00214 0.00454 O35 5 0.522485 0.886967 -1.661381 11.00000 0.03403 0.03771 = 0.01037 0.00835 0.00882 0.03019 O36 5 0.150162 0.761148 -1.639845 11.00000 0.03973 0.01647 = 0.01833 0.00833 0.00761 0.01549 O37 5 0.405384 0.702138 -1.902365 11.00000 0.07440 0.06249 = 0.01771 0.01445 0.02488 0.05575 O38 5 -0.172539 0.667551 -1.923131 11.00000 0.02725 0.03823 = 0.03530 0.00622 -0.01173 -0.00428 O39 5 0.478581 0.693580 -1.662021 11.00000 0.06809 0.05799 = 0.01648 0.00248 -0.00012 0.04602 O40 5 0.187101 0.949013 -1.761492 11.00000 0.01452 0.02023 = 0.00661 -0.00322 0.00505 0.00244 O41 5 0.315621 0.873548 -1.707723 11.00000 0.01347 0.01300 = 0.01300 0.00165 0.00305 0.00530 C1 1 -0.095963 0.311495 -1.804037 11.00000 0.04899 0.04887 = 0.04918 0.00613 0.01249 0.01988 AFIX 43 H1A 2 -0.102098 0.370330 -1.797226 11.00000 -1.20000 AFIX 0 C3 1 -0.203793 0.800695 -1.461589 11.00000 0.01223 0.05065 = 0.02215 0.01395 0.00586 0.01957 AFIX 43 H3A 2 -0.208578 0.761162 -1.428583 11.00000 -1.20000 AFIX 0 C5 1 0.661509 0.623331 -0.679154 11.00000 0.06881 0.06889 = 0.06894 0.00906 0.01780 0.02761 AFIX 43 H5A 2 0.684979 0.607325 -0.637938 11.00000 -1.20000 AFIX 0 C7 1 0.592790 0.659222 -0.801710 11.00000 0.09336 0.09344 = 0.09335 0.01235 0.02411 0.03725 AFIX 43 H7A 2 0.570198 0.668290 -0.845019 11.00000 -1.20000 AFIX 0 C8 1 0.672792 0.738491 -0.760922 11.00000 0.04299 0.07098 = 0.08864 0.00811 0.01656 0.02077 C9 1 0.548264 0.579700 -0.788626 11.00000 0.11920 0.11906 = 0.11914 0.01578 0.03076 0.04763 C10 1 0.710589 0.716781 -0.693180 11.00000 0.10409 0.07814 = 0.08498 -0.00076 0.02996 0.05774 AFIX 43 H10A 2 0.765970 0.765257 -0.661240 11.00000 -1.20000 AFIX 0 C11 1 0.711232 0.913386 -0.740482 11.00000 0.06280 0.09315 = 0.05577 0.02241 0.02315 0.04991 AFIX 43 H11A 2 0.695391 0.917700 -0.700202 11.00000 -1.20000 AFIX 0 C12 1 -0.169651 0.232165 -1.845719 11.00000 0.04013 0.04019 = 0.04043 0.00524 0.01004 0.01632 AFIX 43 H12A 2 -0.239621 0.226585 -1.870753 11.00000 -1.20000 AFIX 0 C13 1 0.735947 0.978584 -0.778685 11.00000 0.07165 0.05690 = 0.01514 0.00363 0.00569 0.03339 AFIX 43 H13A 2 0.742720 1.041035 -0.766975 11.00000 -1.20000 AFIX 0 C14 1 0.064785 0.533354 -1.576151 11.00000 0.06445 0.06474 = 0.06465 0.00815 0.01673 0.02586 AFIX 43 H14A 2 -0.007821 0.490546 -1.598191 11.00000 -1.20000 AFIX 0 C15 1 0.742124 0.864224 -0.826943 11.00000 0.03677 0.05115 = 0.05154 0.00621 0.01358 0.00645 AFIX 43 H15A 2 0.754665 0.825459 -0.856713 11.00000 -1.20000 AFIX 0 C16 1 0.419983 0.653469 -1.056592 11.00000 0.04216 0.04225 = 0.04184 0.00563 0.01084 0.01671 AFIX 43 H16A 2 0.438902 0.657905 -1.011230 11.00000 -1.20000 AFIX 0 C17 1 0.283354 0.399297 -1.677461 11.00000 0.04023 0.11508 = 0.05236 -0.00072 0.01421 0.05195 AFIX 43 H17A 2 0.353489 0.399872 -1.677983 11.00000 -1.20000 AFIX 0 C18 1 0.624608 0.845259 -0.997929 11.00000 0.03740 0.02353 = 0.03239 0.00003 -0.01274 0.00158 AFIX 43 H18A 2 0.569543 0.847477 -0.978242 11.00000 -1.20000 AFIX 0 C19 1 0.703082 0.804008 -1.066726 11.00000 0.05090 0.02452 = 0.00998 -0.00583 0.00589 0.00604 AFIX 43 H19A 2 0.714389 0.774776 -1.102292 11.00000 -1.20000 AFIX 0 C20 1 -0.190262 0.917623 -1.561260 11.00000 0.04615 0.04739 = 0.02187 0.01354 0.01471 0.02439 AFIX 43 H20A 2 -0.185152 0.954940 -1.595482 11.00000 -1.20000 AFIX 0 C21 1 0.112345 0.798184 -1.373264 11.00000 0.03112 0.05883 = 0.01717 0.01443 0.01195 0.03943 AFIX 43 H21A 2 0.150303 0.791347 -1.332290 11.00000 -1.20000 AFIX 0 C22 1 -0.432539 0.699510 -1.447788 11.00000 0.03946 0.03956 = 0.03976 0.00530 0.01024 0.01595 AFIX 43 H22A 2 -0.402086 0.653174 -1.447562 11.00000 -1.20000 AFIX 0 C23 1 0.090073 0.601501 -1.528840 11.00000 0.03764 0.03778 = 0.03768 0.00433 0.00993 0.01509 AFIX 43 H23A 2 0.038076 0.615130 -1.511800 11.00000 -1.20000 AFIX 0 C24 1 -0.525987 0.692573 -1.427195 11.00000 0.04061 0.05066 = 0.04627 0.02239 0.02693 0.02751 AFIX 43 H24A 2 -0.564800 0.643254 -1.405501 11.00000 -1.20000 AFIX 0 C25 1 0.343482 0.720977 -1.291506 11.00000 0.03104 0.02683 = 0.01423 0.00666 0.00628 0.01452 AFIX 43 H25A 2 0.391122 0.784320 -1.273242 11.00000 -1.20000 AFIX 0 C26 1 -0.285309 0.886754 -1.541364 11.00000 0.03180 0.03205 = 0.03174 0.00425 0.00815 0.01274 AFIX 43 H26A 2 -0.344141 0.904602 -1.560013 11.00000 -1.20000 AFIX 0 C27 1 0.781835 0.873630 -1.021501 11.00000 0.02655 0.03305 = 0.03234 0.01506 0.00952 0.01829 AFIX 43 H27A 2 0.858352 0.899527 -1.019834 11.00000 -1.20000 AFIX 0 C28 1 -0.473595 0.824910 -1.467750 11.00000 0.02077 0.02108 = 0.02093 0.00258 0.00524 0.00860 AFIX 43 H28A 2 -0.470914 0.882910 -1.482804 11.00000 -1.20000 AFIX 0 C29 1 -0.096337 0.895153 -1.531669 11.00000 0.02379 0.04122 = 0.01592 0.00084 0.00309 0.01399 AFIX 43 H29A 2 -0.029900 0.919823 -1.545020 11.00000 -1.20000 AFIX 0 C30 1 -0.036186 0.194183 -1.800700 11.00000 0.04824 0.02467 = 0.03032 -0.01079 -0.00854 0.01412 AFIX 43 H30A 2 0.007184 0.158692 -1.787715 11.00000 -1.20000 AFIX 0 C31 1 0.189832 0.336689 -1.719711 11.00000 0.02675 0.02677 = 0.02660 0.00331 0.00678 0.01093 AFIX 43 H31A 2 0.193647 0.288198 -1.746147 11.00000 -1.20000 AFIX 0 C32 1 0.080950 0.409845 -1.680753 11.00000 0.02723 0.03041 = 0.02441 0.00958 0.00635 0.01869 AFIX 43 H32A 2 0.011734 0.413239 -1.682968 11.00000 -1.20000 AFIX 0 C33 1 0.318913 0.587198 -1.089648 11.00000 0.06046 0.02777 = 0.02723 0.00681 0.01581 -0.00456 AFIX 43 H33A 2 0.271617 0.545074 -1.067494 11.00000 -1.20000 AFIX 0 C34 1 0.236232 0.598050 -1.359313 11.00000 0.03284 0.04046 = 0.01573 0.00618 -0.00657 0.01603 AFIX 43 H34A 2 0.193459 0.559050 -1.398749 11.00000 -1.20000 AFIX 0 C35 1 0.089294 0.343135 -1.724447 11.00000 0.03970 0.03000 = 0.01659 0.01555 0.01315 0.02366 C36 1 -0.294414 0.825372 -1.490503 11.00000 0.03033 0.03057 = 0.02144 0.00257 0.00935 0.01953 C37 1 0.241326 0.606444 -1.544516 11.00000 0.02517 0.02540 = 0.02517 0.00315 0.00646 0.00998 AFIX 43 H37A 2 0.317988 0.624127 -1.540395 11.00000 -1.20000 AFIX 0 C38 1 0.067868 0.806790 -1.474208 11.00000 0.03202 0.03915 = 0.01950 0.00659 0.01244 0.01735 AFIX 43 H38A 2 0.069938 0.809493 -1.517712 11.00000 -1.20000 AFIX 0 C39 1 0.462228 0.711464 -1.153360 11.00000 0.01218 0.01027 = 0.02615 0.00733 -0.01029 0.00115 AFIX 43 H39A 2 0.510149 0.753572 -1.175213 11.00000 -1.20000 AFIX 0 C40 1 0.274300 0.465643 -1.631265 11.00000 0.03024 0.03011 = 0.03022 0.00365 0.00772 0.01216 AFIX 43 H40A 2 0.337978 0.505306 -1.599019 11.00000 -1.20000 AFIX 0 C41 1 0.020258 0.815350 -1.385064 11.00000 0.02370 0.02393 = 0.02373 0.00332 0.00600 0.00961 AFIX 43 H41A 2 -0.015896 0.824305 -1.354109 11.00000 -1.20000 AFIX 0 C42 1 0.359907 0.647528 -1.187133 11.00000 0.05782 0.03498 = 0.00863 0.01033 0.01039 0.03652 C43 1 -0.105849 0.837706 -1.484190 11.00000 0.01091 0.03391 = 0.02906 0.01573 0.00141 0.01406 C44 1 0.497405 0.715243 -1.085381 11.00000 0.04747 0.02282 = 0.01500 0.00546 0.00952 0.01773 C45 1 0.176797 0.470947 -1.634058 11.00000 0.02693 0.01866 = 0.03046 0.00494 0.01445 0.01821 C46 1 0.285809 0.581833 -1.155802 11.00000 0.04678 0.01363 = 0.02691 0.00368 0.01039 0.01142 AFIX 43 H46A 2 0.216167 0.536038 -1.179655 11.00000 -1.20000 AFIX 0 C47 1 0.249615 0.563748 -1.301313 11.00000 0.02566 0.02563 = 0.02553 0.00343 0.00624 0.01036 AFIX 43 H47A 2 0.218717 0.499909 -1.293079 11.00000 -1.20000 AFIX 0 C48 1 0.574583 0.552003 -0.728675 11.00000 0.08253 0.08252 = 0.08258 0.01085 0.02136 0.03302 AFIX 43 H48A 2 0.537264 0.489067 -0.720465 11.00000 -1.20000 AFIX 0 N1 4 -0.129886 0.160383 -1.847123 11.00000 0.04176 0.02328 = 0.01779 -0.00939 -0.00002 0.01852 N2 4 0.291746 0.695274 -1.353889 11.00000 0.02658 0.03496 = 0.01464 0.01710 0.01043 0.01886 N3 4 0.319926 0.645313 -1.256742 11.00000 0.01440 0.01298 = 0.02146 0.00064 -0.00310 0.00268 N5 4 0.601562 0.782756 -1.051583 11.00000 0.02816 0.02819 = 0.02803 0.00376 0.00722 0.01108 N6 4 0.733400 0.903348 -0.975865 11.00000 0.04247 0.02203 = 0.01657 -0.00732 -0.00506 0.01356 N7 4 -0.393761 0.787753 -1.468518 11.00000 0.02093 0.02135 = 0.02127 0.00275 0.00551 0.00869 N8 4 0.144465 0.791797 -1.429333 11.00000 0.01733 0.02549 = 0.01694 0.00543 0.00066 0.00900 N9 4 -0.013275 0.817762 -1.451065 11.00000 0.02513 0.03931 = 0.02623 -0.00434 0.00920 0.02225 N11 4 0.204639 0.650073 -1.507940 11.00000 0.01428 0.01437 = 0.01407 0.00140 0.00379 0.00568 N12 4 0.163242 0.534904 -1.588326 11.00000 0.02564 0.01922 = 0.01919 -0.01066 -0.00176 0.00652 N13 4 0.714240 0.836034 -0.774351 11.00000 0.05329 0.05164 = 0.04692 0.03179 0.03073 0.02568 N14 4 0.751360 0.954445 -0.834742 11.00000 0.08968 0.04248 = 0.02010 -0.00051 0.02375 0.01617 N15 4 -0.007943 0.285443 -1.773227 11.00000 0.02667 0.02659 = 0.02638 0.00319 0.00684 0.01055 N16 4 -0.553077 0.768897 -1.443393 11.00000 0.01784 0.01816 = 0.01802 0.00201 0.00484 0.00744 AFIX 9 N4 4 0.446285 0.518291 -0.835579 11.00000 0.14658 0.14658 = 0.14664 0.01916 0.03780 0.05863 C6 1 0.441809 0.490437 -0.899991 11.00000 0.14935 0.14942 = 0.14938 0.01961 0.03854 0.05964 AFIX 43 H6A 2 0.503321 0.504338 -0.917730 11.00000 -1.20000 AFIX 5 N10 4 0.328762 0.438054 -0.933083 11.00000 0.15153 0.15157 = 0.15158 0.01989 0.03909 0.06042 C4 1 0.263371 0.433553 -0.889134 11.00000 0.14869 0.14880 = 0.14870 0.01935 0.03852 0.05938 AFIX 43 H4A 2 0.185166 0.402909 -0.898375 11.00000 -1.20000 AFIX 5 C2 1 0.336009 0.483134 -0.828886 11.00000 0.15053 0.15051 = 0.15056 0.01980 0.03880 0.06008 AFIX 43 H2A 2 0.314681 0.491311 -0.790944 11.00000 -1.20000 AFIX 0 B1 3 0.224752 0.866683 -1.768951 11.00000 10.02000 HKLF 4 REM ytt in P-1 REM R1 = 0.0546 for 9245 Fo > 4sig(Fo) and 0.0921 for all 13465 data REM 1067 parameters refined using 269 restraints END WGHT 0.0785 0.0567 REM Highest difference peak 4.034, deepest hole -2.359, 1-sigma level 0.428 Q1 1 0.3508 0.9278 -1.5872 11.00000 0.05 4.03 Q2 1 0.4924 1.0729 -1.8251 11.00000 0.05 3.83 Q3 1 0.1625 1.0417 -1.6692 11.00000 0.05 3.74 Q4 1 0.0159 0.7802 -1.8503 11.00000 0.05 3.72 Q5 1 0.0458 0.9150 -1.6930 11.00000 0.05 3.69 Q6 1 0.3715 1.1793 -1.7259 11.00000 0.05 3.63 Q7 1 0.4286 0.9315 -1.6808 11.00000 0.05 3.47 Q8 1 0.2923 0.7070 -1.8783 11.00000 0.05 3.45 Q9 1 0.5407 1.0631 -1.6565 11.00000 0.05 3.41 Q10 1 0.0838 0.5480 -1.8047 11.00000 0.05 3.29 Q11 1 0.1150 0.8072 -1.9511 11.00000 0.05 3.26 Q12 1 0.0060 0.9137 -1.8509 11.00000 0.05 3.25 Q13 1 -0.0934 0.6568 -1.8750 11.00000 0.05 3.20 Q14 1 0.2367 1.0533 -1.7589 11.00000 0.05 3.11 Q15 1 0.2525 0.9269 -1.9176 11.00000 0.05 3.02 Q16 1 0.4023 0.8494 -1.8609 11.00000 0.05 2.99 Q17 1 0.4634 0.8201 -1.6785 11.00000 0.05 2.98 Q18 1 0.2385 0.7912 -1.6092 11.00000 0.05 2.98 Q19 1 0.0725 0.4951 -0.9755 11.00000 0.05 2.93 Q20 1 -0.0530 0.6567 -1.7215 11.00000 0.05 2.91 Q21 1 0.3828 0.9422 -1.8522 11.00000 0.05 2.89 Q22 1 0.1736 0.6809 -1.7873 11.00000 0.05 2.89 Q23 1 0.1053 1.0475 -1.8327 11.00000 0.05 2.89 Q24 1 0.3344 0.6927 -1.7062 11.00000 0.05 2.80 Q25 1 0.1975 0.8136 -1.6169 11.00000 0.05 2.62 Q26 1 0.0675 0.7782 -1.6948 11.00000 0.05 2.56 Q27 1 0.1373 1.0284 -1.8198 11.00000 0.05 2.56 Q28 1 0.0623 0.3322 -0.9282 11.00000 0.05 2.34 Q29 1 -0.3611 0.5400 -1.5280 11.00000 0.05 2.30 Q30 1 0.0638 0.5628 -2.0009 11.00000 0.05 2.26 Q31 1 0.1024 0.2824 -0.9097 11.00000 0.05 2.13 Q32 1 0.2195 1.1003 -1.7488 11.00000 0.05 2.02 Q33 1 0.3832 0.9679 -1.6805 11.00000 0.05 1.98 Q34 1 0.1178 0.4441 -0.9455 11.00000 0.05 1.84 Q35 1 0.6474 0.5824 -0.6287 11.00000 0.05 1.83 Q36 1 0.2366 0.4942 -0.9187 11.00000 0.05 1.80 Q37 1 0.5828 0.5507 -0.5985 11.00000 0.05 1.76 Q38 1 0.4858 1.0074 -1.6325 11.00000 0.05 1.67 Q39 1 0.0172 0.4218 -0.9585 11.00000 0.05 1.67 Q40 1 0.7391 0.5943 -0.5136 11.00000 0.05 1.65 Q41 1 0.7613 0.6156 -0.5773 11.00000 0.05 1.61 Q42 1 0.2785 0.3860 -0.8593 11.00000 0.05 1.57 Q43 1 0.4351 1.0079 -1.7990 11.00000 0.05 1.55 Q44 1 0.3448 0.8342 -1.4277 11.00000 0.05 1.53 Q45 1 -0.1169 0.2707 -1.7805 11.00000 0.05 1.52 Q46 1 0.1169 0.5444 -1.0006 11.00000 0.05 1.51 Q47 1 0.3423 0.9207 -1.9133 11.00000 0.05 1.50 Q48 1 0.8161 0.6098 -0.5210 11.00000 0.05 1.49 Q49 1 0.1069 0.9759 -1.7139 11.00000 0.05 1.48 Q50 1 0.5737 0.5333 -0.5592 11.00000 0.05 1.48 ; _shelx_res_checksum 86123 _shelx_hkl_file ; -2 0 0 25.11 1.27 -2 0 0 29.60 1.14 -3 0 0 36.44 1.51 -3 0 0 35.36 1.75 -4 0 0 2.91 0.60 -4 0 0 1.95 0.38 -5 0 0 13.21 0.90 -5 0 0 14.86 1.21 -6 0 0 4.03 0.60 -6 0 0 5.02 0.83 -7 0 0 18.84 1.63 -7 0 0 18.10 1.26 -8 0 0 13.36 1.47 -8 0 0 13.05 1.19 -9 0 0 8.20 1.27 -9 0 0 8.18 1.07 -10 0 0 31.38 2.09 -11 0 0 2.22 0.92 -12 0 0 4.35 1.27 -13 0 0 7.63 1.52 -14 0 0 1.89 1.28 -14 1 0 2.46 1.32 -13 1 0 10.52 1.67 -12 1 0 11.44 1.52 -11 1 0 3.76 0.99 -10 1 0 17.38 1.54 -9 1 0 17.12 1.70 -9 1 0 20.09 1.50 -8 1 0 64.93 3.35 -8 1 0 58.81 2.81 -7 1 0 1.01 0.67 -7 1 0 0.40 0.40 -6 1 0 4.20 0.56 -6 1 0 4.75 0.77 -5 1 0 1.11 0.55 -5 1 0 0.17 0.32 4 -1 0 49.58 2.37 -4 1 0 51.23 2.06 3 -1 0 29.41 1.44 -3 1 0 27.23 1.19 2 -1 0 12.11 0.67 1 -1 0 300.92 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