# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_Complex_1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C96 H148 N32 Pd6), 12(N O3), 42.5(H2O)' _chemical_formula_sum 'C96 H233 N44 O78.5 Pd6' _chemical_formula_weight 3898.54 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' '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' 'Pd' 'Pd' -0.9988 1.0072 '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' _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 17.4691(17) _cell_length_b 21.082(2) _cell_length_c 21.428(2) _cell_angle_alpha 95.022(5) _cell_angle_beta 91.544(4) _cell_angle_gamma 98.679(5) _cell_volume 7764.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26909 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'colorless' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.667 _exptl_crystal_F_000 4065.0 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.794 _shelx_estimated_absorpt_T_min 0.921 _shelx_estimated_absorpt_T_max 0.959 _exptl_absorpt_correction_type 'EMPIRICAL' _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details 'SADBAS' _exptl_special_details ; 'The refinement was carried out employing OMIT 0 50 restrain keep the coverage 25. and therby to increase the data completeness.We have used DFIX restraints on N10 C26, N10 C27, C27 C28, C28 N9, C9 C10, C26 C27, We have used EADP constraint on C26 C27, C28 C27.' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_reflns_number 122039 _diffrn_reflns_av_unetI/netI 0.0642 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.180 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measured_fraction_theta_full 0.957 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_Laue_measured_fraction_full 0.957 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_point_group_measured_fraction_full 0.957 _reflns_number_total 26909 _reflns_number_gt 19419 _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 'Bruker kappa Apex-II ccd' _computing_cell_refinement 'Bruker saint' _computing_data_reduction 'Bruker saint' _computing_structure_solution SHELXL-2013 _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ORTEP-III _computing_publication_material WinGXv1.80.05 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0622P)^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 26909 _refine_ls_number_parameters 1195 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.009 _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 C1 C 0.4378(3) 0.4392(2) 0.5742(2) 0.0420(11) Uani 1 1 d . . . . . H1A H 0.3954 0.4488 0.5491 0.063 Uiso 1 1 calc R U . . . H1B H 0.4803 0.4740 0.5752 0.063 Uiso 1 1 calc R U . . . H1C H 0.4215 0.4338 0.6161 0.063 Uiso 1 1 calc R U . . . C2 C 0.5266(3) 0.3645(2) 0.5850(3) 0.0669(18) Uani 1 1 d . . . . . H2A H 0.5424 0.3257 0.5664 0.100 Uiso 1 1 calc R U . . . H2B H 0.5103 0.3582 0.6267 0.100 Uiso 1 1 calc R U . . . H2C H 0.5692 0.3992 0.5865 0.100 Uiso 1 1 calc R U . . . C3 C 0.4845(3) 0.3906(3) 0.4805(3) 0.0626(16) Uani 1 1 d . . . . . H3A H 0.4518 0.4187 0.4633 0.075 Uiso 1 1 calc R U . . . H3B H 0.5378 0.4120 0.4808 0.075 Uiso 1 1 calc R U . . . C4 C 0.4767(3) 0.3317(3) 0.4413(3) 0.0704(18) Uani 1 1 d . . . . . H4A H 0.5151 0.3063 0.4545 0.084 Uiso 1 1 calc R U . . . H4B H 0.4862 0.3409 0.3984 0.084 Uiso 1 1 calc R U . . . C5 C 0.4008(3) 0.2252(3) 0.4195(2) 0.0637(16) Uani 1 1 d . . . . . H5A H 0.4389 0.2081 0.4435 0.096 Uiso 1 1 calc R U . . . H5B H 0.4142 0.2236 0.3763 0.096 Uiso 1 1 calc R U . . . H5C H 0.3508 0.1999 0.4230 0.096 Uiso 1 1 calc R U . . . C6 C 0.3402(3) 0.3176(3) 0.4056(2) 0.0629(15) Uani 1 1 d . . . . . H6A H 0.3368 0.3615 0.4202 0.094 Uiso 1 1 calc R U . . . H6B H 0.2908 0.2914 0.4087 0.094 Uiso 1 1 calc R U . . . H6C H 0.3548 0.3155 0.3627 0.094 Uiso 1 1 calc R U . . . C7 C -0.0774(3) 0.3239(4) 0.3273(3) 0.098(3) Uani 1 1 d . . . . . H7A H -0.0466 0.3615 0.3485 0.146 Uiso 1 1 calc R U . . . H7B H -0.0660 0.3210 0.2837 0.146 Uiso 1 1 calc R U . . . H7C H -0.0657 0.2862 0.3454 0.146 Uiso 1 1 calc R U . . . C8 C -0.2040(3) 0.2702(3) 0.3000(2) 0.0658(16) Uani 1 1 d . . . . . H8A H -0.2585 0.2718 0.3017 0.099 Uiso 1 1 calc R U . . . H8B H -0.1924 0.2330 0.3190 0.099 Uiso 1 1 calc R U . . . H8C H -0.1895 0.2676 0.2571 0.099 Uiso 1 1 calc R U . . . C9 C -0.1788(5) 0.3862(3) 0.3061(3) 0.094(2) Uani 1 1 d D . . . . H9A H -0.1313 0.4167 0.3057 0.113 Uiso 1 1 calc R U . . . H9B H -0.1966 0.3739 0.2629 0.113 Uiso 1 1 calc R U . . . C10 C -0.2325(5) 0.4165(5) 0.3353(4) 0.135(4) Uani 1 1 d D . . . . H10A H -0.2834 0.3954 0.3196 0.162 Uiso 1 1 calc R U . . . H10B H -0.2262 0.4605 0.3240 0.162 Uiso 1 1 calc R U . . . C11 C -0.1800(5) 0.4763(4) 0.4339(6) 0.166(5) Uani 1 1 d . . . . . H11A H -0.1279 0.4756 0.4212 0.250 Uiso 1 1 calc R U . . . H11B H -0.1811 0.4785 0.4788 0.250 Uiso 1 1 calc R U . . . H11C H -0.1985 0.5134 0.4195 0.250 Uiso 1 1 calc R U . . . C12 C -0.3103(4) 0.4180(4) 0.4247(3) 0.096(2) Uani 1 1 d . . . . . H12A H -0.3415 0.3786 0.4075 0.144 Uiso 1 1 calc R U . . . H12B H -0.3297 0.4539 0.4087 0.144 Uiso 1 1 calc R U . . . H12C H -0.3124 0.4214 0.4696 0.144 Uiso 1 1 calc R U . . . C13 C -0.3771(3) 0.4679(2) 1.0269(3) 0.0614(15) Uani 1 1 d . . . . . H13A H -0.3744 0.4642 0.9821 0.092 Uiso 1 1 calc R U . . . H13B H -0.3256 0.4759 1.0457 0.092 Uiso 1 1 calc R U . . . H13C H -0.4041 0.5030 1.0399 0.092 Uiso 1 1 calc R U . . . C14 C -0.4988(3) 0.3958(3) 1.0195(3) 0.0603(15) Uani 1 1 d . . . . . H14A H -0.4972 0.3912 0.9746 0.090 Uiso 1 1 calc R U . . . H14B H -0.5247 0.4316 1.0324 0.090 Uiso 1 1 calc R U . . . H14C H -0.5266 0.3572 1.0336 0.090 Uiso 1 1 calc R U . . . C15 C -0.4217(3) 0.4140(2) 1.1163(2) 0.0517(13) Uani 1 1 d . . . . . H15A H -0.4615 0.4394 1.1290 0.062 Uiso 1 1 calc R U . . . H15B H -0.3723 0.4363 1.1342 0.062 Uiso 1 1 calc R U . . . C16 C -0.4386(3) 0.3496(2) 1.1396(2) 0.0533(13) Uani 1 1 d . . . . . H16A H -0.4899 0.3288 1.1245 0.064 Uiso 1 1 calc R U . . . H16B H -0.4375 0.3539 1.1850 0.064 Uiso 1 1 calc R U . . . C17 C -0.4085(3) 0.2424(2) 1.1258(2) 0.0532(13) Uani 1 1 d . . . . . H17A H -0.4569 0.2289 1.1025 0.080 Uiso 1 1 calc R U . . . H17B H -0.4160 0.2377 1.1694 0.080 Uiso 1 1 calc R U . . . H17C H -0.3712 0.2162 1.1108 0.080 Uiso 1 1 calc R U . . . C18 C -0.3068(3) 0.3295(3) 1.1528(2) 0.0714(17) Uani 1 1 d . . . . . H18A H -0.2876 0.3737 1.1475 0.107 Uiso 1 1 calc R U . . . H18B H -0.2699 0.3029 1.1377 0.107 Uiso 1 1 calc R U . . . H18C H -0.3143 0.3247 1.1964 0.107 Uiso 1 1 calc R U . . . C19 C 0.2743(4) 0.4561(3) 1.1624(4) 0.086(2) Uani 1 1 d . . . . . H19A H 0.2222 0.4647 1.1670 0.129 Uiso 1 1 calc R U . . . H19B H 0.2872 0.4566 1.1192 0.129 Uiso 1 1 calc R U . . . H19C H 0.3094 0.4885 1.1874 0.129 Uiso 1 1 calc R U . . . C20 C 0.3609(3) 0.3797(3) 1.1758(2) 0.0643(16) Uani 1 1 d . . . . . H20A H 0.3651 0.3381 1.1891 0.096 Uiso 1 1 calc R U . . . H20B H 0.3961 0.4121 1.2008 0.096 Uiso 1 1 calc R U . . . H20C H 0.3736 0.3806 1.1325 0.096 Uiso 1 1 calc R U . . . C21 C 0.2586(4) 0.3938(4) 1.2495(3) 0.098(3) Uani 1 1 d . . . . . H21A H 0.3050 0.4088 1.2758 0.117 Uiso 1 1 calc R U . . . H21B H 0.2238 0.4252 1.2568 0.117 Uiso 1 1 calc R U . . . C22 C 0.2247(3) 0.3377(4) 1.2684(2) 0.090(2) Uani 1 1 d . . . . . H22A H 0.1989 0.3467 1.3070 0.108 Uiso 1 1 calc R U . . . H22B H 0.2648 0.3125 1.2779 0.108 Uiso 1 1 calc R U . . . C23 C 0.1553(6) 0.2291(4) 1.2315(3) 0.137(4) Uani 1 1 d . . . . . H23A H 0.1178 0.2070 1.2005 0.205 Uiso 1 1 calc R U . . . H23B H 0.1368 0.2226 1.2726 0.205 Uiso 1 1 calc R U . . . H23C H 0.2033 0.2126 1.2268 0.205 Uiso 1 1 calc R U . . . C24 C 0.0913(3) 0.3201(4) 1.2316(3) 0.115(3) Uani 1 1 d . . . . . H24A H 0.0538 0.2952 1.2021 0.172 Uiso 1 1 calc R U . . . H24B H 0.0958 0.3649 1.2245 0.172 Uiso 1 1 calc R U . . . H24C H 0.0750 0.3145 1.2735 0.172 Uiso 1 1 calc R U . . . C25 C 0.2078(3) -0.0705(3) 0.6997(3) 0.0591(15) Uani 1 1 d . . . . . H25A H 0.1617 -0.0916 0.7171 0.089 Uiso 1 1 calc R U . . . H25B H 0.2348 -0.1023 0.6791 0.089 Uiso 1 1 calc R U . . . H25C H 0.1939 -0.0423 0.6699 0.089 Uiso 1 1 calc R U . . . C26 C 0.3238(5) 0.0000(4) 0.7168(4) 0.132(2) Uani 1 1 d D . . . . H26A H 0.3601 0.0255 0.7469 0.198 Uiso 1 1 calc R U . . . H26B H 0.3049 0.0274 0.6884 0.198 Uiso 1 1 calc R U . . . H26C H 0.3489 -0.0316 0.6937 0.198 Uiso 1 1 calc R U . . . C27 C 0.2845(5) -0.0778(4) 0.7927(4) 0.132(2) Uani 1 1 d D . . . . H27A H 0.2590 -0.1208 0.7776 0.158 Uiso 1 1 calc R U . . . H27B H 0.3394 -0.0772 0.7865 0.158 Uiso 1 1 calc R U . . . C28 C 0.2759(5) -0.0713(4) 0.8553(4) 0.132(2) Uani 1 1 d D . . . . H28A H 0.3269 -0.0643 0.8761 0.158 Uiso 1 1 calc R U . . . H28B H 0.2483 -0.1114 0.8676 0.158 Uiso 1 1 calc R U . . . C29 C 0.2879(4) 0.0242(3) 0.9244(3) 0.099(3) Uani 1 1 d . . . . . H29A H 0.3330 0.0430 0.9041 0.149 Uiso 1 1 calc R U . . . H29B H 0.3034 -0.0007 0.9567 0.149 Uiso 1 1 calc R U . . . H29C H 0.2617 0.0577 0.9427 0.149 Uiso 1 1 calc R U . . . C30 C 0.1669(3) -0.0478(2) 0.9084(2) 0.0577(15) Uani 1 1 d . . . . . H30A H 0.1329 -0.0758 0.8784 0.087 Uiso 1 1 calc R U . . . H30B H 0.1402 -0.0146 0.9266 0.087 Uiso 1 1 calc R U . . . H30C H 0.1830 -0.0723 0.9407 0.087 Uiso 1 1 calc R U . . . C31 C -0.3167(3) -0.0403(3) 0.5806(2) 0.0573(15) Uani 1 1 d . . . . . H31A H -0.2907 -0.0656 0.6070 0.086 Uiso 1 1 calc R U . . . H31B H -0.2794 -0.0077 0.5652 0.086 Uiso 1 1 calc R U . . . H31C H -0.3429 -0.0677 0.5459 0.086 Uiso 1 1 calc R U . . . C32 C -0.4124(3) 0.0290(3) 0.5779(2) 0.0587(14) Uani 1 1 d . . . . . H32A H -0.4485 0.0496 0.6023 0.088 Uiso 1 1 calc R U . . . H32B H -0.4398 0.0019 0.5435 0.088 Uiso 1 1 calc R U . . . H32C H -0.3750 0.0611 0.5620 0.088 Uiso 1 1 calc R U . . . C33 C -0.4299(3) -0.0606(3) 0.6422(2) 0.0551(14) Uani 1 1 d . . . . . H33A H -0.4696 -0.0778 0.6101 0.066 Uiso 1 1 calc R U . . . H33B H -0.4033 -0.0956 0.6530 0.066 Uiso 1 1 calc R U . . . C34 C -0.4660(3) -0.0360(3) 0.6969(2) 0.0604(15) Uani 1 1 d . . . . . H34A H -0.4979 -0.0711 0.7147 0.072 Uiso 1 1 calc R U . . . H34B H -0.4993 -0.0057 0.6852 0.072 Uiso 1 1 calc R U . . . C35 C -0.3713(3) -0.0485(3) 0.7792(3) 0.0725(18) Uani 1 1 d . . . . . H35A H -0.3331 -0.0248 0.8089 0.109 Uiso 1 1 calc R U . . . H35B H -0.3471 -0.0765 0.7510 0.109 Uiso 1 1 calc R U . . . H35C H -0.4105 -0.0737 0.8011 0.109 Uiso 1 1 calc R U . . . C36 C -0.4457(3) 0.0393(3) 0.7894(3) 0.0762(19) Uani 1 1 d . . . . . H36A H -0.4697 0.0689 0.7667 0.114 Uiso 1 1 calc R U . . . H36B H -0.4076 0.0630 0.8192 0.114 Uiso 1 1 calc R U . . . H36C H -0.4843 0.0132 0.8109 0.114 Uiso 1 1 calc R U . . . C37 C 0.2142(2) 0.22849(18) 0.53325(16) 0.0238(8) Uani 1 1 d . . . . . H37 H 0.1915 0.2652 0.5297 0.029 Uiso 1 1 calc R U . . . C38 C 0.2986(2) 0.16461(19) 0.53935(18) 0.0288(9) Uani 1 1 d . . . . . H38 H 0.3461 0.1498 0.5405 0.035 Uiso 1 1 calc R U . . . C39 C 0.2294(2) 0.12849(19) 0.54642(18) 0.0272(9) Uani 1 1 d . . . . . H39 H 0.2199 0.0850 0.5528 0.033 Uiso 1 1 calc R U . . . C40 C -0.0878(2) 0.2476(2) 0.47556(18) 0.0332(10) Uani 1 1 d . . . . . H40 H -0.0470 0.2807 0.4868 0.040 Uiso 1 1 calc R U . . . C41 C -0.1596(2) 0.1518(2) 0.46466(19) 0.0368(11) Uani 1 1 d . . . . . H41 H -0.1767 0.1082 0.4671 0.044 Uiso 1 1 calc R U . . . C42 C -0.1968(2) 0.1923(2) 0.43768(19) 0.0370(11) Uani 1 1 d . . . . . H42 H -0.2454 0.1820 0.4173 0.044 Uiso 1 1 calc R U . . . C43 C -0.1760(2) 0.0864(2) 0.62867(18) 0.0298(9) Uani 1 1 d . . . . . H43 H -0.1579 0.0478 0.6336 0.036 Uiso 1 1 calc R U . . . C44 C -0.1811(2) 0.1853(2) 0.60514(19) 0.0313(10) Uani 1 1 d . . . . . H44 H -0.1681 0.2260 0.5913 0.038 Uiso 1 1 calc R U . . . C45 C -0.2482(2) 0.1616(2) 0.63005(18) 0.0320(10) Uani 1 1 d . . . . . H45 H -0.2901 0.1835 0.6365 0.038 Uiso 1 1 calc R U . . . C46 C 0.1273(2) 0.07392(18) 0.69155(17) 0.0245(9) Uani 1 1 d . . . . . H46 H 0.0897 0.0374 0.6863 0.029 Uiso 1 1 calc R U . . . C47 C 0.2276(2) 0.14303(18) 0.72642(17) 0.0267(9) Uani 1 1 d . . . . . H47 H 0.2721 0.1618 0.7499 0.032 Uiso 1 1 calc R U . . . C48 C 0.1924(2) 0.16994(19) 0.68069(18) 0.0280(9) Uani 1 1 d . . . . . H48 H 0.2076 0.2104 0.6669 0.034 Uiso 1 1 calc R U . . . C49 C 0.0721(2) 0.24863(19) 1.05704(17) 0.0258(9) Uani 1 1 d . . . . . H49 H 0.0498 0.2857 1.0542 0.031 Uiso 1 1 calc R U . . . C50 C 0.1474(3) 0.1827(2) 1.0832(2) 0.0398(11) Uani 1 1 d . . . . . H50 H 0.1876 0.1665 1.1028 0.048 Uiso 1 1 calc R U . . . C51 C 0.0946(2) 0.1487(2) 1.0416(2) 0.0359(10) Uani 1 1 d . . . . . H51 H 0.0914 0.1056 1.0269 0.043 Uiso 1 1 calc R U . . . C52 C -0.2372(2) 0.25334(19) 0.99620(18) 0.0296(9) Uani 1 1 d . . . . . H52 H -0.1999 0.2897 1.0048 0.035 Uiso 1 1 calc R U . . . C53 C -0.2924(2) 0.15373(19) 0.96597(19) 0.0296(9) Uani 1 1 d . . . . . H53 H -0.3003 0.1105 0.9505 0.036 Uiso 1 1 calc R U . . . C54 C -0.3465(2) 0.18897(19) 0.98652(19) 0.0321(10) Uani 1 1 d . . . . . H54 H -0.3992 0.1739 0.9879 0.039 Uiso 1 1 calc R U . . . C55 C 0.0847(2) 0.09105(19) 0.86685(18) 0.0266(9) Uani 1 1 d . . . . . H55 H 0.0473 0.0563 0.8523 0.032 Uiso 1 1 calc R U . . . C56 C 0.1931(2) 0.15407(19) 0.88534(18) 0.0295(9) Uani 1 1 d . . . . . H56 H 0.2457 0.1699 0.8856 0.035 Uiso 1 1 calc R U . . . C57 C 0.1392(2) 0.1854(2) 0.91107(19) 0.0316(10) Uani 1 1 d . . . . . H57 H 0.1469 0.2264 0.9324 0.038 Uiso 1 1 calc R U . . . C58 C -0.2211(2) 0.09853(19) 0.80669(18) 0.0296(9) Uani 1 1 d . . . . . H58 H -0.1980 0.0615 0.8052 0.036 Uiso 1 1 calc R U . . . C59 C -0.2947(2) 0.1676(2) 0.78634(19) 0.0316(10) Uani 1 1 d . . . . . H59 H -0.3330 0.1866 0.7674 0.038 Uiso 1 1 calc R U . . . C60 C -0.2462(2) 0.19571(19) 0.83420(19) 0.0291(9) Uani 1 1 d . . . . . H60 H -0.2445 0.2368 0.8545 0.035 Uiso 1 1 calc R U . . . C61 C 0.0963(2) 0.15792(18) 0.55620(17) 0.0233(8) Uani 1 1 d . . . . . C62 C 0.0406(2) 0.17360(19) 0.51422(17) 0.0272(9) Uani 1 1 d . . . . . H62 H 0.0553 0.1894 0.4764 0.033 Uiso 1 1 calc R U . . . C63 C -0.0351(2) 0.1655(2) 0.52951(17) 0.0285(9) Uani 1 1 d . . . . . C64 C -0.0582(2) 0.14166(19) 0.58512(17) 0.0260(9) Uani 1 1 d . . . . . C65 C -0.0035(2) 0.12517(19) 0.62656(18) 0.0267(9) Uani 1 1 d . . . . . H65 H -0.0188 0.1081 0.6636 0.032 Uiso 1 1 calc R U . . . C66 C 0.0733(2) 0.13433(18) 0.61236(17) 0.0244(8) Uani 1 1 d . . . . . C67 C -0.1486(2) 0.18050(18) 0.95473(18) 0.0270(9) Uani 1 1 d . . . . . C68 C -0.0884(2) 0.19100(18) 0.99791(18) 0.0287(9) Uani 1 1 d . . . . . H68 H -0.0961 0.2057 1.0391 0.034 Uiso 1 1 calc R U . . . C69 C -0.0160(2) 0.17968(18) 0.98024(18) 0.0291(9) Uani 1 1 d . . . . . C70 C -0.0052(2) 0.15709(19) 0.91894(18) 0.0290(9) Uani 1 1 d . . . . . C71 C -0.0664(2) 0.14580(18) 0.87558(18) 0.0275(9) Uani 1 1 d . . . . . H71 H -0.0596 0.1291 0.8348 0.033 Uiso 1 1 calc R U . . . C72 C -0.1376(2) 0.15943(19) 0.89291(18) 0.0291(9) Uani 1 1 d . . . . . C73 C 0.2993(3) 0.3439(2) 0.6534(2) 0.0365(10) Uani 1 1 d . . . . . H73 H 0.2728 0.3667 0.6270 0.044 Uiso 1 1 calc R U . . . C74 C 0.2815(3) 0.3447(2) 0.7161(2) 0.0425(12) Uani 1 1 d . . . . . H74 H 0.2437 0.3677 0.7318 0.051 Uiso 1 1 calc R U . . . C75 C 0.3224(3) 0.3096(2) 0.7560(2) 0.0483(13) Uani 1 1 d . . . . . C76 C 0.3765(3) 0.2781(2) 0.7302(2) 0.0477(13) Uani 1 1 d . . . . . H76 H 0.4051 0.2556 0.7553 0.057 Uiso 1 1 calc R U . . . C77 C 0.3907(2) 0.2783(2) 0.6678(2) 0.0378(11) Uani 1 1 d . . . . . H77 H 0.4276 0.2547 0.6515 0.045 Uiso 1 1 calc R U . . . C78 C 0.3061(4) 0.3071(2) 0.8246(2) 0.0744(19) Uani 1 1 d . . . . . H78A H 0.2655 0.2710 0.8283 0.089 Uiso 1 1 calc R U . . . H78B H 0.3523 0.2979 0.8459 0.089 Uiso 1 1 calc R U . . . C79 C 0.2832(3) 0.3638(3) 0.8580(2) 0.0573(14) Uani 1 1 d . . . . . H79A H 0.2356 0.3726 0.8386 0.069 Uiso 1 1 calc R U . . . H79B H 0.3230 0.4006 0.8543 0.069 Uiso 1 1 calc R U . . . C80 C 0.2936(3) 0.3104(2) 1.0224(2) 0.0464(12) Uani 1 1 d . . . . . H80 H 0.3195 0.2833 1.0444 0.056 Uiso 1 1 calc R U . . . C81 C 0.3110(3) 0.3190(3) 0.9606(2) 0.0539(14) Uani 1 1 d . . . . . H81 H 0.3501 0.2994 0.9421 0.065 Uiso 1 1 calc R U . . . C82 C 0.2710(3) 0.3561(2) 0.9270(2) 0.0443(12) Uani 1 1 d . . . . . C83 C 0.2151(3) 0.3855(2) 0.9560(2) 0.0576(14) Uani 1 1 d . . . . . H83 H 0.1861 0.4105 0.9340 0.069 Uiso 1 1 calc R U . . . C84 C 0.2024(3) 0.3775(2) 1.0175(2) 0.0520(13) Uani 1 1 d . . . . . H84 H 0.1656 0.3990 1.0371 0.062 Uiso 1 1 calc R U . . . C85 C -0.1662(4) 0.3742(3) 0.5638(3) 0.0770(19) Uani 1 1 d . . . . . H85 H -0.1209 0.3992 0.5529 0.092 Uiso 1 1 calc R U . . . C86 C -0.1797(4) 0.3686(3) 0.6260(3) 0.0795(19) Uani 1 1 d . . . . . H86 H -0.1416 0.3870 0.6562 0.095 Uiso 1 1 calc R U . . . C87 C -0.2484(4) 0.3364(3) 0.6445(3) 0.0651(16) Uani 1 1 d . . . . . C88 C -0.2995(3) 0.3068(3) 0.5978(3) 0.0570(15) Uani 1 1 d . . . . . H88 H -0.3465 0.2841 0.6083 0.068 Uiso 1 1 calc R U . . . C89 C -0.2834(3) 0.3096(3) 0.5357(2) 0.0504(13) Uani 1 1 d . . . . . H89 H -0.3188 0.2872 0.5053 0.060 Uiso 1 1 calc R U . . . C90 C -0.2616(4) 0.3291(3) 0.7150(3) 0.086(2) Uani 1 1 d . . . . . H90A H -0.2847 0.2849 0.7195 0.103 Uiso 1 1 calc R U . . . H90B H -0.2117 0.3368 0.7375 0.103 Uiso 1 1 calc R U . . . C91 C -0.3083(4) 0.3698(3) 0.7426(3) 0.085(2) Uani 1 1 d . . . . . H91A H -0.3575 0.3631 0.7191 0.102 Uiso 1 1 calc R U . . . H91B H -0.2843 0.4139 0.7392 0.102 Uiso 1 1 calc R U . . . C92 C -0.3236(4) 0.3617(3) 0.8100(2) 0.0581(15) Uani 1 1 d . . . . . C93 C -0.2685(3) 0.3867(2) 0.8547(3) 0.0579(15) Uani 1 1 d . . . . . H93 H -0.2215 0.4088 0.8434 0.070 Uiso 1 1 calc R U . . . C94 C -0.2822(3) 0.3791(2) 0.9185(2) 0.0455(12) Uani 1 1 d . . . . . H94 H -0.2442 0.3969 0.9490 0.055 Uiso 1 1 calc R U . . . C95 C -0.3914(3) 0.3277(3) 0.8283(2) 0.0595(14) Uani 1 1 d . . . . . H95 H -0.4298 0.3096 0.7983 0.071 Uiso 1 1 calc R U . . . C96 C -0.4028(3) 0.3204(2) 0.8907(2) 0.0469(12) Uani 1 1 d . . . . . H96 H -0.4488 0.2966 0.9021 0.056 Uiso 1 1 calc R U . . . N1 N 0.46232(19) 0.38018(17) 0.54744(18) 0.0381(9) Uani 1 1 d . . . . . N2 N 0.3985(2) 0.29412(17) 0.44414(16) 0.0371(9) Uani 1 1 d . . . . . N3 N -0.2295(3) 0.4180(3) 0.4068(3) 0.0774(15) Uani 1 1 d . . . . . N4 N -0.1606(2) 0.3284(2) 0.33391(19) 0.0518(11) Uani 1 1 d . . . . . N5 N -0.4192(2) 0.40733(17) 1.04715(17) 0.0390(9) Uani 1 1 d . . . . . N6 N -0.3804(2) 0.30987(18) 1.11746(16) 0.0392(9) Uani 1 1 d . . . . . N7 N 0.1678(2) 0.2982(2) 1.22344(17) 0.0600(13) Uani 1 1 d . . . . . N8 N 0.2805(2) 0.3929(2) 1.18321(18) 0.0470(10) Uani 1 1 d . . . . . N9 N 0.2345(2) -0.01880(17) 0.87725(17) 0.0418(9) Uani 1 1 d D . . . . N10 N 0.2579(2) -0.03308(19) 0.74990(19) 0.0448(10) Uani 1 1 d D . . . . N11 N -0.37324(19) -0.00971(18) 0.61680(17) 0.0403(9) Uani 1 1 d . . . . . N12 N -0.4067(2) -0.00365(18) 0.74385(17) 0.0388(9) Uani 1 1 d . . . . . N13 N 0.28854(18) 0.22654(16) 0.53019(14) 0.0274(8) Uani 1 1 d . . . . . N14 N 0.17517(16) 0.17020(15) 0.54218(14) 0.0239(7) Uani 1 1 d . . . . . N15 N -0.15199(19) 0.25375(19) 0.44431(16) 0.0381(9) Uani 1 1 d . . . . . N16 N -0.09025(18) 0.18653(17) 0.48859(15) 0.0302(8) Uani 1 1 d . . . . . N17 N -0.24523(17) 0.10012(16) 0.64440(15) 0.0289(8) Uani 1 1 d . . . . . N18 N -0.13647(17) 0.13800(15) 0.60435(14) 0.0252(7) Uani 1 1 d . . . . . N19 N 0.18572(17) 0.08260(15) 0.73216(15) 0.0271(7) Uani 1 1 d . . . . . N20 N 0.12920(17) 0.12511(15) 0.65860(14) 0.0236(7) Uani 1 1 d . . . . . N21 N -0.31120(19) 0.25105(15) 1.00515(15) 0.0295(8) Uani 1 1 d . . . . . N22 N -0.22303(18) 0.19515(16) 0.97273(15) 0.0290(8) Uani 1 1 d . . . . . N23 N 0.13294(19) 0.24498(16) 1.09241(15) 0.0304(8) Uani 1 1 d . . . . . N24 N 0.04594(18) 0.19104(15) 1.02517(15) 0.0299(8) Uani 1 1 d . . . . . N25 N 0.15850(17) 0.09471(15) 0.85845(14) 0.0236(7) Uani 1 1 d . . . . . N26 N 0.07040(18) 0.14514(15) 0.89978(15) 0.0286(8) Uani 1 1 d . . . . . N27 N -0.27902(17) 0.10704(15) 0.76993(15) 0.0273(7) Uani 1 1 d . . . . . N28 N -0.19985(18) 0.15111(15) 0.84675(15) 0.0285(8) Uani 1 1 d . . . . . N29 N 0.2395(2) 0.34072(17) 1.05108(16) 0.0370(9) Uani 1 1 d . . . . . N30 N 0.35356(18) 0.31106(16) 0.62956(15) 0.0305(8) Uani 1 1 d . . . . . N31 N -0.2173(2) 0.3441(2) 0.51730(19) 0.0510(11) Uani 1 1 d . . . . . N32 N -0.3494(2) 0.34654(16) 0.93567(17) 0.0351(8) Uani 1 1 d . . . . . Pd1 Pd 0.37385(2) 0.30326(2) 0.53768(2) 0.02690(8) Uani 1 1 d . . . . . Pd2 Pd -0.18842(2) 0.33675(2) 0.42658(2) 0.04299(10) Uani 1 1 d . . . . . Pd3 Pd -0.36458(2) 0.32863(2) 1.02557(2) 0.02927(8) Uani 1 1 d . . . . . Pd4 Pd 0.20462(2) 0.31956(2) 1.13694(2) 0.03007(9) Uani 1 1 d . . . . . Pd5 Pd 0.20861(2) 0.03087(2) 0.80363(2) 0.02547(8) Uani 1 1 d . . . . . Pd6 Pd -0.32465(2) 0.04841(2) 0.69414(2) 0.02737(8) 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 C1 0.041(3) 0.033(3) 0.050(3) 0.008(2) 0.001(2) -0.002(2) C2 0.024(3) 0.049(3) 0.129(5) 0.033(3) -0.018(3) 0.001(2) C3 0.057(3) 0.051(3) 0.077(4) 0.007(3) 0.038(3) -0.007(3) C4 0.059(4) 0.089(5) 0.052(3) 0.005(3) 0.024(3) -0.028(3) C5 0.094(4) 0.059(4) 0.045(3) 0.011(3) 0.022(3) 0.027(3) C6 0.073(4) 0.087(4) 0.033(3) 0.013(3) 0.009(3) 0.019(3) C7 0.059(4) 0.196(8) 0.044(4) 0.023(4) 0.011(3) 0.028(5) C8 0.092(4) 0.070(4) 0.035(3) 0.008(3) 0.005(3) 0.010(3) C9 0.162(7) 0.073(5) 0.055(4) 0.013(3) -0.014(4) 0.039(5) C10 0.174(8) 0.178(9) 0.104(6) 0.094(6) 0.069(6) 0.135(7) C11 0.132(8) 0.068(6) 0.304(16) 0.020(7) -0.044(9) 0.036(5) C12 0.090(5) 0.141(6) 0.080(5) 0.021(4) 0.009(4) 0.086(5) C13 0.064(4) 0.031(3) 0.089(4) -0.004(3) 0.019(3) 0.008(3) C14 0.049(3) 0.072(4) 0.065(4) -0.003(3) -0.006(3) 0.034(3) C15 0.065(3) 0.050(3) 0.043(3) -0.009(2) 0.010(2) 0.025(3) C16 0.066(3) 0.061(3) 0.041(3) 0.005(2) 0.018(2) 0.031(3) C17 0.081(4) 0.052(3) 0.032(3) 0.010(2) 0.018(3) 0.021(3) C18 0.070(4) 0.109(5) 0.037(3) -0.012(3) -0.012(3) 0.034(4) C19 0.066(4) 0.054(4) 0.131(6) -0.007(4) -0.023(4) 0.000(3) C20 0.028(3) 0.104(5) 0.055(3) -0.025(3) -0.008(2) 0.010(3) C21 0.091(5) 0.130(6) 0.044(4) -0.043(4) 0.018(3) -0.044(5) C22 0.061(4) 0.174(7) 0.018(3) 0.000(4) -0.001(2) -0.030(4) C23 0.261(11) 0.099(6) 0.044(4) 0.041(4) 0.017(6) -0.011(6) C24 0.040(4) 0.242(10) 0.055(4) 0.006(5) 0.027(3) -0.002(5) C25 0.044(3) 0.059(3) 0.067(4) -0.023(3) -0.006(3) 0.000(3) C26 0.143(4) 0.111(4) 0.152(5) -0.048(4) 0.009(4) 0.086(3) C27 0.143(4) 0.111(4) 0.152(5) -0.048(4) 0.009(4) 0.086(3) C28 0.143(4) 0.111(4) 0.152(5) -0.048(4) 0.009(4) 0.086(3) C29 0.147(6) 0.056(4) 0.084(5) 0.019(3) -0.082(5) -0.010(4) C30 0.081(4) 0.057(3) 0.043(3) 0.026(3) 0.025(3) 0.022(3) C31 0.029(3) 0.080(4) 0.056(3) -0.031(3) 0.000(2) 0.007(3) C32 0.055(3) 0.077(4) 0.040(3) 0.008(3) -0.018(2) 0.000(3) C33 0.036(3) 0.058(3) 0.061(4) -0.009(3) -0.004(2) -0.014(2) C34 0.046(3) 0.076(4) 0.048(3) 0.007(3) -0.007(2) -0.023(3) C35 0.066(4) 0.081(4) 0.070(4) 0.044(3) -0.022(3) -0.005(3) C36 0.064(4) 0.085(4) 0.072(4) -0.002(3) 0.045(3) -0.015(3) C37 0.021(2) 0.033(2) 0.019(2) 0.0073(17) 0.0017(15) 0.0057(17) C38 0.022(2) 0.035(2) 0.031(2) 0.0060(18) 0.0046(17) 0.0071(18) C39 0.025(2) 0.030(2) 0.028(2) 0.0036(17) 0.0060(17) 0.0051(18) C40 0.022(2) 0.058(3) 0.022(2) 0.003(2) 0.0007(16) 0.012(2) C41 0.018(2) 0.063(3) 0.028(2) -0.008(2) -0.0012(17) 0.008(2) C42 0.022(2) 0.060(3) 0.029(2) -0.005(2) -0.0023(18) 0.012(2) C43 0.021(2) 0.041(3) 0.025(2) -0.0019(18) -0.0011(16) 0.0012(18) C44 0.024(2) 0.039(3) 0.032(2) 0.0042(19) 0.0064(18) 0.0081(19) C45 0.027(2) 0.042(3) 0.030(2) -0.0004(19) 0.0076(18) 0.0149(19) C46 0.020(2) 0.028(2) 0.025(2) 0.0030(17) 0.0077(16) 0.0015(17) C47 0.024(2) 0.033(2) 0.022(2) -0.0002(17) -0.0014(16) 0.0002(18) C48 0.020(2) 0.033(2) 0.029(2) 0.0014(18) 0.0045(17) -0.0028(18) C49 0.023(2) 0.027(2) 0.026(2) -0.0019(17) 0.0008(17) 0.0053(17) C50 0.046(3) 0.036(3) 0.040(3) 0.018(2) -0.001(2) 0.006(2) C51 0.043(3) 0.028(2) 0.037(3) 0.0066(19) -0.003(2) 0.005(2) C52 0.030(2) 0.026(2) 0.032(2) -0.0004(18) 0.0075(18) 0.0019(18) C53 0.026(2) 0.027(2) 0.036(2) 0.0026(18) 0.0095(18) 0.0033(18) C54 0.032(2) 0.032(2) 0.031(2) 0.0029(19) 0.0078(18) 0.0020(19) C55 0.024(2) 0.027(2) 0.026(2) -0.0026(17) 0.0038(16) 0.0013(17) C56 0.019(2) 0.039(3) 0.029(2) 0.0049(19) 0.0028(17) -0.0010(19) C57 0.031(2) 0.028(2) 0.033(2) -0.0025(18) 0.0013(18) -0.0008(19) C58 0.029(2) 0.029(2) 0.030(2) -0.0032(18) 0.0100(18) 0.0027(18) C59 0.026(2) 0.040(3) 0.031(2) 0.0028(19) 0.0067(18) 0.0100(19) C60 0.025(2) 0.028(2) 0.034(2) 0.0018(18) 0.0048(18) 0.0051(18) C61 0.0144(19) 0.032(2) 0.022(2) 0.0039(17) 0.0010(15) -0.0029(16) C62 0.031(2) 0.038(2) 0.0122(19) 0.0056(17) 0.0021(16) 0.0036(18) C63 0.018(2) 0.046(3) 0.020(2) 0.0002(18) -0.0025(16) 0.0064(18) C64 0.0136(19) 0.040(2) 0.023(2) 0.0023(17) 0.0056(15) -0.0005(17) C65 0.021(2) 0.035(2) 0.023(2) 0.0013(17) 0.0009(16) 0.0030(17) C66 0.019(2) 0.030(2) 0.023(2) 0.0045(17) -0.0019(16) -0.0002(16) C67 0.023(2) 0.029(2) 0.028(2) -0.0012(17) 0.0048(17) 0.0034(17) C68 0.037(2) 0.024(2) 0.023(2) -0.0043(17) 0.0036(17) 0.0006(18) C69 0.031(2) 0.026(2) 0.029(2) -0.0035(17) -0.0018(18) 0.0019(18) C70 0.024(2) 0.032(2) 0.030(2) -0.0033(18) 0.0072(17) 0.0033(18) C71 0.028(2) 0.030(2) 0.022(2) -0.0049(17) 0.0036(17) 0.0030(18) C72 0.027(2) 0.029(2) 0.028(2) -0.0081(18) -0.0010(17) -0.0022(18) C73 0.046(3) 0.029(2) 0.031(2) 0.0021(19) 0.004(2) -0.005(2) C74 0.062(3) 0.030(3) 0.031(3) -0.006(2) 0.010(2) -0.002(2) C75 0.076(4) 0.034(3) 0.025(2) -0.003(2) -0.007(2) -0.016(3) C76 0.047(3) 0.046(3) 0.044(3) 0.012(2) -0.019(2) -0.012(2) C77 0.036(3) 0.045(3) 0.030(2) 0.012(2) -0.0091(19) -0.004(2) C78 0.149(6) 0.045(3) 0.025(3) 0.006(2) 0.018(3) 0.000(4) C79 0.075(4) 0.060(3) 0.038(3) 0.012(3) 0.013(3) 0.007(3) C80 0.033(3) 0.071(4) 0.036(3) 0.005(2) 0.009(2) 0.008(2) C81 0.040(3) 0.087(4) 0.031(3) -0.007(3) 0.006(2) 0.005(3) C82 0.057(3) 0.035(3) 0.036(3) 0.008(2) 0.003(2) -0.008(2) C83 0.096(4) 0.043(3) 0.039(3) 0.015(2) 0.014(3) 0.020(3) C84 0.076(4) 0.046(3) 0.040(3) 0.017(2) 0.015(3) 0.022(3) C85 0.065(4) 0.098(5) 0.059(4) -0.024(3) 0.016(3) -0.004(4) C86 0.093(5) 0.093(5) 0.045(4) -0.022(3) 0.011(3) 0.006(4) C87 0.085(4) 0.067(4) 0.050(4) 0.003(3) 0.028(3) 0.032(3) C88 0.045(3) 0.074(4) 0.065(4) 0.022(3) 0.025(3) 0.038(3) C89 0.035(3) 0.067(4) 0.052(3) -0.003(3) -0.001(2) 0.025(3) C90 0.112(5) 0.096(5) 0.063(4) 0.010(3) 0.039(4) 0.050(4) C91 0.116(5) 0.100(5) 0.058(4) 0.031(3) 0.041(4) 0.059(4) C92 0.077(4) 0.067(4) 0.039(3) 0.014(3) 0.022(3) 0.031(3) C93 0.077(4) 0.040(3) 0.060(4) 0.014(3) 0.029(3) 0.012(3) C94 0.050(3) 0.037(3) 0.052(3) 0.013(2) 0.021(2) 0.006(2) C95 0.069(4) 0.071(4) 0.041(3) 0.005(3) 0.006(3) 0.015(3) C96 0.063(3) 0.043(3) 0.036(3) 0.006(2) 0.007(2) 0.009(2) N1 0.030(2) 0.034(2) 0.051(2) 0.0125(18) 0.0061(17) 0.0044(16) N2 0.040(2) 0.041(2) 0.030(2) 0.0099(17) 0.0160(16) -0.0001(17) N3 0.066(3) 0.080(4) 0.097(4) 0.013(3) 0.016(3) 0.043(3) N4 0.047(3) 0.070(3) 0.043(2) 0.009(2) -0.0093(19) 0.022(2) N5 0.040(2) 0.039(2) 0.039(2) -0.0071(17) 0.0089(17) 0.0125(17) N6 0.046(2) 0.048(2) 0.026(2) -0.0066(17) 0.0040(16) 0.0178(19) N7 0.053(3) 0.101(4) 0.021(2) 0.001(2) 0.0047(18) -0.005(2) N8 0.035(2) 0.057(3) 0.043(2) -0.014(2) 0.0025(17) -0.0008(19) N9 0.048(2) 0.037(2) 0.040(2) 0.0039(17) -0.0160(18) 0.0090(18) N10 0.028(2) 0.057(3) 0.054(3) -0.005(2) -0.0020(18) 0.0262(19) N11 0.027(2) 0.054(2) 0.037(2) -0.0029(18) -0.0053(16) 0.0020(18) N12 0.031(2) 0.048(2) 0.035(2) 0.0115(18) 0.0030(16) -0.0024(17) N13 0.0238(18) 0.038(2) 0.0204(17) 0.0058(15) 0.0075(13) 0.0021(15) N14 0.0162(16) 0.0336(19) 0.0215(17) 0.0050(14) 0.0020(13) 0.0014(14) N15 0.0262(19) 0.065(3) 0.0259(19) -0.0001(17) -0.0029(15) 0.0181(19) N16 0.0213(18) 0.048(2) 0.0213(18) 0.0031(16) 0.0001(13) 0.0056(16) N17 0.0165(17) 0.040(2) 0.0285(19) -0.0041(15) 0.0021(14) 0.0013(15) N18 0.0171(16) 0.037(2) 0.0225(17) 0.0012(14) 0.0053(13) 0.0066(15) N19 0.0185(17) 0.036(2) 0.0278(18) 0.0061(15) 0.0074(14) 0.0031(15) N20 0.0204(17) 0.0296(18) 0.0205(17) 0.0050(14) 0.0041(13) 0.0003(14) N21 0.031(2) 0.0277(19) 0.0301(19) -0.0018(15) 0.0095(15) 0.0054(15) N22 0.0245(18) 0.034(2) 0.0272(19) -0.0058(15) 0.0055(14) 0.0045(15) N23 0.034(2) 0.031(2) 0.0257(19) 0.0037(15) 0.0027(15) 0.0047(16) N24 0.0301(19) 0.0276(19) 0.033(2) -0.0022(15) 0.0023(15) 0.0095(15) N25 0.0188(17) 0.0267(18) 0.0262(18) 0.0057(14) 0.0032(13) 0.0042(14) N26 0.0245(18) 0.0299(19) 0.0301(19) 0.0018(15) 0.0028(14) -0.0002(15) N27 0.0211(17) 0.035(2) 0.0259(18) 0.0009(15) 0.0034(14) 0.0059(15) N28 0.0274(18) 0.0308(19) 0.0250(18) -0.0050(15) 0.0027(14) 0.0015(15) N29 0.041(2) 0.040(2) 0.0268(19) 0.0014(16) 0.0054(16) -0.0028(18) N30 0.0272(19) 0.038(2) 0.0235(18) 0.0011(15) -0.0022(14) -0.0015(16) N31 0.039(2) 0.072(3) 0.045(3) -0.002(2) 0.0110(19) 0.018(2) N32 0.034(2) 0.031(2) 0.042(2) 0.0017(17) 0.0073(17) 0.0095(16) Pd1 0.01953(16) 0.03305(18) 0.02863(17) 0.00789(13) 0.00646(12) 0.00182(13) Pd2 0.0343(2) 0.0640(3) 0.0349(2) 0.00195(17) 0.00059(15) 0.02302(18) Pd3 0.02816(18) 0.03071(18) 0.02921(18) -0.00207(14) 0.00708(13) 0.00719(14) Pd4 0.02809(18) 0.0393(2) 0.02079(16) -0.00100(14) 0.00243(13) 0.00073(14) Pd5 0.02296(16) 0.02896(18) 0.02575(17) 0.00288(13) -0.00083(12) 0.00818(13) Pd6 0.01700(16) 0.03593(19) 0.02777(17) -0.00059(14) 0.00103(12) 0.00158(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.452(5) . ? C2 N1 1.458(6) . ? C3 C4 1.424(7) . ? C3 N1 1.523(6) . ? C4 N2 1.477(6) . ? C5 N2 1.509(6) . ? C6 N2 1.463(6) . ? C7 N4 1.480(7) . ? C8 N4 1.463(6) . ? C9 C10 1.349(8) . ? C9 N4 1.475(7) . ? C10 N3 1.530(9) . ? C11 N3 1.457(9) . ? C12 N3 1.472(7) . ? C13 N5 1.480(6) . ? C14 N5 1.474(6) . ? C15 N5 1.478(6) . ? C15 C16 1.480(7) . ? C16 N6 1.473(6) . ? C17 N6 1.461(6) . ? C18 N6 1.460(6) . ? C19 N8 1.459(7) . ? C20 N8 1.483(6) . ? C21 C22 1.341(9) . ? C21 N8 1.481(7) . ? C22 N7 1.472(7) . ? C23 N7 1.465(8) . ? C24 N7 1.489(8) . ? C25 N10 1.463(6) . ? C26 N10 1.483(8) . ? C27 C28 1.351(10) . ? C27 N10 1.485(8) . ? C28 N9 1.463(7) . ? C29 N9 1.499(6) . ? C30 N9 1.453(6) . ? C31 N11 1.463(6) . ? C32 N11 1.444(6) . ? C33 C34 1.439(7) . ? C33 N11 1.497(6) . ? C34 N12 1.470(6) . ? C35 N12 1.458(6) . ? C36 N12 1.517(6) . ? C37 N13 1.308(5) . ? C37 N14 1.344(5) . ? C38 C39 1.348(5) . ? C38 N13 1.374(5) . ? C39 N14 1.393(5) . ? C40 N15 1.320(5) . ? C40 N16 1.335(5) . ? C41 C42 1.312(6) . ? C41 N16 1.378(5) . ? C42 N15 1.402(6) . ? C43 N17 1.331(5) . ? C43 N18 1.351(5) . ? C44 C45 1.347(5) . ? C44 N18 1.356(5) . ? C45 N17 1.365(5) . ? C46 N19 1.304(5) . ? C46 N20 1.337(5) . ? C47 C48 1.353(5) . ? C47 N19 1.387(5) . ? C48 N20 1.383(5) . ? C49 N23 1.305(5) . ? C49 N24 1.349(5) . ? C50 C51 1.344(6) . ? C50 N23 1.373(5) . ? C51 N24 1.381(5) . ? C52 N21 1.306(5) . ? C52 N22 1.345(5) . ? C53 C54 1.347(5) . ? C53 N22 1.379(5) . ? C54 N21 1.380(5) . ? C55 N25 1.298(5) . ? C55 N26 1.347(5) . ? C56 C57 1.334(5) . ? C56 N25 1.375(5) . ? C57 N26 1.365(5) . ? C58 N27 1.309(5) . ? C58 N28 1.340(5) . ? C59 C60 1.348(6) . ? C59 N27 1.365(5) . ? C60 N28 1.368(5) . ? C61 C66 1.388(5) . ? C61 C62 1.402(5) . ? C61 N14 1.408(4) . ? C62 C63 1.360(5) . ? C63 C64 1.380(5) . ? C63 N16 1.431(5) . ? C64 C65 1.390(5) . ? C64 N18 1.431(4) . ? C65 C66 1.373(5) . ? C66 N20 1.418(5) . ? C67 C68 1.361(5) . ? C67 C72 1.387(5) . ? C67 N22 1.437(5) . ? C68 C69 1.378(5) . ? C69 C70 1.385(5) . ? C69 N24 1.408(5) . ? C70 C71 1.376(5) . ? C70 N26 1.445(5) . ? C71 C72 1.372(5) . ? C72 N28 1.430(5) . ? C73 N30 1.342(5) . ? C73 C74 1.388(6) . ? C74 C75 1.423(7) . ? C75 C76 1.339(7) . ? C75 C78 1.507(6) . ? C76 C77 1.366(6) . ? C77 N30 1.333(5) . ? C78 C79 1.454(7) . ? C79 C82 1.519(6) . ? C80 N29 1.350(6) . ? C80 C81 1.388(6) . ? C81 C82 1.363(7) . ? C82 C83 1.367(7) . ? C83 C84 1.364(6) . ? C84 N29 1.328(6) . ? C85 N31 1.364(7) . ? C85 C86 1.373(8) . ? C86 C87 1.374(8) . ? C87 C88 1.364(8) . ? C87 C90 1.552(8) . ? C88 C89 1.372(7) . ? C89 N31 1.356(6) . ? C90 C91 1.378(7) . ? C91 C92 1.497(7) . ? C92 C93 1.353(8) . ? C92 C95 1.375(7) . ? C93 C94 1.412(7) . ? C94 N32 1.346(5) . ? C95 C96 1.376(6) . ? C96 N32 1.344(6) . ? N1 Pd1 2.056(3) . ? N2 Pd1 2.060(3) . ? N3 Pd2 2.028(5) . ? N4 Pd2 2.056(4) . ? N5 Pd3 2.060(3) . ? N6 Pd3 2.060(3) . ? N7 Pd4 2.044(4) . ? N8 Pd4 2.043(4) . ? N9 Pd5 2.046(4) . ? N10 Pd5 2.004(4) . ? N11 Pd6 2.055(3) . ? N12 Pd6 2.051(3) . ? N13 Pd1 2.019(3) . ? N15 Pd2 2.013(4) . ? N17 Pd6 2.019(3) . ? N19 Pd5 2.021(3) . ? N21 Pd3 2.023(3) . ? N23 Pd4 2.007(3) . ? N25 Pd5 2.023(3) . ? N27 Pd6 2.020(3) . ? N29 Pd4 2.019(3) . ? N30 Pd1 2.007(3) . ? N31 Pd2 2.020(4) . ? N32 Pd3 2.012(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 C4 C3 N1 112.1(4) . . ? C3 C4 N2 111.4(4) . . ? C10 C9 N4 115.7(6) . . ? C9 C10 N3 115.3(6) . . ? N5 C15 C16 109.8(4) . . ? C15 C16 N6 109.7(4) . . ? C22 C21 N8 116.4(5) . . ? C21 C22 N7 115.8(5) . . ? C28 C27 N10 122.8(6) . . ? C27 C28 N9 114.6(7) . . ? C34 C33 N11 112.0(4) . . ? C33 C34 N12 110.2(4) . . ? N13 C37 N14 110.8(3) . . ? C39 C38 N13 109.9(3) . . ? C38 C39 N14 105.3(3) . . ? N15 C40 N16 109.7(4) . . ? C42 C41 N16 106.6(4) . . ? C41 C42 N15 109.4(4) . . ? N17 C43 N18 108.5(4) . . ? C45 C44 N18 106.1(4) . . ? C44 C45 N17 109.4(4) . . ? N19 C46 N20 110.2(3) . . ? C48 C47 N19 108.0(3) . . ? C47 C48 N20 106.1(3) . . ? N23 C49 N24 110.5(3) . . ? C51 C50 N23 109.4(4) . . ? C50 C51 N24 106.0(4) . . ? N21 C52 N22 109.8(3) . . ? C54 C53 N22 105.5(4) . . ? C53 C54 N21 109.2(4) . . ? N25 C55 N26 109.8(3) . . ? C57 C56 N25 109.3(3) . . ? C56 C57 N26 106.0(4) . . ? N27 C58 N28 110.0(4) . . ? C60 C59 N27 109.4(4) . . ? C59 C60 N28 105.6(4) . . ? C66 C61 C62 119.6(3) . . ? C66 C61 N14 121.2(3) . . ? C62 C61 N14 119.1(3) . . ? C63 C62 C61 119.1(3) . . ? C62 C63 C64 121.4(3) . . ? C62 C63 N16 118.4(3) . . ? C64 C63 N16 120.0(3) . . ? C63 C64 C65 119.7(3) . . ? C63 C64 N18 122.1(3) . . ? C65 C64 N18 118.0(3) . . ? C66 C65 C64 119.5(3) . . ? C65 C66 C61 120.6(3) . . ? C65 C66 N20 118.6(3) . . ? C61 C66 N20 120.6(3) . . ? C68 C67 C72 120.7(4) . . ? C68 C67 N22 119.4(3) . . ? C72 C67 N22 119.8(3) . . ? C67 C68 C69 119.6(4) . . ? C68 C69 C70 119.9(4) . . ? C68 C69 N24 119.2(3) . . ? C70 C69 N24 120.9(4) . . ? C71 C70 C69 120.3(4) . . ? C71 C70 N26 119.3(3) . . ? C69 C70 N26 120.4(4) . . ? C70 C71 C72 119.5(4) . . ? C71 C72 C67 119.9(4) . . ? C71 C72 N28 119.2(3) . . ? C67 C72 N28 120.9(3) . . ? N30 C73 C74 121.9(4) . . ? C73 C74 C75 118.6(5) . . ? C76 C75 C74 117.3(4) . . ? C76 C75 C78 120.5(5) . . ? C74 C75 C78 122.2(5) . . ? C75 C76 C77 121.5(5) . . ? N30 C77 C76 122.4(5) . . ? C79 C78 C75 117.8(4) . . ? C78 C79 C82 112.8(4) . . ? N29 C80 C81 120.9(5) . . ? C82 C81 C80 120.1(5) . . ? C83 C82 C81 118.6(4) . . ? C83 C82 C79 118.6(5) . . ? C81 C82 C79 122.8(5) . . ? C84 C83 C82 118.9(5) . . ? N29 C84 C83 123.8(5) . . ? N31 C85 C86 122.0(6) . . ? C85 C86 C87 121.1(6) . . ? C86 C87 C88 116.4(5) . . ? C86 C87 C90 120.3(6) . . ? C88 C87 C90 123.0(6) . . ? C89 C88 C87 121.8(5) . . ? N31 C89 C88 121.8(5) . . ? C91 C90 C87 114.6(5) . . ? C90 C91 C92 115.1(5) . . ? C93 C92 C95 118.3(5) . . ? C93 C92 C91 119.6(6) . . ? C95 C92 C91 122.0(6) . . ? C92 C93 C94 120.1(5) . . ? N32 C94 C93 120.7(5) . . ? C92 C95 C96 120.3(5) . . ? N32 C96 C95 121.8(5) . . ? C1 N1 C2 110.5(4) . . ? C1 N1 C3 107.2(3) . . ? C2 N1 C3 112.0(4) . . ? C1 N1 Pd1 112.9(3) . . ? C2 N1 Pd1 109.9(3) . . ? C3 N1 Pd1 104.2(3) . . ? C6 N2 C4 112.8(4) . . ? C6 N2 C5 107.0(4) . . ? C4 N2 C5 108.9(4) . . ? C6 N2 Pd1 111.1(3) . . ? C4 N2 Pd1 104.4(3) . . ? C5 N2 Pd1 112.7(3) . . ? C11 N3 C12 110.9(6) . . ? C11 N3 C10 109.8(7) . . ? C12 N3 C10 104.9(5) . . ? C11 N3 Pd2 112.5(4) . . ? C12 N3 Pd2 112.6(4) . . ? C10 N3 Pd2 105.7(4) . . ? C9 N4 C8 110.2(4) . . ? C9 N4 C7 109.6(5) . . ? C8 N4 C7 106.6(5) . . ? C9 N4 Pd2 107.5(4) . . ? C8 N4 Pd2 111.5(3) . . ? C7 N4 Pd2 111.4(3) . . ? C14 N5 C15 109.5(4) . . ? C14 N5 C13 109.5(4) . . ? C15 N5 C13 108.4(4) . . ? C14 N5 Pd3 110.5(3) . . ? C15 N5 Pd3 105.4(3) . . ? C13 N5 Pd3 113.4(3) . . ? C17 N6 C18 108.8(4) . . ? C17 N6 C16 109.2(4) . . ? C18 N6 C16 111.0(4) . . ? C17 N6 Pd3 114.3(3) . . ? C18 N6 Pd3 108.6(3) . . ? C16 N6 Pd3 105.0(3) . . ? C22 N7 C23 114.8(6) . . ? C22 N7 C24 108.5(5) . . ? C23 N7 C24 106.2(6) . . ? C22 N7 Pd4 105.2(3) . . ? C23 N7 Pd4 114.0(4) . . ? C24 N7 Pd4 107.8(4) . . ? C19 N8 C20 109.2(4) . . ? C19 N8 C21 107.7(5) . . ? C20 N8 C21 111.6(5) . . ? C19 N8 Pd4 113.7(3) . . ? C20 N8 Pd4 109.6(3) . . ? C21 N8 Pd4 105.0(3) . . ? C30 N9 C28 106.7(5) . . ? C30 N9 C29 109.3(5) . . ? C28 N9 C29 106.4(5) . . ? C30 N9 Pd5 113.8(3) . . ? C28 N9 Pd5 109.9(4) . . ? C29 N9 Pd5 110.4(3) . . ? C25 N10 C27 109.0(5) . . ? C25 N10 C26 104.2(5) . . ? C27 N10 C26 111.0(5) . . ? C25 N10 Pd5 115.6(3) . . ? C27 N10 Pd5 106.4(4) . . ? C26 N10 Pd5 110.7(3) . . ? C32 N11 C31 110.2(4) . . ? C32 N11 C33 110.9(4) . . ? C31 N11 C33 109.2(4) . . ? C32 N11 Pd6 108.1(3) . . ? C31 N11 Pd6 113.3(3) . . ? C33 N11 Pd6 105.1(3) . . ? C35 N12 C34 113.1(4) . . ? C35 N12 C36 108.4(4) . . ? C34 N12 C36 107.6(4) . . ? C35 N12 Pd6 110.2(3) . . ? C34 N12 Pd6 105.4(3) . . ? C36 N12 Pd6 112.1(3) . . ? C37 N13 C38 106.6(3) . . ? C37 N13 Pd1 126.1(3) . . ? C38 N13 Pd1 124.9(3) . . ? C37 N14 C39 107.4(3) . . ? C37 N14 C61 124.9(3) . . ? C39 N14 C61 126.8(3) . . ? C40 N15 C42 105.9(4) . . ? C40 N15 Pd2 126.7(3) . . ? C42 N15 Pd2 126.1(3) . . ? C40 N16 C41 108.4(4) . . ? C40 N16 C63 123.8(3) . . ? C41 N16 C63 127.1(4) . . ? C43 N17 C45 107.1(3) . . ? C43 N17 Pd6 127.5(3) . . ? C45 N17 Pd6 124.6(3) . . ? C43 N18 C44 109.0(3) . . ? C43 N18 C64 124.0(3) . . ? C44 N18 C64 127.0(3) . . ? C46 N19 C47 107.6(3) . . ? C46 N19 Pd5 130.3(3) . . ? C47 N19 Pd5 121.2(2) . . ? C46 N20 C48 108.0(3) . . ? C46 N20 C66 126.3(3) . . ? C48 N20 C66 125.5(3) . . ? C52 N21 C54 107.2(3) . . ? C52 N21 Pd3 125.0(3) . . ? C54 N21 Pd3 126.7(3) . . ? C52 N22 C53 108.3(3) . . ? C52 N22 C67 125.2(3) . . ? C53 N22 C67 126.5(3) . . ? C49 N23 C50 106.9(3) . . ? C49 N23 Pd4 126.1(3) . . ? C50 N23 Pd4 125.7(3) . . ? C49 N24 C51 107.2(3) . . ? C49 N24 C69 124.6(3) . . ? C51 N24 C69 127.9(3) . . ? C55 N25 C56 106.9(3) . . ? C55 N25 Pd5 125.4(3) . . ? C56 N25 Pd5 127.0(2) . . ? C55 N26 C57 107.9(3) . . ? C55 N26 C70 124.9(3) . . ? C57 N26 C70 127.1(3) . . ? C58 N27 C59 106.9(3) . . ? C58 N27 Pd6 126.6(3) . . ? C59 N27 Pd6 125.8(3) . . ? C58 N28 C60 108.1(3) . . ? C58 N28 C72 125.4(3) . . ? C60 N28 C72 126.4(3) . . ? C84 N29 C80 117.6(4) . . ? C84 N29 Pd4 120.9(3) . . ? C80 N29 Pd4 120.7(3) . . ? C77 N30 C73 118.3(4) . . ? C77 N30 Pd1 119.1(3) . . ? C73 N30 Pd1 122.4(3) . . ? C89 N31 C85 116.6(4) . . ? C89 N31 Pd2 120.5(3) . . ? C85 N31 Pd2 121.9(3) . . ? C94 N32 C96 118.6(4) . . ? C94 N32 Pd3 120.5(3) . . ? C96 N32 Pd3 120.5(3) . . ? N30 Pd1 N13 86.38(12) . . ? N30 Pd1 N1 92.55(14) . . ? N13 Pd1 N1 178.27(14) . . ? N30 Pd1 N2 177.89(14) . . ? N13 Pd1 N2 94.30(13) . . ? N1 Pd1 N2 86.72(14) . . ? N15 Pd2 N31 86.29(16) . . ? N15 Pd2 N3 177.41(19) . . ? N31 Pd2 N3 94.24(19) . . ? N15 Pd2 N4 93.63(15) . . ? N31 Pd2 N4 179.13(17) . . ? N3 Pd2 N4 85.81(19) . . ? N32 Pd3 N21 86.14(13) . . ? N32 Pd3 N6 179.72(16) . . ? N21 Pd3 N6 93.74(13) . . ? N32 Pd3 N5 94.38(14) . . ? N21 Pd3 N5 179.47(14) . . ? N6 Pd3 N5 85.74(14) . . ? N23 Pd4 N29 86.36(13) . . ? N23 Pd4 N8 177.68(16) . . ? N29 Pd4 N8 94.14(15) . . ? N23 Pd4 N7 93.19(15) . . ? N29 Pd4 N7 179.23(16) . . ? N8 Pd4 N7 86.33(16) . . ? N10 Pd5 N19 94.56(15) . . ? N10 Pd5 N25 179.41(15) . . ? N19 Pd5 N25 85.96(12) . . ? N10 Pd5 N9 86.20(16) . . ? N19 Pd5 N9 178.00(14) . . ? N25 Pd5 N9 93.29(14) . . ? N27 Pd6 N17 86.42(12) . . ? N27 Pd6 N12 94.01(13) . . ? N17 Pd6 N12 179.09(14) . . ? N27 Pd6 N11 178.50(14) . . ? N17 Pd6 N11 93.72(13) . . ? N12 Pd6 N11 85.84(14) . . ? _refine_diff_density_max 1.235 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.086 _shelxl_version_number 2013-4 _shelx_res_file ; TITL dspd71 in P-1 CELL 0.71073 17.4691 21.0821 21.4283 95.022 91.544 98.679 ZERR 2.00 0.0017 0.0022 0.0022 0.005 0.004 0.005 LATT 1 SFAC C N O PD H UNIT 343 2 2 14 330 MERG 2 OMIT 0.00 50.00 DFIX 1.600 0.020 N10 C26 DFIX 1.600 0.020 N10 C27 DFIX 1.500 0.020 C27 C28 DFIX 1.500 0.020 C28 N9 DFIX 1.500 0.020 C9 C10 EADP C26 C27 EADP C28 C27 FMAP 2 PLAN 50 SIZE 0.050 0.080 0.100 ACTA L.S. 10 WGHT 0.062200 FVAR 0.31975 C1 1 0.437817 0.439172 0.574248 11.00000 0.04064 0.03342 = 0.05016 0.00794 0.00074 -0.00189 AFIX 33 H1A 5 0.395435 0.448760 0.549122 11.00000 -1.50000 H1B 5 0.480285 0.473982 0.575204 11.00000 -1.50000 H1C 5 0.421531 0.433772 0.616140 11.00000 -1.50000 AFIX 0 C2 1 0.526559 0.364476 0.584971 11.00000 0.02405 0.04933 = 0.12923 0.03346 -0.01802 0.00128 AFIX 33 H2A 5 0.542439 0.325681 0.566405 11.00000 -1.50000 H2B 5 0.510293 0.358246 0.626727 11.00000 -1.50000 H2C 5 0.569239 0.399159 0.586493 11.00000 -1.50000 AFIX 0 C3 1 0.484515 0.390640 0.480462 11.00000 0.05721 0.05092 = 0.07713 0.00705 0.03837 -0.00729 AFIX 23 H3A 5 0.451810 0.418701 0.463270 11.00000 -1.20000 H3B 5 0.537781 0.411965 0.480779 11.00000 -1.20000 AFIX 0 C4 1 0.476652 0.331687 0.441324 11.00000 0.05898 0.08874 = 0.05201 0.00535 0.02371 -0.02848 AFIX 23 H4A 5 0.515096 0.306340 0.454507 11.00000 -1.20000 H4B 5 0.486156 0.340873 0.398397 11.00000 -1.20000 AFIX 0 C5 1 0.400821 0.225189 0.419456 11.00000 0.09353 0.05946 = 0.04499 0.01146 0.02232 0.02674 AFIX 33 H5A 5 0.438876 0.208141 0.443454 11.00000 -1.50000 H5B 5 0.414218 0.223650 0.376252 11.00000 -1.50000 H5C 5 0.350846 0.199929 0.422959 11.00000 -1.50000 AFIX 0 C6 1 0.340239 0.317638 0.405623 11.00000 0.07269 0.08681 = 0.03305 0.01278 0.00870 0.01942 AFIX 33 H6A 5 0.336821 0.361462 0.420175 11.00000 -1.50000 H6B 5 0.290828 0.291358 0.408717 11.00000 -1.50000 H6C 5 0.354849 0.315523 0.362711 11.00000 -1.50000 AFIX 0 C7 1 -0.077434 0.323885 0.327294 11.00000 0.05863 0.19589 = 0.04357 0.02267 0.01140 0.02767 AFIX 33 H7A 5 -0.046606 0.361533 0.348530 11.00000 -1.50000 H7B 5 -0.066005 0.320966 0.283659 11.00000 -1.50000 H7C 5 -0.065747 0.286214 0.345402 11.00000 -1.50000 AFIX 0 C8 1 -0.203976 0.270217 0.300005 11.00000 0.09237 0.06980 = 0.03520 0.00777 0.00524 0.01008 AFIX 33 H8A 5 -0.258507 0.271847 0.301749 11.00000 -1.50000 H8B 5 -0.192372 0.232985 0.318961 11.00000 -1.50000 H8C 5 -0.189502 0.267633 0.257061 11.00000 -1.50000 AFIX 0 C9 1 -0.178778 0.386226 0.306109 11.00000 0.16180 0.07299 = 0.05464 0.01280 -0.01358 0.03920 AFIX 23 H9A 5 -0.131297 0.416676 0.305681 11.00000 -1.20000 H9B 5 -0.196608 0.373865 0.262875 11.00000 -1.20000 AFIX 0 C10 1 -0.232466 0.416483 0.335262 11.00000 0.17445 0.17845 = 0.10421 0.09401 0.06936 0.13542 AFIX 23 H10A 5 -0.283423 0.395436 0.319570 11.00000 -1.20000 H10B 5 -0.226211 0.460490 0.324003 11.00000 -1.20000 AFIX 0 C11 1 -0.180039 0.476343 0.433862 11.00000 0.13181 0.06757 = 0.30403 0.02030 -0.04394 0.03649 AFIX 33 H11A 5 -0.127873 0.475589 0.421176 11.00000 -1.50000 H11B 5 -0.181130 0.478478 0.478759 11.00000 -1.50000 H11C 5 -0.198494 0.513385 0.419476 11.00000 -1.50000 AFIX 0 C12 1 -0.310311 0.417958 0.424704 11.00000 0.08991 0.14119 = 0.08033 0.02138 0.00932 0.08638 AFIX 33 H12A 5 -0.341507 0.378579 0.407464 11.00000 -1.50000 H12B 5 -0.329661 0.453895 0.408745 11.00000 -1.50000 H12C 5 -0.312443 0.421357 0.469572 11.00000 -1.50000 AFIX 0 C13 1 -0.377135 0.467915 1.026928 11.00000 0.06358 0.03112 = 0.08879 -0.00351 0.01884 0.00775 AFIX 33 H13A 5 -0.374427 0.464160 0.982098 11.00000 -1.50000 H13B 5 -0.325646 0.475888 1.045665 11.00000 -1.50000 H13C 5 -0.404053 0.503002 1.039904 11.00000 -1.50000 AFIX 0 C14 1 -0.498846 0.395847 1.019534 11.00000 0.04892 0.07208 = 0.06512 -0.00345 -0.00566 0.03364 AFIX 33 H14A 5 -0.497178 0.391237 0.974644 11.00000 -1.50000 H14B 5 -0.524651 0.431646 1.032380 11.00000 -1.50000 H14C 5 -0.526572 0.357182 1.033599 11.00000 -1.50000 AFIX 0 C15 1 -0.421687 0.414047 1.116256 11.00000 0.06517 0.04968 = 0.04320 -0.00855 0.01003 0.02460 AFIX 23 H15A 5 -0.461495 0.439416 1.128976 11.00000 -1.20000 H15B 5 -0.372275 0.436255 1.134210 11.00000 -1.20000 AFIX 0 C16 1 -0.438564 0.349565 1.139556 11.00000 0.06577 0.06102 = 0.04056 0.00457 0.01829 0.03073 AFIX 23 H16A 5 -0.489889 0.328818 1.124477 11.00000 -1.20000 H16B 5 -0.437523 0.353890 1.185024 11.00000 -1.20000 AFIX 0 C17 1 -0.408536 0.242398 1.125752 11.00000 0.08112 0.05192 = 0.03191 0.00973 0.01777 0.02102 AFIX 33 H17A 5 -0.456853 0.228924 1.102499 11.00000 -1.50000 H17B 5 -0.416040 0.237684 1.169420 11.00000 -1.50000 H17C 5 -0.371179 0.216247 1.110785 11.00000 -1.50000 AFIX 0 C18 1 -0.306770 0.329471 1.152786 11.00000 0.06990 0.10947 = 0.03709 -0.01159 -0.01190 0.03371 AFIX 33 H18A 5 -0.287608 0.373715 1.147460 11.00000 -1.50000 H18B 5 -0.269932 0.302874 1.137684 11.00000 -1.50000 H18C 5 -0.314334 0.324709 1.196439 11.00000 -1.50000 AFIX 0 C19 1 0.274305 0.456091 1.162409 11.00000 0.06580 0.05420 = 0.13114 -0.00658 -0.02314 -0.00021 AFIX 33 H19A 5 0.222231 0.464702 1.166976 11.00000 -1.50000 H19B 5 0.287222 0.456625 1.119176 11.00000 -1.50000 H19C 5 0.309409 0.488515 1.187390 11.00000 -1.50000 AFIX 0 C20 1 0.360886 0.379746 1.175753 11.00000 0.02784 0.10378 = 0.05510 -0.02505 -0.00752 0.01049 AFIX 33 H20A 5 0.365083 0.338079 1.189131 11.00000 -1.50000 H20B 5 0.396054 0.412059 1.200808 11.00000 -1.50000 H20C 5 0.373594 0.380577 1.132495 11.00000 -1.50000 AFIX 0 C21 1 0.258627 0.393804 1.249535 11.00000 0.09143 0.13023 = 0.04411 -0.04259 0.01813 -0.04404 AFIX 23 H21A 5 0.305019 0.408755 1.275833 11.00000 -1.20000 H21B 5 0.223765 0.425167 1.256796 11.00000 -1.20000 AFIX 0 C22 1 0.224680 0.337698 1.268359 11.00000 0.06125 0.17391 = 0.01820 -0.00025 -0.00141 -0.02983 AFIX 23 H22A 5 0.198935 0.346728 1.306957 11.00000 -1.20000 H22B 5 0.264839 0.312472 1.277919 11.00000 -1.20000 AFIX 0 C23 1 0.155335 0.229148 1.231528 11.00000 0.26071 0.09936 = 0.04450 0.04135 0.01702 -0.01145 AFIX 33 H23A 5 0.117752 0.207001 1.200465 11.00000 -1.50000 H23B 5 0.136765 0.222612 1.272591 11.00000 -1.50000 H23C 5 0.203329 0.212592 1.226831 11.00000 -1.50000 AFIX 0 C24 1 0.091296 0.320147 1.231599 11.00000 0.03960 0.24240 = 0.05471 0.00629 0.02679 -0.00171 AFIX 33 H24A 5 0.053750 0.295238 1.202080 11.00000 -1.50000 H24B 5 0.095781 0.364873 1.224522 11.00000 -1.50000 H24C 5 0.075032 0.314508 1.273458 11.00000 -1.50000 AFIX 0 C25 1 0.207784 -0.070523 0.699679 11.00000 0.04419 0.05860 = 0.06659 -0.02316 -0.00555 0.00048 AFIX 33 H25A 5 0.161708 -0.091564 0.717109 11.00000 -1.50000 H25B 5 0.234809 -0.102296 0.679064 11.00000 -1.50000 H25C 5 0.193937 -0.042282 0.669907 11.00000 -1.50000 AFIX 0 C26 1 0.323777 -0.000044 0.716796 11.00000 0.14262 0.11098 = 0.15234 -0.04769 0.00893 0.08626 AFIX 33 H26A 5 0.360139 0.025458 0.746852 11.00000 -1.50000 H26B 5 0.304901 0.027371 0.688389 11.00000 -1.50000 H26C 5 0.348916 -0.031583 0.693727 11.00000 -1.50000 AFIX 0 C27 1 0.284528 -0.077819 0.792665 11.00000 0.14262 0.11098 = 0.15234 -0.04769 0.00893 0.08626 AFIX 23 H27A 5 0.259031 -0.120751 0.777632 11.00000 -1.20000 H27B 5 0.339430 -0.077163 0.786462 11.00000 -1.20000 AFIX 0 C28 1 0.275921 -0.071335 0.855276 11.00000 0.14262 0.11098 = 0.15234 -0.04769 0.00893 0.08626 AFIX 23 H28A 5 0.326864 -0.064268 0.876139 11.00000 -1.20000 H28B 5 0.248260 -0.111422 0.867647 11.00000 -1.20000 AFIX 0 C29 1 0.287938 0.024169 0.924414 11.00000 0.14666 0.05637 = 0.08434 0.01884 -0.08222 -0.01025 AFIX 33 H29A 5 0.332979 0.043043 0.904079 11.00000 -1.50000 H29B 5 0.303375 -0.000685 0.956688 11.00000 -1.50000 H29C 5 0.261676 0.057671 0.942680 11.00000 -1.50000 AFIX 0 C30 1 0.166905 -0.047831 0.908363 11.00000 0.08129 0.05711 = 0.04339 0.02628 0.02467 0.02189 AFIX 33 H30A 5 0.132869 -0.075799 0.878367 11.00000 -1.50000 H30B 5 0.140188 -0.014589 0.926554 11.00000 -1.50000 H30C 5 0.182974 -0.072290 0.940732 11.00000 -1.50000 AFIX 0 C31 1 -0.316708 -0.040322 0.580592 11.00000 0.02868 0.07977 = 0.05643 -0.03091 0.00001 0.00713 AFIX 33 H31A 5 -0.290734 -0.065630 0.606951 11.00000 -1.50000 H31B 5 -0.279409 -0.007748 0.565172 11.00000 -1.50000 H31C 5 -0.342879 -0.067680 0.545891 11.00000 -1.50000 AFIX 0 C32 1 -0.412421 0.028969 0.577902 11.00000 0.05492 0.07746 = 0.03968 0.00786 -0.01801 -0.00047 AFIX 33 H32A 5 -0.448496 0.049613 0.602347 11.00000 -1.50000 H32B 5 -0.439790 0.001896 0.543541 11.00000 -1.50000 H32C 5 -0.375030 0.061113 0.561958 11.00000 -1.50000 AFIX 0 C33 1 -0.429910 -0.060611 0.642238 11.00000 0.03645 0.05816 = 0.06133 -0.00942 -0.00377 -0.01370 AFIX 23 H33A 5 -0.469590 -0.077799 0.610097 11.00000 -1.20000 H33B 5 -0.403283 -0.095606 0.652956 11.00000 -1.20000 AFIX 0 C34 1 -0.466009 -0.035987 0.696915 11.00000 0.04644 0.07592 = 0.04839 0.00694 -0.00682 -0.02314 AFIX 23 H34A 5 -0.497873 -0.071144 0.714705 11.00000 -1.20000 H34B 5 -0.499257 -0.005696 0.685152 11.00000 -1.20000 AFIX 0 C35 1 -0.371337 -0.048495 0.779239 11.00000 0.06566 0.08126 = 0.07049 0.04366 -0.02207 -0.00534 AFIX 33 H35A 5 -0.333069 -0.024793 0.808914 11.00000 -1.50000 H35B 5 -0.347142 -0.076543 0.750975 11.00000 -1.50000 H35C 5 -0.410529 -0.073670 0.801125 11.00000 -1.50000 AFIX 0 C36 1 -0.445656 0.039283 0.789357 11.00000 0.06446 0.08478 = 0.07183 -0.00167 0.04462 -0.01507 AFIX 33 H36A 5 -0.469684 0.068856 0.766700 11.00000 -1.50000 H36B 5 -0.407624 0.062961 0.819238 11.00000 -1.50000 H36C 5 -0.484324 0.013204 0.810933 11.00000 -1.50000 AFIX 0 C37 1 0.214218 0.228489 0.533246 11.00000 0.02122 0.03300 = 0.01869 0.00727 0.00174 0.00568 AFIX 43 H37 5 0.191479 0.265227 0.529715 11.00000 -1.20000 AFIX 0 C38 1 0.298608 0.164607 0.539353 11.00000 0.02206 0.03537 = 0.03065 0.00598 0.00464 0.00711 AFIX 43 H38 5 0.346104 0.149799 0.540509 11.00000 -1.20000 AFIX 0 C39 1 0.229386 0.128487 0.546418 11.00000 0.02475 0.02989 = 0.02778 0.00363 0.00603 0.00510 AFIX 43 H39 5 0.219863 0.084970 0.552770 11.00000 -1.20000 AFIX 0 C40 1 -0.087795 0.247557 0.475563 11.00000 0.02199 0.05786 = 0.02170 0.00344 0.00068 0.01228 AFIX 43 H40 5 -0.047016 0.280703 0.486810 11.00000 -1.20000 AFIX 0 C41 1 -0.159596 0.151804 0.464659 11.00000 0.01780 0.06272 = 0.02787 -0.00834 -0.00122 0.00770 AFIX 43 H41 5 -0.176662 0.108161 0.467144 11.00000 -1.20000 AFIX 0 C42 1 -0.196841 0.192344 0.437683 11.00000 0.02208 0.06002 = 0.02889 -0.00465 -0.00230 0.01217 AFIX 43 H42 5 -0.245406 0.181964 0.417347 11.00000 -1.20000 AFIX 0 C43 1 -0.176001 0.086378 0.628674 11.00000 0.02123 0.04075 = 0.02532 -0.00190 -0.00106 0.00124 AFIX 43 H43 5 -0.157895 0.047763 0.633599 11.00000 -1.20000 AFIX 0 C44 1 -0.181142 0.185331 0.605143 11.00000 0.02425 0.03871 = 0.03245 0.00418 0.00637 0.00812 AFIX 43 H44 5 -0.168086 0.226010 0.591283 11.00000 -1.20000 AFIX 0 C45 1 -0.248239 0.161551 0.630053 11.00000 0.02704 0.04203 = 0.02954 -0.00039 0.00762 0.01490 AFIX 43 H45 5 -0.290090 0.183540 0.636481 11.00000 -1.20000 AFIX 0 C46 1 0.127268 0.073925 0.691551 11.00000 0.01969 0.02831 = 0.02514 0.00303 0.00767 0.00151 AFIX 43 H46 5 0.089676 0.037408 0.686276 11.00000 -1.20000 AFIX 0 C47 1 0.227630 0.143032 0.726417 11.00000 0.02374 0.03293 = 0.02165 -0.00018 -0.00137 0.00016 AFIX 43 H47 5 0.272143 0.161764 0.749881 11.00000 -1.20000 AFIX 0 C48 1 0.192381 0.169938 0.680685 11.00000 0.01962 0.03320 = 0.02886 0.00135 0.00452 -0.00283 AFIX 43 H48 5 0.207562 0.210385 0.666893 11.00000 -1.20000 AFIX 0 C49 1 0.072074 0.248632 1.057045 11.00000 0.02348 0.02736 = 0.02631 -0.00190 0.00084 0.00531 AFIX 43 H49 5 0.049831 0.285724 1.054211 11.00000 -1.20000 AFIX 0 C50 1 0.147444 0.182700 1.083247 11.00000 0.04560 0.03566 = 0.04037 0.01842 -0.00132 0.00570 AFIX 43 H50 5 0.187598 0.166536 1.102795 11.00000 -1.20000 AFIX 0 C51 1 0.094563 0.148742 1.041626 11.00000 0.04301 0.02822 = 0.03670 0.00658 -0.00308 0.00495 AFIX 43 H51 5 0.091350 0.105559 1.026897 11.00000 -1.20000 AFIX 0 C52 1 -0.237223 0.253338 0.996196 11.00000 0.03031 0.02576 = 0.03167 -0.00038 0.00754 0.00193 AFIX 43 H52 5 -0.199939 0.289741 1.004758 11.00000 -1.20000 AFIX 0 C53 1 -0.292437 0.153725 0.965972 11.00000 0.02630 0.02687 = 0.03581 0.00260 0.00955 0.00325 AFIX 43 H53 5 -0.300276 0.110538 0.950484 11.00000 -1.20000 AFIX 0 C54 1 -0.346467 0.188975 0.986516 11.00000 0.03191 0.03239 = 0.03141 0.00287 0.00780 0.00200 AFIX 43 H54 5 -0.399180 0.173874 0.987920 11.00000 -1.20000 AFIX 0 C55 1 0.084709 0.091045 0.866850 11.00000 0.02443 0.02747 = 0.02631 -0.00260 0.00382 0.00129 AFIX 43 H55 5 0.047322 0.056297 0.852316 11.00000 -1.20000 AFIX 0 C56 1 0.193058 0.154066 0.885344 11.00000 0.01886 0.03889 = 0.02936 0.00494 0.00279 -0.00095 AFIX 43 H56 5 0.245735 0.169884 0.885565 11.00000 -1.20000 AFIX 0 C57 1 0.139169 0.185409 0.911069 11.00000 0.03117 0.02819 = 0.03281 -0.00246 0.00129 -0.00078 AFIX 43 H57 5 0.146879 0.226375 0.932367 11.00000 -1.20000 AFIX 0 C58 1 -0.221073 0.098528 0.806686 11.00000 0.02858 0.02894 = 0.03018 -0.00323 0.00999 0.00271 AFIX 43 H58 5 -0.198037 0.061460 0.805208 11.00000 -1.20000 AFIX 0 C59 1 -0.294744 0.167642 0.786337 11.00000 0.02556 0.04005 = 0.03082 0.00277 0.00671 0.01005 AFIX 43 H59 5 -0.333003 0.186610 0.767443 11.00000 -1.20000 AFIX 0 C60 1 -0.246152 0.195706 0.834201 11.00000 0.02528 0.02801 = 0.03435 0.00181 0.00485 0.00508 AFIX 43 H60 5 -0.244456 0.236782 0.854455 11.00000 -1.20000 AFIX 0 C61 1 0.096301 0.157921 0.556201 11.00000 0.01438 0.03187 = 0.02200 0.00388 0.00104 -0.00286 C62 1 0.040638 0.173604 0.514221 11.00000 0.03126 0.03829 = 0.01224 0.00565 0.00213 0.00364 AFIX 43 H62 5 0.055286 0.189352 0.476408 11.00000 -1.20000 AFIX 0 C63 1 -0.035058 0.165489 0.529512 11.00000 0.01848 0.04637 = 0.02044 0.00019 -0.00254 0.00645 C64 1 -0.058235 0.141662 0.585116 11.00000 0.01361 0.04005 = 0.02314 0.00227 0.00563 -0.00051 C65 1 -0.003491 0.125172 0.626564 11.00000 0.02076 0.03535 = 0.02336 0.00128 0.00094 0.00299 AFIX 43 H65 5 -0.018792 0.108064 0.663631 11.00000 -1.20000 AFIX 0 C66 1 0.073319 0.134333 0.612364 11.00000 0.01925 0.02998 = 0.02301 0.00454 -0.00191 -0.00019 C67 1 -0.148565 0.180500 0.954725 11.00000 0.02307 0.02922 = 0.02791 -0.00116 0.00479 0.00340 C68 1 -0.088389 0.190996 0.997908 11.00000 0.03718 0.02418 = 0.02250 -0.00430 0.00358 0.00055 AFIX 43 H68 5 -0.096055 0.205727 1.039113 11.00000 -1.20000 AFIX 0 C69 1 -0.016021 0.179678 0.980244 11.00000 0.03100 0.02565 = 0.02872 -0.00352 -0.00183 0.00190 C70 1 -0.005208 0.157091 0.918937 11.00000 0.02381 0.03208 = 0.03011 -0.00333 0.00721 0.00329 C71 1 -0.066431 0.145799 0.875575 11.00000 0.02816 0.03032 = 0.02226 -0.00487 0.00363 0.00300 AFIX 43 H71 5 -0.059578 0.129058 0.834850 11.00000 -1.20000 AFIX 0 C72 1 -0.137617 0.159432 0.892907 11.00000 0.02657 0.02863 = 0.02801 -0.00811 -0.00097 -0.00222 C73 1 0.299266 0.343884 0.653354 11.00000 0.04562 0.02943 = 0.03107 0.00212 0.00429 -0.00506 AFIX 43 H73 5 0.272789 0.366733 0.627031 11.00000 -1.20000 AFIX 0 C74 1 0.281510 0.344703 0.716120 11.00000 0.06184 0.03042 = 0.03125 -0.00563 0.01003 -0.00217 AFIX 43 H74 5 0.243698 0.367725 0.731797 11.00000 -1.20000 AFIX 0 C75 1 0.322357 0.309585 0.756006 11.00000 0.07619 0.03445 = 0.02509 -0.00348 -0.00712 -0.01577 C76 1 0.376501 0.278100 0.730214 11.00000 0.04735 0.04639 = 0.04357 0.01161 -0.01898 -0.01160 AFIX 43 H76 5 0.405061 0.255604 0.755320 11.00000 -1.20000 AFIX 0 C77 1 0.390699 0.278304 0.667842 11.00000 0.03613 0.04512 = 0.02972 0.01228 -0.00906 -0.00437 AFIX 43 H77 5 0.427640 0.254720 0.651493 11.00000 -1.20000 AFIX 0 C78 1 0.306134 0.307107 0.824562 11.00000 0.14933 0.04542 = 0.02513 0.00645 0.01817 0.00013 AFIX 23 H78A 5 0.265479 0.271004 0.828324 11.00000 -1.20000 H78B 5 0.352346 0.297872 0.845853 11.00000 -1.20000 AFIX 0 C79 1 0.283239 0.363841 0.858017 11.00000 0.07485 0.05986 = 0.03795 0.01247 0.01298 0.00666 AFIX 23 H79A 5 0.235596 0.372586 0.838598 11.00000 -1.20000 H79B 5 0.322962 0.400633 0.854296 11.00000 -1.20000 AFIX 0 C80 1 0.293574 0.310369 1.022431 11.00000 0.03258 0.07135 = 0.03579 0.00546 0.00912 0.00808 AFIX 43 H80 5 0.319467 0.283314 1.044397 11.00000 -1.20000 AFIX 0 C81 1 0.311028 0.318997 0.960628 11.00000 0.03967 0.08734 = 0.03114 -0.00731 0.00551 0.00493 AFIX 43 H81 5 0.350122 0.299419 0.942130 11.00000 -1.20000 AFIX 0 C82 1 0.270973 0.356104 0.927022 11.00000 0.05718 0.03539 = 0.03632 0.00802 0.00283 -0.00834 C83 1 0.215061 0.385459 0.955968 11.00000 0.09598 0.04290 = 0.03945 0.01485 0.01442 0.01981 AFIX 43 H83 5 0.186148 0.410474 0.934044 11.00000 -1.20000 AFIX 0 C84 1 0.202375 0.377460 1.017512 11.00000 0.07639 0.04644 = 0.04007 0.01750 0.01477 0.02202 AFIX 43 H84 5 0.165569 0.398991 1.037100 11.00000 -1.20000 AFIX 0 C85 1 -0.166213 0.374169 0.563755 11.00000 0.06458 0.09776 = 0.05881 -0.02354 0.01589 -0.00374 AFIX 43 H85 5 -0.120878 0.399206 0.552921 11.00000 -1.20000 AFIX 0 C86 1 -0.179661 0.368622 0.626032 11.00000 0.09326 0.09296 = 0.04503 -0.02242 0.01118 0.00595 AFIX 43 H86 5 -0.141621 0.386999 0.656201 11.00000 -1.20000 AFIX 0 C87 1 -0.248401 0.336365 0.644483 11.00000 0.08542 0.06667 = 0.05045 0.00301 0.02839 0.03208 C88 1 -0.299469 0.306803 0.597775 11.00000 0.04511 0.07403 = 0.06478 0.02157 0.02463 0.03782 AFIX 43 H88 5 -0.346490 0.284122 0.608328 11.00000 -1.20000 AFIX 0 C89 1 -0.283407 0.309592 0.535679 11.00000 0.03545 0.06680 = 0.05248 -0.00311 -0.00072 0.02501 AFIX 43 H89 5 -0.318839 0.287204 0.505343 11.00000 -1.20000 AFIX 0 C90 1 -0.261647 0.329051 0.715004 11.00000 0.11160 0.09567 = 0.06272 0.00994 0.03928 0.04998 AFIX 23 H90A 5 -0.284726 0.284942 0.719464 11.00000 -1.20000 H90B 5 -0.211715 0.336790 0.737522 11.00000 -1.20000 AFIX 0 C91 1 -0.308294 0.369805 0.742568 11.00000 0.11575 0.10026 = 0.05808 0.03074 0.04113 0.05924 AFIX 23 H91A 5 -0.357547 0.363077 0.719089 11.00000 -1.20000 H91B 5 -0.284289 0.413906 0.739241 11.00000 -1.20000 AFIX 0 C92 1 -0.323613 0.361745 0.810050 11.00000 0.07710 0.06667 = 0.03934 0.01433 0.02197 0.03060 C93 1 -0.268499 0.386664 0.854740 11.00000 0.07748 0.04023 = 0.06038 0.01441 0.02924 0.01250 AFIX 43 H93 5 -0.221521 0.408805 0.843440 11.00000 -1.20000 AFIX 0 C94 1 -0.282155 0.379126 0.918532 11.00000 0.05010 0.03698 = 0.05206 0.01306 0.02094 0.00648 AFIX 43 H94 5 -0.244241 0.396870 0.949035 11.00000 -1.20000 AFIX 0 C95 1 -0.391434 0.327713 0.828324 11.00000 0.06859 0.07062 = 0.04060 0.00454 0.00641 0.01458 AFIX 43 H95 5 -0.429817 0.309562 0.798349 11.00000 -1.20000 AFIX 0 C96 1 -0.402835 0.320360 0.890729 11.00000 0.06263 0.04299 = 0.03588 0.00564 0.00723 0.00852 AFIX 43 H96 5 -0.448771 0.296608 0.902118 11.00000 -1.20000 AFIX 0 N1 2 0.462319 0.380182 0.547438 11.00000 0.03003 0.03437 = 0.05149 0.01245 0.00608 0.00445 N2 2 0.398499 0.294120 0.444140 11.00000 0.03972 0.04125 = 0.03040 0.00992 0.01603 -0.00006 N3 2 -0.229549 0.418027 0.406812 11.00000 0.06599 0.08034 = 0.09707 0.01283 0.01636 0.04283 N4 2 -0.160605 0.328424 0.333910 11.00000 0.04671 0.06961 = 0.04327 0.00890 -0.00929 0.02186 N5 2 -0.419187 0.407328 1.047150 11.00000 0.04019 0.03857 = 0.03878 -0.00707 0.00892 0.01252 N6 2 -0.380439 0.309871 1.117464 11.00000 0.04569 0.04791 = 0.02577 -0.00655 0.00400 0.01784 N7 2 0.167781 0.298162 1.223437 11.00000 0.05298 0.10073 = 0.02051 0.00069 0.00469 -0.00457 N8 2 0.280467 0.392911 1.183209 11.00000 0.03537 0.05671 = 0.04330 -0.01401 0.00245 -0.00075 N9 2 0.234516 -0.018800 0.877249 11.00000 0.04814 0.03735 = 0.03967 0.00389 -0.01599 0.00898 N10 2 0.257910 -0.033078 0.749896 11.00000 0.02782 0.05679 = 0.05400 -0.00493 -0.00202 0.02619 N11 2 -0.373240 -0.009708 0.616797 11.00000 0.02692 0.05437 = 0.03663 -0.00294 -0.00535 0.00203 N12 2 -0.406685 -0.003652 0.743847 11.00000 0.03148 0.04843 = 0.03534 0.01145 0.00298 -0.00243 N13 2 0.288537 0.226540 0.530191 11.00000 0.02379 0.03805 = 0.02044 0.00580 0.00747 0.00214 N14 2 0.175171 0.170199 0.542181 11.00000 0.01624 0.03362 = 0.02153 0.00497 0.00203 0.00139 N15 2 -0.151988 0.253752 0.444308 11.00000 0.02622 0.06468 = 0.02585 -0.00008 -0.00295 0.01809 N16 2 -0.090246 0.186527 0.488590 11.00000 0.02125 0.04800 = 0.02126 0.00308 0.00009 0.00560 N17 2 -0.245230 0.100125 0.644395 11.00000 0.01647 0.03958 = 0.02852 -0.00412 0.00213 0.00125 N18 2 -0.136470 0.138002 0.604350 11.00000 0.01705 0.03683 = 0.02248 0.00117 0.00527 0.00657 N19 2 0.185722 0.082602 0.732161 11.00000 0.01851 0.03561 = 0.02775 0.00607 0.00736 0.00307 N20 2 0.129197 0.125114 0.658597 11.00000 0.02040 0.02955 = 0.02050 0.00502 0.00411 0.00034 N21 2 -0.311195 0.251049 1.005148 11.00000 0.03063 0.02766 = 0.03006 -0.00181 0.00949 0.00536 N22 2 -0.223026 0.195146 0.972734 11.00000 0.02451 0.03400 = 0.02725 -0.00582 0.00547 0.00447 N23 2 0.132941 0.244975 1.092407 11.00000 0.03444 0.03138 = 0.02566 0.00366 0.00270 0.00467 N24 2 0.045942 0.191037 1.025171 11.00000 0.03013 0.02763 = 0.03265 -0.00218 0.00231 0.00954 N25 2 0.158503 0.094706 0.858452 11.00000 0.01880 0.02672 = 0.02623 0.00566 0.00317 0.00422 N26 2 0.070396 0.145138 0.899782 11.00000 0.02449 0.02988 = 0.03008 0.00175 0.00282 -0.00024 N27 2 -0.279023 0.107040 0.769932 11.00000 0.02113 0.03516 = 0.02586 0.00086 0.00341 0.00587 N28 2 -0.199851 0.151106 0.846746 11.00000 0.02738 0.03084 = 0.02501 -0.00504 0.00274 0.00150 N29 2 0.239528 0.340718 1.051080 11.00000 0.04111 0.04022 = 0.02677 0.00141 0.00537 -0.00275 N30 2 0.353556 0.311059 0.629560 11.00000 0.02718 0.03842 = 0.02347 0.00108 -0.00223 -0.00149 N31 2 -0.217301 0.344088 0.517296 11.00000 0.03860 0.07156 = 0.04488 -0.00247 0.01096 0.01787 N32 2 -0.349442 0.346543 0.935666 11.00000 0.03383 0.03088 = 0.04208 0.00168 0.00734 0.00953 PD1 4 0.373852 0.303259 0.537676 11.00000 0.01953 0.03305 = 0.02863 0.00789 0.00646 0.00182 PD2 4 -0.188416 0.336754 0.426579 11.00000 0.03433 0.06401 = 0.03492 0.00195 0.00059 0.02302 PD3 4 -0.364580 0.328629 1.025569 11.00000 0.02816 0.03071 = 0.02921 -0.00207 0.00708 0.00719 PD4 4 0.204618 0.319557 1.136940 11.00000 0.02809 0.03935 = 0.02079 -0.00100 0.00243 0.00073 PD5 4 0.208606 0.030874 0.803626 11.00000 0.02296 0.02896 = 0.02575 0.00288 -0.00083 0.00818 PD6 4 -0.324654 0.048411 0.694145 11.00000 0.01700 0.03593 = 0.02777 -0.00059 0.00103 0.00158 HKLF 4 REM dspd71 in P-1 REM R1 = 0.0445 for 19419 Fo > 4sig(Fo) and 0.0636 for all 26909 data REM 1195 parameters refined using 5 restraints END WGHT 0.0607 0.0000 REM Highest difference peak 1.235, deepest hole -1.192, 1-sigma level 0.086 Q1 1 0.2416 -0.0977 0.7923 11.00000 0.05 1.24 Q2 1 0.3365 -0.0158 0.7434 11.00000 0.05 1.20 Q3 1 0.3224 -0.0531 0.7871 11.00000 0.05 1.14 Q4 1 -0.1617 0.3746 0.4423 11.00000 0.05 0.96 Q5 1 0.3121 0.0112 0.6947 11.00000 0.05 0.83 Q6 1 0.3861 0.3339 0.5949 11.00000 0.05 0.74 Q7 1 0.2249 0.2400 1.2474 11.00000 0.05 0.65 Q8 1 -0.1842 0.4460 0.3662 11.00000 0.05 0.57 Q9 1 -0.3355 0.0449 0.6499 11.00000 0.05 0.57 Q10 1 0.2153 0.3443 1.1905 11.00000 0.05 0.52 Q11 1 0.2160 0.0212 0.7638 11.00000 0.05 0.51 Q12 1 -0.1955 0.3008 0.3644 11.00000 0.05 0.51 Q13 1 0.3009 0.3656 1.2549 11.00000 0.05 0.50 Q14 1 0.2736 0.4328 1.2327 11.00000 0.05 0.50 Q15 1 -0.1788 0.3747 0.4968 11.00000 0.05 0.48 Q16 1 0.5202 0.3603 0.5037 11.00000 0.05 0.47 Q17 1 -0.3186 0.0938 0.6864 11.00000 0.05 0.45 Q18 1 0.3405 0.3586 0.8742 11.00000 0.05 0.45 Q19 1 -0.3206 0.0164 0.6149 11.00000 0.05 0.44 Q20 1 0.3778 -0.0132 0.7814 11.00000 0.05 0.44 Q21 1 -0.1798 0.3102 0.2996 11.00000 0.05 0.43 Q22 1 -0.2279 0.3699 0.3132 11.00000 0.05 0.43 Q23 1 0.2574 0.0324 0.9313 11.00000 0.05 0.43 Q24 1 -0.3443 0.3964 1.0504 11.00000 0.05 0.42 Q25 1 -0.3167 0.0871 0.7555 11.00000 0.05 0.42 Q26 1 -0.4617 0.0266 0.7481 11.00000 0.05 0.41 Q27 1 -0.3456 0.3667 1.0796 11.00000 0.05 0.41 Q28 1 -0.1983 0.4611 0.4179 11.00000 0.05 0.41 Q29 1 0.2988 0.0124 0.8964 11.00000 0.05 0.41 Q30 1 -0.3736 0.2800 0.9515 11.00000 0.05 0.41 Q31 1 0.2525 0.3256 0.8172 11.00000 0.05 0.40 Q32 1 -0.1359 0.4329 0.3364 11.00000 0.05 0.40 Q33 1 0.4206 0.2732 0.5472 11.00000 0.05 0.40 Q34 1 0.2204 0.0525 0.8499 11.00000 0.05 0.39 Q35 1 -0.2333 0.3870 0.6459 11.00000 0.05 0.38 Q36 1 0.1563 0.2597 1.1188 11.00000 0.05 0.38 Q37 1 -0.2604 0.1996 0.7872 11.00000 0.05 0.38 Q38 1 0.3002 0.0697 0.9199 11.00000 0.05 0.38 Q39 1 -0.1868 0.4909 0.4113 11.00000 0.05 0.38 Q40 1 -0.2230 0.2672 0.3081 11.00000 0.05 0.38 Q41 1 -0.0379 0.3106 0.5013 11.00000 0.05 0.38 Q42 1 -0.3620 0.2927 0.9580 11.00000 0.05 0.38 Q43 1 -0.2390 0.3853 0.7292 11.00000 0.05 0.37 Q44 1 -0.4435 0.0858 0.7789 11.00000 0.05 0.37 Q45 1 -0.2971 0.0877 0.7261 11.00000 0.05 0.37 Q46 1 -0.1960 0.3238 0.4359 11.00000 0.05 0.37 Q47 1 -0.1814 0.2640 0.4033 11.00000 0.05 0.37 Q48 1 0.2569 0.0860 0.8226 11.00000 0.05 0.37 Q49 1 0.1636 0.2705 1.1013 11.00000 0.05 0.36 Q50 1 -0.2772 0.1429 0.7612 11.00000 0.05 0.35 ; _shelx_res_checksum 9733 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.005 -0.007 -0.005 3346 1617 ' ' _platon_squeeze_details ; 12(N O3), 42.5(H2O) have been removed from the formula unit by squeeze process. ; _database_code_depnum_ccdc_archive 'CCDC 951436' ####################################################################### # # 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_Complex_2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H148 N32 Pd6, 12(N O3), 41(H2O)' _chemical_formula_sum 'C104 H230 N44 O77 Pd6' _chemical_formula_weight 3967.61 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' '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' 'Pd' 'Pd' -0.9988 1.0072 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 50.0277(19) _cell_length_b 11.5534(5) _cell_length_c 35.1453(14) _cell_angle_alpha 90 _cell_angle_beta 127.435(2) _cell_angle_gamma 90 _cell_volume 16129.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14208 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25 _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'colorless' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.634 _exptl_crystal_F_000 8253.0 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.765 _shelx_estimated_absorpt_T_min 0.915 _shelx_estimated_absorpt_T_max 0.956 _exptl_absorpt_correction_type 'EMPIriCAL' _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; 'The refinement was carried out employing OMIT 0 50 restrain keep the coverage 25. and therby to increase the data completeness.We have used DFIX restraints on C15 C16.' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_reflns_number 123439 _diffrn_reflns_av_unetI/netI 0.0907 _diffrn_reflns_av_R_equivalents 0.1156 _diffrn_reflns_limit_h_min -59 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.025 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 14208 _reflns_number_gt 8341 _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 'Bruker kappa Apex-II ccd' _computing_cell_refinement 'Bruker saint' _computing_data_reduction 'Bruker saint' _computing_structure_solution SHELXL-2013 _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ORTEP-III _computing_publication_material WinGXv1.80.05 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0797P)^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 14208 _refine_ls_number_parameters 640 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1105 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.005 _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 C1 C 0.8182(3) 0.2826(7) 1.2933(4) 0.147(4) Uani 1 1 d . . . . . H1A H 0.8033 0.2951 1.2593 0.220 Uiso 1 1 calc R U . . . H1B H 0.8096 0.2216 1.3016 0.220 Uiso 1 1 calc R U . . . H1C H 0.8401 0.2613 1.3028 0.220 Uiso 1 1 calc R U . . . C2 C 0.8443(2) 0.3798(10) 1.3736(3) 0.145(5) Uani 1 1 d . . . . . H2A H 0.8661 0.3540 1.3843 0.218 Uiso 1 1 calc R U . . . H2B H 0.8349 0.3240 1.3828 0.218 Uiso 1 1 calc R U . . . H2C H 0.8464 0.4530 1.3881 0.218 Uiso 1 1 calc R U . . . C3 C 0.7878(2) 0.4298(8) 1.3048(3) 0.104(3) Uani 1 1 d . . . . . H3A H 0.7751 0.3619 1.3016 0.125 Uiso 1 1 calc R U . . . H3B H 0.7911 0.4778 1.3300 0.125 Uiso 1 1 calc R U . . . C4 C 0.7692(2) 0.4914(8) 1.2619(4) 0.109(3) Uani 1 1 d . . . . . H4A H 0.7493 0.5230 1.2571 0.130 Uiso 1 1 calc R U . . . H4B H 0.7615 0.4382 1.2358 0.130 Uiso 1 1 calc R U . . . C5 C 0.7845(2) 0.6964(9) 1.2778(4) 0.141(4) Uani 1 1 d . . . . . H5A H 0.7971 0.7558 1.2758 0.211 Uiso 1 1 calc R U . . . H5B H 0.7932 0.6867 1.3106 0.211 Uiso 1 1 calc R U . . . H5C H 0.7613 0.7183 1.2589 0.211 Uiso 1 1 calc R U . . . C6 C 0.7726(2) 0.6039(9) 1.2080(3) 0.135(4) Uani 1 1 d . . . . . H6A H 0.7752 0.5343 1.1956 0.202 Uiso 1 1 calc R U . . . H6B H 0.7838 0.6665 1.2050 0.202 Uiso 1 1 calc R U . . . H6C H 0.7491 0.6217 1.1903 0.202 Uiso 1 1 calc R U . . . C7 C 0.7429(2) 0.5070(8) 0.9973(3) 0.113(3) Uani 1 1 d . . . . . H7A H 0.7561 0.5676 1.0200 0.169 Uiso 1 1 calc R U . . . H7B H 0.7520 0.4332 1.0124 0.169 Uiso 1 1 calc R U . . . H7C H 0.7201 0.5127 0.9863 0.169 Uiso 1 1 calc R U . . . C8 C 0.73143(19) 0.6334(8) 0.9370(3) 0.103(3) Uani 1 1 d . . . . . H8A H 0.7457 0.6901 0.9611 0.155 Uiso 1 1 calc R U . . . H8B H 0.7089 0.6418 0.9269 0.155 Uiso 1 1 calc R U . . . H8C H 0.7316 0.6445 0.9101 0.155 Uiso 1 1 calc R U . . . C9 C 0.7227(2) 0.4295(12) 0.9199(5) 0.175(6) Uani 1 1 d . . . . . H9A H 0.7066 0.4029 0.9247 0.210 Uiso 1 1 calc R U . . . H9B H 0.7100 0.4677 0.8890 0.210 Uiso 1 1 calc R U . . . C10 C 0.7372(3) 0.3335(10) 0.9167(5) 0.159(5) Uani 1 1 d . . . . . H10A H 0.7232 0.3081 0.8835 0.190 Uiso 1 1 calc R U . . . H10B H 0.7371 0.2723 0.9355 0.190 Uiso 1 1 calc R U . . . C11 C 0.7718(2) 0.3590(8) 0.8908(3) 0.118(3) Uani 1 1 d . . . . . H11A H 0.7945 0.3694 0.9017 0.177 Uiso 1 1 calc R U . . . H11B H 0.7585 0.4249 0.8721 0.177 Uiso 1 1 calc R U . . . H11C H 0.7624 0.2905 0.8714 0.177 Uiso 1 1 calc R U . . . C12 C 0.7899(2) 0.2372(7) 0.9577(3) 0.124(3) Uani 1 1 d . . . . . H12A H 0.8125 0.2412 0.9677 0.186 Uiso 1 1 calc R U . . . H12B H 0.7784 0.1729 0.9363 0.186 Uiso 1 1 calc R U . . . H12C H 0.7904 0.2270 0.9853 0.186 Uiso 1 1 calc R U . . . C13 C 1.0179(2) 0.9626(6) 1.0679(3) 0.098(3) Uani 1 1 d . . . . . H13A H 1.0345 0.9187 1.0959 0.147 Uiso 1 1 calc R U . . . H13B H 1.0289 1.0129 1.0596 0.147 Uiso 1 1 calc R U . . . H13C H 1.0032 0.9108 1.0417 0.147 Uiso 1 1 calc R U . . . C14 C 1.0230(2) 1.1076(7) 1.1211(3) 0.111(3) Uani 1 1 d . . . . . H14A H 1.0389 1.0592 1.1479 0.166 Uiso 1 1 calc R U . . . H14B H 1.0109 1.1536 1.1289 0.166 Uiso 1 1 calc R U . . . H14C H 1.0347 1.1574 1.1138 0.166 Uiso 1 1 calc R U . . . C15 C 0.9738(3) 1.0987(8) 1.0352(3) 0.122(3) Uani 1 1 d D . . . . H15A H 0.9814 1.1785 1.0417 0.146 Uiso 1 1 calc R U . . . H15B H 0.9746 1.0718 1.0098 0.146 Uiso 1 1 calc R U . . . C16 C 0.9410(3) 1.0984(12) 1.0179(5) 0.204(8) Uani 1 1 d D . . . . H16A H 0.9276 1.0845 0.9836 0.245 Uiso 1 1 calc R U . . . H16B H 0.9357 1.1761 1.0219 0.245 Uiso 1 1 calc R U . . . C17 C 0.9127(3) 1.0883(8) 1.0512(3) 0.135(4) Uani 1 1 d . . . . . H17A H 0.9034 1.0351 1.0615 0.203 Uiso 1 1 calc R U . . . H17B H 0.8949 1.1340 1.0251 0.203 Uiso 1 1 calc R U . . . H17C H 0.9286 1.1382 1.0774 0.203 Uiso 1 1 calc R U . . . C18 C 0.9043(2) 0.9477(8) 0.9957(3) 0.129(4) Uani 1 1 d . . . . . H18A H 0.8958 0.8942 1.0068 0.193 Uiso 1 1 calc R U . . . H18B H 0.9145 0.9056 0.9840 0.193 Uiso 1 1 calc R U . . . H18C H 0.8862 0.9941 0.9703 0.193 Uiso 1 1 calc R U . . . C19 C 0.85782(14) 0.6469(6) 1.2456(2) 0.0559(16) Uani 1 1 d . . . . . H19 H 0.8512 0.5831 1.2256 0.067 Uiso 1 1 calc R U . . . C20 C 0.87942(16) 0.8137(6) 1.2798(2) 0.0627(18) Uani 1 1 d . . . . . H20 H 0.8903 0.8849 1.2883 0.075 Uiso 1 1 calc R U . . . C21 C 0.86560(17) 0.7637(6) 1.2979(2) 0.0660(19) Uani 1 1 d . . . . . H21 H 0.8651 0.7960 1.3216 0.079 Uiso 1 1 calc R U . . . C22 C 0.83170(14) 0.6242(6) 1.0689(2) 0.0540(16) Uani 1 1 d . . . . . H22 H 0.8335 0.5595 1.0860 0.065 Uiso 1 1 calc R U . . . C23 C 0.83950(15) 0.7995(6) 1.0528(2) 0.0589(17) Uani 1 1 d . . . . . H23 H 0.8470 0.8751 1.0557 0.071 Uiso 1 1 calc R U . . . C24 C 0.81754(16) 0.7395(6) 1.0115(2) 0.0585(17) Uani 1 1 d . . . . . H24 H 0.8073 0.7681 0.9808 0.070 Uiso 1 1 calc R U . . . C25 C 0.93505(14) 0.8561(5) 1.13051(19) 0.0439(14) Uani 1 1 d . . . . . H25 H 0.9411 0.9236 1.1484 0.053 Uiso 1 1 calc R U . . . C26 C 0.91454(15) 0.6884(5) 1.1013(2) 0.0572(17) Uani 1 1 d . . . . . H26 H 0.9037 0.6177 1.0948 0.069 Uiso 1 1 calc R U . . . C27 C 0.93007(14) 0.7261(5) 1.0827(2) 0.0502(15) Uani 1 1 d . . . . . H27 H 0.9318 0.6871 1.0612 0.060 Uiso 1 1 calc R U . . . C28 C 0.95148(15) 0.6954(5) 1.3214(2) 0.0561(17) Uani 1 1 d . . . . . H28 H 0.9399 0.6267 1.3158 0.067 Uiso 1 1 calc R U . . . C29 C 0.96701(14) 0.8656(5) 1.3109(2) 0.0468(15) Uani 1 1 d . . . . . H29 H 0.9676 0.9321 1.2966 0.056 Uiso 1 1 calc R U . . . C30 C 0.97905(15) 0.7359(5) 1.3641(2) 0.0505(15) Uani 1 1 d . . . . . H30 H 0.9898 0.6978 1.3933 0.061 Uiso 1 1 calc R U . . . C31 C 0.88562(15) 0.7466(5) 1.2171(2) 0.0483(15) Uani 1 1 d . . . . . C32 C 0.86259(15) 0.7347(5) 1.1679(2) 0.0541(16) Uani 1 1 d . . . . . H32 H 0.8401 0.7208 1.1539 0.065 Uiso 1 1 calc R U . . . C33 C 0.87274(14) 0.7434(5) 1.1400(2) 0.0449(14) Uani 1 1 d . . . . . C34 C 0.90573(14) 0.7661(4) 1.1590(2) 0.0412(14) Uani 1 1 d . . . . . C35 C 0.92920(15) 0.7828(5) 1.2080(2) 0.0504(15) Uani 1 1 d . . . . . H35 H 0.9514 0.8014 1.2212 0.060 Uiso 1 1 calc R U . . . C36 C 0.91911(14) 0.7713(5) 1.2373(2) 0.0480(15) Uani 1 1 d . . . . . C37 C 0.86011(16) 0.3949(5) 1.0362(2) 0.0614(18) Uani 1 1 d . . . . . H37 H 0.8523 0.3577 1.0512 0.074 Uiso 1 1 calc R U . . . C38 C 0.89375(16) 0.3821(5) 1.0547(2) 0.0606(17) Uani 1 1 d . . . . . H38 H 0.9079 0.3347 1.0811 0.073 Uiso 1 1 calc R U . . . C39 C 0.90603(15) 0.4378(5) 1.0345(2) 0.0520(16) Uani 1 1 d . . . . . C40 C 0.88372(15) 0.5074(5) 0.9949(2) 0.0555(17) Uani 1 1 d . . . . . H40 H 0.8912 0.5480 0.9801 0.067 Uiso 1 1 calc R U . . . C41 C 0.85077(15) 0.5159(6) 0.9777(2) 0.0598(17) Uani 1 1 d . . . . . H41 H 0.8363 0.5630 0.9513 0.072 Uiso 1 1 calc R U . . . C42 C 0.94222(15) 0.4326(5) 1.0547(2) 0.0491(15) Uani 1 1 d . . . . . C43 C 1.10434(15) 0.4056(5) 1.1812(2) 0.0563(17) Uani 1 1 d . . . . . H43 H 1.1204 0.3685 1.2100 0.068 Uiso 1 1 calc R U . . . C44 C 1.07168(16) 0.3859(5) 1.1608(2) 0.0575(17) Uani 1 1 d . . . . . H44 H 1.0657 0.3360 1.1754 0.069 Uiso 1 1 calc R U . . . C45 C 1.04625(15) 0.4420(5) 1.1168(2) 0.0518(16) Uani 1 1 d . . . . . C46 C 1.05740(17) 0.5075(6) 1.0969(2) 0.0640(18) Uani 1 1 d . . . . . H46 H 1.0420 0.5403 1.0669 0.077 Uiso 1 1 calc R U . . . C47 C 1.09168(17) 0.5257(6) 1.1211(3) 0.0642(19) Uani 1 1 d . . . . . H47 H 1.0986 0.5754 1.1078 0.077 Uiso 1 1 calc R U . . . C48 C 0.95225(16) 0.4371(5) 1.0264(2) 0.0582(17) Uani 1 1 d . . . . . H48 H 0.9361 0.4410 0.9933 0.070 Uiso 1 1 calc R U . . . C49 C 0.98609(16) 0.4362(5) 1.0462(2) 0.0595(17) Uani 1 1 d . . . . . H49 H 0.9924 0.4390 1.0261 0.071 Uiso 1 1 calc R U . . . C50 C 1.01083(15) 0.4311(5) 1.0955(2) 0.0480(15) Uani 1 1 d . . . . . C51 C 1.00010(15) 0.4267(5) 1.1238(2) 0.0559(16) Uani 1 1 d . . . . . H51 H 1.0161 0.4251 1.1569 0.067 Uiso 1 1 calc R U . . . C52 C 0.96605(16) 0.4247(5) 1.1040(2) 0.0595(17) Uani 1 1 d . . . . . H52 H 0.9594 0.4182 1.1235 0.071 Uiso 1 1 calc R U . . . N1 N 0.82104(14) 0.3928(5) 1.3189(2) 0.0758(17) Uani 1 1 d . . . . . N2 N 0.78780(13) 0.5872(6) 1.2597(2) 0.0762(18) Uani 1 1 d . . . . . N3 N 0.74376(13) 0.5183(6) 0.9565(2) 0.0737(17) Uani 1 1 d . . . . . N4 N 0.77162(14) 0.3471(6) 0.9325(2) 0.0795(18) Uani 1 1 d . . . . . N5 N 0.99822(14) 1.0320(4) 1.07772(19) 0.0591(14) Uani 1 1 d . . . . . N6 N 0.92967(13) 1.0234(4) 1.03559(18) 0.0572(14) Uani 1 1 d . . . . . N7 N 1.11507(14) 0.4740(4) 1.16298(19) 0.0538(13) Uani 1 1 d . . . . . N8 N 0.83873(12) 0.4598(4) 0.99721(19) 0.0556(14) Uani 1 1 d . . . . . N9 N 0.85232(12) 0.6593(5) 1.27714(18) 0.0578(14) Uani 1 1 d . . . . . N10 N 0.87431(11) 0.7385(4) 1.24601(17) 0.0483(12) Uani 1 1 d . . . . . N11 N 0.81275(11) 0.6298(5) 1.02210(17) 0.0536(13) Uani 1 1 d . . . . . N12 N 0.84828(11) 0.7248(4) 1.08905(17) 0.0464(12) Uani 1 1 d . . . . . N13 N 0.94274(11) 0.8337(4) 1.10221(15) 0.0391(11) Uani 1 1 d . . . . . N14 N 0.91764(11) 0.7719(4) 1.13093(15) 0.0418(11) Uani 1 1 d . . . . . N15 N 0.98846(11) 0.8394(4) 1.35795(16) 0.0403(11) Uani 1 1 d . . . . . N16 N 0.94445(11) 0.7784(4) 1.28824(16) 0.0441(12) Uani 1 1 d . . . . . Pd1 Pd 0.83677(2) 0.52898(5) 1.29856(2) 0.05596(16) Uani 1 1 d . . . . . Pd2 Pd 0.79177(2) 0.49124(4) 0.97710(2) 0.05584(17) Uani 1 1 d . . . . . Pd3 Pd 0.97082(2) 0.93138(4) 1.09022(2) 0.04113(14) 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 C1 0.218(12) 0.054(6) 0.182(11) -0.027(6) 0.129(10) -0.027(6) C2 0.089(6) 0.239(12) 0.093(7) 0.080(7) 0.047(6) -0.024(7) C3 0.081(6) 0.122(7) 0.133(8) 0.038(6) 0.077(6) -0.002(5) C4 0.069(6) 0.129(8) 0.134(8) 0.031(7) 0.065(6) 0.009(6) C5 0.118(8) 0.156(10) 0.166(10) -0.023(8) 0.096(8) 0.035(7) C6 0.093(7) 0.218(12) 0.064(6) 0.057(7) 0.033(5) 0.033(7) C7 0.082(6) 0.170(9) 0.119(7) 0.045(7) 0.077(6) 0.039(6) C8 0.073(6) 0.131(8) 0.114(7) 0.043(6) 0.061(5) 0.046(5) C9 0.050(6) 0.223(14) 0.213(13) -0.110(11) 0.059(7) -0.064(8) C10 0.116(9) 0.149(10) 0.250(14) -0.106(10) 0.131(10) -0.074(8) C11 0.152(9) 0.113(7) 0.082(6) -0.035(5) 0.066(6) -0.039(6) C12 0.161(9) 0.053(5) 0.141(8) -0.015(5) 0.083(8) -0.009(6) C13 0.157(8) 0.072(5) 0.154(8) 0.005(5) 0.141(7) -0.012(5) C14 0.166(9) 0.073(6) 0.114(7) -0.030(5) 0.096(7) -0.058(6) C15 0.136(9) 0.133(8) 0.107(7) 0.072(6) 0.080(7) 0.011(7) C16 0.119(10) 0.240(15) 0.210(14) 0.180(12) 0.077(10) 0.040(10) C17 0.182(10) 0.105(7) 0.134(8) 0.032(6) 0.103(8) 0.102(7) C18 0.100(7) 0.130(8) 0.066(6) 0.002(6) 0.004(5) 0.018(6) C19 0.055(4) 0.069(4) 0.050(4) -0.003(3) 0.035(4) -0.011(3) C20 0.072(5) 0.068(5) 0.072(5) -0.008(4) 0.056(4) -0.010(4) C21 0.076(5) 0.079(5) 0.066(5) -0.003(4) 0.055(4) 0.002(4) C22 0.043(4) 0.072(5) 0.047(4) -0.002(3) 0.028(3) -0.003(3) C23 0.060(5) 0.060(4) 0.062(4) 0.013(4) 0.040(4) 0.010(3) C24 0.059(4) 0.063(5) 0.050(4) 0.010(4) 0.031(4) 0.008(4) C25 0.054(4) 0.045(4) 0.039(3) 0.003(3) 0.031(3) -0.004(3) C26 0.071(5) 0.041(4) 0.086(5) -0.010(3) 0.061(4) -0.012(3) C27 0.059(4) 0.048(4) 0.059(4) -0.008(3) 0.043(4) -0.006(3) C28 0.062(4) 0.048(4) 0.061(4) 0.009(3) 0.039(4) -0.009(3) C29 0.054(4) 0.049(4) 0.055(4) 0.002(3) 0.042(4) -0.001(3) C30 0.052(4) 0.059(4) 0.034(3) 0.004(3) 0.023(3) -0.001(3) C31 0.049(4) 0.057(4) 0.047(4) 0.003(3) 0.033(3) -0.010(3) C32 0.049(4) 0.064(4) 0.059(4) 0.003(3) 0.038(4) -0.013(3) C33 0.043(4) 0.051(4) 0.047(4) 0.006(3) 0.031(3) -0.003(3) C34 0.052(4) 0.042(3) 0.041(3) 0.001(3) 0.035(3) -0.011(3) C35 0.052(4) 0.049(4) 0.064(4) 0.003(3) 0.043(4) -0.007(3) C36 0.044(4) 0.057(4) 0.051(4) 0.009(3) 0.033(3) -0.002(3) C37 0.054(4) 0.052(4) 0.077(5) 0.007(4) 0.040(4) 0.006(3) C38 0.051(4) 0.057(4) 0.071(5) 0.003(4) 0.035(4) 0.001(3) C39 0.056(4) 0.038(3) 0.064(4) -0.002(3) 0.037(4) -0.002(3) C40 0.057(4) 0.055(4) 0.075(5) -0.008(4) 0.051(4) -0.004(3) C41 0.049(4) 0.075(5) 0.057(4) 0.011(4) 0.032(4) 0.003(3) C42 0.049(4) 0.037(3) 0.057(4) -0.004(3) 0.029(4) -0.002(3) C43 0.041(4) 0.053(4) 0.059(4) 0.001(3) 0.022(4) 0.006(3) C44 0.056(4) 0.050(4) 0.075(5) 0.005(3) 0.044(4) 0.006(3) C45 0.048(4) 0.040(3) 0.081(5) -0.012(3) 0.046(4) -0.003(3) C46 0.060(5) 0.075(5) 0.060(4) 0.011(4) 0.038(4) 0.007(4) C47 0.059(5) 0.086(5) 0.069(5) -0.015(4) 0.051(4) -0.015(4) C48 0.056(4) 0.063(4) 0.044(4) 0.003(3) 0.025(3) 0.000(3) C49 0.056(4) 0.060(4) 0.076(5) 0.005(4) 0.047(4) 0.000(3) C50 0.052(4) 0.034(3) 0.059(4) -0.004(3) 0.034(4) -0.003(3) C51 0.045(4) 0.058(4) 0.063(4) 0.003(3) 0.032(3) 0.002(3) C52 0.065(5) 0.054(4) 0.068(5) -0.012(4) 0.045(4) -0.003(3) N1 0.055(4) 0.096(5) 0.090(5) 0.024(4) 0.051(4) 0.003(3) N2 0.053(4) 0.113(5) 0.068(4) 0.018(4) 0.040(3) 0.009(4) N3 0.043(3) 0.096(5) 0.077(4) 0.003(4) 0.034(3) -0.009(3) N4 0.055(4) 0.098(5) 0.089(5) -0.024(4) 0.045(4) -0.012(3) N5 0.088(4) 0.049(3) 0.065(4) -0.008(3) 0.059(3) -0.012(3) N6 0.073(4) 0.046(3) 0.058(3) 0.019(3) 0.043(3) 0.021(3) N7 0.069(4) 0.047(3) 0.064(4) -0.003(3) 0.051(3) -0.010(3) N8 0.045(3) 0.059(3) 0.070(4) -0.009(3) 0.038(3) -0.007(3) N9 0.054(3) 0.083(4) 0.056(3) -0.002(3) 0.044(3) -0.004(3) N10 0.044(3) 0.061(3) 0.051(3) 0.001(3) 0.035(3) -0.008(2) N11 0.041(3) 0.071(4) 0.043(3) -0.001(3) 0.023(3) 0.002(3) N12 0.041(3) 0.054(3) 0.048(3) 0.004(3) 0.029(3) -0.006(2) N13 0.051(3) 0.034(3) 0.042(3) 0.003(2) 0.033(3) 0.002(2) N14 0.044(3) 0.049(3) 0.038(3) -0.001(2) 0.028(2) -0.007(2) N15 0.044(3) 0.041(3) 0.038(3) 0.000(2) 0.027(2) -0.005(2) N16 0.050(3) 0.045(3) 0.042(3) 0.001(2) 0.030(3) -0.007(2) Pd1 0.0440(3) 0.0758(4) 0.0561(3) 0.0074(3) 0.0346(3) -0.0011(2) Pd2 0.0416(3) 0.0680(4) 0.0579(3) -0.0048(3) 0.0302(3) -0.0048(2) Pd3 0.0546(3) 0.0360(2) 0.0444(3) 0.0041(2) 0.0361(2) -0.0003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.516(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.535(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.394(11) . ? C3 N1 1.481(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.481(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N2 1.467(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.493(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N3 1.463(9) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N3 1.451(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.366(12) . ? C9 N3 1.473(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.462(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.476(9) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.500(10) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N5 1.466(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N5 1.524(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.359(10) . ? C15 N5 1.448(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N6 1.375(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N6 1.469(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N6 1.475(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N9 1.301(7) . ? C19 N10 1.337(7) . ? C19 H19 0.9300 . ? C20 C21 1.322(8) . ? C20 N10 1.364(7) . ? C20 H20 0.9300 . ? C21 N9 1.357(8) . ? C21 H21 0.9300 . ? C22 N11 1.308(7) . ? C22 N12 1.351(7) . ? C22 H22 0.9300 . ? C23 C24 1.361(8) . ? C23 N12 1.373(7) . ? C23 H23 0.9300 . ? C24 N11 1.382(7) . ? C24 H24 0.9300 . ? C25 N13 1.292(6) . ? C25 N14 1.312(6) . ? C25 H25 0.9300 . ? C26 C27 1.354(8) . ? C26 N14 1.358(7) . ? C26 H26 0.9300 . ? C27 N13 1.374(7) . ? C27 H27 0.9300 . ? C28 C30 1.363(8) . ? C28 N16 1.380(7) . ? C28 H28 0.9300 . ? C29 N15 1.348(7) . ? C29 N16 1.353(7) . ? C29 H29 0.9300 . ? C30 N15 1.351(7) . ? C30 H30 0.9300 . ? C31 C32 1.385(8) . ? C31 C36 1.395(7) . ? C31 N10 1.434(7) . ? C32 C33 1.354(8) . ? C32 H32 0.9300 . ? C33 C34 1.378(7) . ? C33 N12 1.444(7) . ? C34 C35 1.386(7) . ? C34 N14 1.432(6) . ? C35 C36 1.403(7) . ? C35 H35 0.9300 . ? C36 N16 1.435(7) . ? C37 N8 1.342(8) . ? C37 C38 1.396(8) . ? C37 H37 0.9300 . ? C38 C39 1.349(8) . ? C38 H38 0.9300 . ? C39 C40 1.395(8) . ? C39 C42 1.491(8) . ? C40 C41 1.372(8) . ? C40 H40 0.9300 . ? C41 N8 1.325(7) . ? C41 H41 0.9300 . ? C42 C48 1.359(8) . ? C42 C52 1.385(8) . ? C43 N7 1.318(8) . ? C43 C44 1.346(8) . ? C43 H43 0.9300 . ? C44 C45 1.428(8) . ? C44 H44 0.9300 . ? C45 C46 1.359(8) . ? C45 C50 1.450(8) . ? C46 C47 1.392(8) . ? C46 H46 0.9300 . ? C47 N7 1.341(8) . ? C47 H47 0.9300 . ? C48 C49 1.386(8) . ? C48 H48 0.9300 . ? C49 C50 1.391(8) . ? C49 H49 0.9300 . ? C50 C51 1.387(8) . ? C51 C52 1.395(8) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? N1 Pd1 2.071(5) . ? N2 Pd1 2.062(5) . ? N3 Pd2 2.069(5) . ? N4 Pd2 2.080(6) . ? N5 Pd3 2.039(5) . ? N6 Pd3 2.061(5) . ? N7 Pd1 2.019(5) 2_757 ? N8 Pd2 2.033(5) . ? N9 Pd1 2.037(5) . ? N11 Pd2 2.037(5) . ? N13 Pd3 2.036(4) . ? N15 Pd3 2.021(4) 2_757 ? Pd1 N7 2.019(5) 2_757 ? Pd3 N15 2.021(4) 2_757 ? 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 N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 112.7(7) . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N1 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 N2 114.3(7) . . ? C3 C4 H4A 108.7 . . ? N2 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? N2 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N3 120.4(9) . . ? C10 C9 H9A 107.2 . . ? N3 C9 H9A 107.2 . . ? C10 C9 H9B 107.2 . . ? N3 C9 H9B 107.2 . . ? H9A C9 H9B 106.9 . . ? C9 C10 N4 116.3(8) . . ? C9 C10 H10A 108.2 . . ? N4 C10 H10A 108.2 . . ? C9 C10 H10B 108.2 . . ? N4 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 H13A 109.5 . . ? N5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N5 119.5(7) . . ? C16 C15 H15A 107.4 . . ? N5 C15 H15A 107.4 . . ? C16 C15 H15B 107.4 . . ? N5 C15 H15B 107.4 . . ? H15A C15 H15B 107.0 . . ? C15 C16 N6 121.1(8) . . ? C15 C16 H16A 107.1 . . ? N6 C16 H16A 107.1 . . ? C15 C16 H16B 107.1 . . ? N6 C16 H16B 107.1 . . ? H16A C16 H16B 106.8 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N9 C19 N10 110.7(6) . . ? N9 C19 H19 124.7 . . ? N10 C19 H19 124.7 . . ? C21 C20 N10 105.3(6) . . ? C21 C20 H20 127.3 . . ? N10 C20 H20 127.3 . . ? C20 C21 N9 111.0(6) . . ? C20 C21 H21 124.5 . . ? N9 C21 H21 124.5 . . ? N11 C22 N12 111.2(6) . . ? N11 C22 H22 124.4 . . ? N12 C22 H22 124.4 . . ? C24 C23 N12 105.3(6) . . ? C24 C23 H23 127.3 . . ? N12 C23 H23 127.3 . . ? C23 C24 N11 109.9(6) . . ? C23 C24 H24 125.0 . . ? N11 C24 H24 125.0 . . ? N13 C25 N14 111.8(5) . . ? N13 C25 H25 124.1 . . ? N14 C25 H25 124.1 . . ? C27 C26 N14 108.1(5) . . ? C27 C26 H26 126.0 . . ? N14 C26 H26 126.0 . . ? C26 C27 N13 106.0(5) . . ? C26 C27 H27 127.0 . . ? N13 C27 H27 127.0 . . ? C30 C28 N16 105.0(5) . . ? C30 C28 H28 127.5 . . ? N16 C28 H28 127.5 . . ? N15 C29 N16 108.2(5) . . ? N15 C29 H29 125.9 . . ? N16 C29 H29 125.9 . . ? N15 C30 C28 110.2(5) . . ? N15 C30 H30 124.9 . . ? C28 C30 H30 124.9 . . ? C32 C31 C36 119.0(5) . . ? C32 C31 N10 119.5(5) . . ? C36 C31 N10 121.4(5) . . ? C33 C32 C31 120.3(6) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 121.9(6) . . ? C32 C33 N12 118.6(5) . . ? C34 C33 N12 119.5(5) . . ? C35 C34 C33 119.3(5) . . ? C35 C34 N14 117.1(5) . . ? C33 C34 N14 123.5(5) . . ? C34 C35 C36 119.2(5) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C31 C36 C35 120.2(6) . . ? C31 C36 N16 121.6(5) . . ? C35 C36 N16 118.1(5) . . ? N8 C37 C38 121.5(6) . . ? N8 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C39 C38 C37 120.7(6) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 117.2(6) . . ? C38 C39 C42 122.7(6) . . ? C40 C39 C42 120.0(6) . . ? C41 C40 C39 119.9(6) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? N8 C41 C40 122.7(6) . . ? N8 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C48 C42 C52 119.8(6) . . ? C48 C42 C39 122.2(6) . . ? C52 C42 C39 118.0(6) . . ? N7 C43 C44 124.4(6) . . ? N7 C43 H43 117.8 . . ? C44 C43 H43 117.8 . . ? C43 C44 C45 119.5(6) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 115.8(6) . . ? C46 C45 C50 122.5(6) . . ? C44 C45 C50 121.6(6) . . ? C45 C46 C47 120.6(6) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? N7 C47 C46 122.1(6) . . ? N7 C47 H47 118.9 . . ? C46 C47 H47 118.9 . . ? C42 C48 C49 121.0(6) . . ? C42 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C48 C49 C50 121.0(6) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C51 C50 C49 117.1(6) . . ? C51 C50 C45 121.1(6) . . ? C49 C50 C45 121.5(6) . . ? C50 C51 C52 122.0(6) . . ? C50 C51 H51 119.0 . . ? C52 C51 H51 119.0 . . ? C42 C52 C51 119.0(6) . . ? C42 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? C3 N1 C2 106.7(7) . . ? C3 N1 C1 111.3(7) . . ? C2 N1 C1 112.8(7) . . ? C3 N1 Pd1 104.5(4) . . ? C2 N1 Pd1 110.5(5) . . ? C1 N1 Pd1 110.5(5) . . ? C5 N2 C6 108.0(7) . . ? C5 N2 C4 112.3(7) . . ? C6 N2 C4 106.9(7) . . ? C5 N2 Pd1 113.2(5) . . ? C6 N2 Pd1 111.7(5) . . ? C4 N2 Pd1 104.7(5) . . ? C7 N3 C8 106.8(6) . . ? C7 N3 C9 111.3(8) . . ? C8 N3 C9 110.6(8) . . ? C7 N3 Pd2 111.2(4) . . ? C8 N3 Pd2 111.9(4) . . ? C9 N3 Pd2 105.1(5) . . ? C10 N4 C11 110.4(8) . . ? C10 N4 C12 106.6(8) . . ? C11 N4 C12 107.3(7) . . ? C10 N4 Pd2 106.9(5) . . ? C11 N4 Pd2 112.5(5) . . ? C12 N4 Pd2 113.0(5) . . ? C15 N5 C13 108.3(6) . . ? C15 N5 C14 113.0(6) . . ? C13 N5 C14 107.2(6) . . ? C15 N5 Pd3 105.6(5) . . ? C13 N5 Pd3 112.0(4) . . ? C14 N5 Pd3 110.8(4) . . ? C16 N6 C17 109.9(8) . . ? C16 N6 C18 107.2(8) . . ? C17 N6 C18 107.4(7) . . ? C16 N6 Pd3 107.1(5) . . ? C17 N6 Pd3 113.1(5) . . ? C18 N6 Pd3 112.0(4) . . ? C43 N7 C47 117.3(6) . . ? C43 N7 Pd1 122.4(5) . 2_757 ? C47 N7 Pd1 119.0(4) . 2_757 ? C41 N8 C37 118.1(5) . . ? C41 N8 Pd2 121.7(5) . . ? C37 N8 Pd2 119.4(4) . . ? C19 N9 C21 105.5(5) . . ? C19 N9 Pd1 124.0(5) . . ? C21 N9 Pd1 129.2(4) . . ? C19 N10 C20 107.5(5) . . ? C19 N10 C31 123.5(5) . . ? C20 N10 C31 128.9(5) . . ? C22 N11 C24 105.7(5) . . ? C22 N11 Pd2 125.1(5) . . ? C24 N11 Pd2 127.2(4) . . ? C22 N12 C23 107.8(5) . . ? C22 N12 C33 124.5(5) . . ? C23 N12 C33 127.6(5) . . ? C25 N13 C27 107.6(5) . . ? C25 N13 Pd3 127.9(4) . . ? C27 N13 Pd3 124.4(4) . . ? C25 N14 C26 106.5(5) . . ? C25 N14 C34 126.8(5) . . ? C26 N14 C34 126.6(5) . . ? C29 N15 C30 107.5(5) . . ? C29 N15 Pd3 127.0(4) . 2_757 ? C30 N15 Pd3 125.4(4) . 2_757 ? C29 N16 C28 109.1(5) . . ? C29 N16 C36 124.4(5) . . ? C28 N16 C36 126.3(5) . . ? N7 Pd1 N9 84.9(2) 2_757 . ? N7 Pd1 N2 179.3(3) 2_757 . ? N9 Pd1 N2 94.6(2) . . ? N7 Pd1 N1 94.5(2) 2_757 . ? N9 Pd1 N1 178.1(2) . . ? N2 Pd1 N1 85.9(2) . . ? N8 Pd2 N11 85.96(19) . . ? N8 Pd2 N3 178.4(2) . . ? N11 Pd2 N3 95.3(2) . . ? N8 Pd2 N4 92.7(2) . . ? N11 Pd2 N4 178.4(2) . . ? N3 Pd2 N4 86.0(2) . . ? N15 Pd3 N13 88.08(17) 2_757 . ? N15 Pd3 N5 93.0(2) 2_757 . ? N13 Pd3 N5 178.76(19) . . ? N15 Pd3 N6 177.83(19) 2_757 . ? N13 Pd3 N6 93.13(19) . . ? N5 Pd3 N6 85.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 N2 -49.9(12) . . . . ? N3 C9 C10 N4 -28(2) . . . . ? N5 C15 C16 N6 -9(2) . . . . ? N10 C20 C21 N9 0.7(8) . . . . ? N12 C23 C24 N11 0.1(7) . . . . ? N14 C26 C27 N13 0.4(7) . . . . ? N16 C28 C30 N15 0.7(7) . . . . ? C36 C31 C32 C33 2.1(9) . . . . ? N10 C31 C32 C33 179.3(5) . . . . ? C31 C32 C33 C34 -1.2(9) . . . . ? C31 C32 C33 N12 176.9(5) . . . . ? C32 C33 C34 C35 -1.2(9) . . . . ? N12 C33 C34 C35 -179.3(5) . . . . ? C32 C33 C34 N14 177.7(5) . . . . ? N12 C33 C34 N14 -0.4(8) . . . . ? C33 C34 C35 C36 2.7(8) . . . . ? N14 C34 C35 C36 -176.3(5) . . . . ? C32 C31 C36 C35 -0.6(9) . . . . ? N10 C31 C36 C35 -177.7(5) . . . . ? C32 C31 C36 N16 -176.6(5) . . . . ? N10 C31 C36 N16 6.3(9) . . . . ? C34 C35 C36 C31 -1.8(9) . . . . ? C34 C35 C36 N16 174.3(5) . . . . ? N8 C37 C38 C39 2.0(10) . . . . ? C37 C38 C39 C40 -0.2(9) . . . . ? C37 C38 C39 C42 176.2(6) . . . . ? C38 C39 C40 C41 -0.7(9) . . . . ? C42 C39 C40 C41 -177.2(6) . . . . ? C39 C40 C41 N8 -0.3(10) . . . . ? C38 C39 C42 C48 147.7(6) . . . . ? C40 C39 C42 C48 -36.0(8) . . . . ? C38 C39 C42 C52 -33.3(9) . . . . ? C40 C39 C42 C52 143.0(6) . . . . ? N7 C43 C44 C45 -0.6(10) . . . . ? C43 C44 C45 C46 3.9(9) . . . . ? C43 C44 C45 C50 -174.9(6) . . . . ? C44 C45 C46 C47 -5.8(9) . . . . ? C50 C45 C46 C47 173.0(6) . . . . ? C45 C46 C47 N7 4.7(10) . . . . ? C52 C42 C48 C49 -1.2(9) . . . . ? C39 C42 C48 C49 177.7(6) . . . . ? C42 C48 C49 C50 -0.3(10) . . . . ? C48 C49 C50 C51 0.2(9) . . . . ? C48 C49 C50 C45 -173.6(5) . . . . ? C46 C45 C50 C51 -142.1(6) . . . . ? C44 C45 C50 C51 36.7(8) . . . . ? C46 C45 C50 C49 31.4(9) . . . . ? C44 C45 C50 C49 -149.8(6) . . . . ? C49 C50 C51 C52 1.5(9) . . . . ? C45 C50 C51 C52 175.3(5) . . . . ? C48 C42 C52 C51 2.8(9) . . . . ? C39 C42 C52 C51 -176.2(5) . . . . ? C50 C51 C52 C42 -3.0(9) . . . . ? C4 C3 N1 C2 154.0(9) . . . . ? C4 C3 N1 C1 -82.4(9) . . . . ? C4 C3 N1 Pd1 36.9(9) . . . . ? C3 C4 N2 C5 -89.4(10) . . . . ? C3 C4 N2 C6 152.4(9) . . . . ? C3 C4 N2 Pd1 33.8(9) . . . . ? C10 C9 N3 C7 -101.2(13) . . . . ? C10 C9 N3 C8 140.3(13) . . . . ? C10 C9 N3 Pd2 19.3(15) . . . . ? C9 C10 N4 C11 -102.0(13) . . . . ? C9 C10 N4 C12 141.7(12) . . . . ? C9 C10 N4 Pd2 20.6(15) . . . . ? C16 C15 N5 C13 130.8(12) . . . . ? C16 C15 N5 C14 -110.7(13) . . . . ? C16 C15 N5 Pd3 10.6(14) . . . . ? C15 C16 N6 C17 125.8(14) . . . . ? C15 C16 N6 C18 -117.8(14) . . . . ? C15 C16 N6 Pd3 2.6(17) . . . . ? C44 C43 N7 C47 -0.9(9) . . . . ? C44 C43 N7 Pd1 165.7(5) . . . 2_757 ? C46 C47 N7 C43 -1.0(9) . . . . ? C46 C47 N7 Pd1 -168.2(5) . . . 2_757 ? C40 C41 N8 C37 2.0(9) . . . . ? C40 C41 N8 Pd2 171.3(5) . . . . ? C38 C37 N8 C41 -2.8(9) . . . . ? C38 C37 N8 Pd2 -172.4(5) . . . . ? N10 C19 N9 C21 0.7(7) . . . . ? N10 C19 N9 Pd1 -167.0(4) . . . . ? C20 C21 N9 C19 -0.9(8) . . . . ? C20 C21 N9 Pd1 165.9(5) . . . . ? N9 C19 N10 C20 -0.2(7) . . . . ? N9 C19 N10 C31 176.3(5) . . . . ? C21 C20 N10 C19 -0.3(7) . . . . ? C21 C20 N10 C31 -176.5(6) . . . . ? C32 C31 N10 C19 56.5(8) . . . . ? C36 C31 N10 C19 -126.4(6) . . . . ? C32 C31 N10 C20 -127.8(7) . . . . ? C36 C31 N10 C20 49.3(9) . . . . ? N12 C22 N11 C24 0.4(7) . . . . ? N12 C22 N11 Pd2 165.2(4) . . . . ? C23 C24 N11 C22 -0.3(7) . . . . ? C23 C24 N11 Pd2 -164.7(4) . . . . ? N11 C22 N12 C23 -0.3(7) . . . . ? N11 C22 N12 C33 -175.9(5) . . . . ? C24 C23 N12 C22 0.1(6) . . . . ? C24 C23 N12 C33 175.5(5) . . . . ? C32 C33 N12 C22 -62.4(8) . . . . ? C34 C33 N12 C22 115.8(6) . . . . ? C32 C33 N12 C23 122.9(6) . . . . ? C34 C33 N12 C23 -58.9(8) . . . . ? N14 C25 N13 C27 -1.0(6) . . . . ? N14 C25 N13 Pd3 -177.5(3) . . . . ? C26 C27 N13 C25 0.3(6) . . . . ? C26 C27 N13 Pd3 177.0(4) . . . . ? N13 C25 N14 C26 1.2(6) . . . . ? N13 C25 N14 C34 178.3(5) . . . . ? C27 C26 N14 C25 -1.0(7) . . . . ? C27 C26 N14 C34 -178.0(5) . . . . ? C35 C34 N14 C25 -52.9(8) . . . . ? C33 C34 N14 C25 128.2(6) . . . . ? C35 C34 N14 C26 123.6(6) . . . . ? C33 C34 N14 C26 -55.3(8) . . . . ? N16 C29 N15 C30 0.0(6) . . . . ? N16 C29 N15 Pd3 176.4(3) . . . 2_757 ? C28 C30 N15 C29 -0.5(7) . . . . ? C28 C30 N15 Pd3 -176.9(4) . . . 2_757 ? N15 C29 N16 C28 0.4(6) . . . . ? N15 C29 N16 C36 -175.3(5) . . . . ? C30 C28 N16 C29 -0.6(6) . . . . ? C30 C28 N16 C36 175.0(5) . . . . ? C31 C36 N16 C29 -132.0(6) . . . . ? C35 C36 N16 C29 52.0(8) . . . . ? C31 C36 N16 C28 53.1(8) . . . . ? C35 C36 N16 C28 -123.0(6) . . . . ? _refine_diff_density_max 1.276 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.089 _shelxl_version_number 2013-4 _shelx_res_file ; TITL ds65 in C2/c CELL 0.71073 50.0277 11.5534 35.1453 90.000 127.435 90.000 ZERR 8.00 0.0019 0.0005 0.0014 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C N O PD H UNIT 528 8 8 32 200 MERG 2 OMIT 0.00 50.00 DFIX 1.500 0.020 C15 C16 FMAP 2 PLAN 50 ACTA BOND $H CONF SIZE 0.050 0.080 0.100 L.S. 6 TEMP 23.00 WGHT 0.079700 FVAR 0.22572 C1 1 0.818221 0.282602 1.293307 11.00000 0.21772 0.05397 = 0.18217 -0.02744 0.12885 -0.02693 AFIX 33 H1A 5 0.803268 0.295123 1.259309 11.00000 -1.50000 H1B 5 0.809555 0.221606 1.301560 11.00000 -1.50000 H1C 5 0.840057 0.261268 1.302832 11.00000 -1.50000 AFIX 0 C2 1 0.844264 0.379753 1.373641 11.00000 0.08898 0.23858 = 0.09331 0.07964 0.04732 -0.02403 AFIX 33 H2A 5 0.866055 0.354024 1.384256 11.00000 -1.50000 H2B 5 0.834873 0.324025 1.382773 11.00000 -1.50000 H2C 5 0.846392 0.453043 1.388127 11.00000 -1.50000 AFIX 0 C3 1 0.787788 0.429790 1.304837 11.00000 0.08072 0.12172 = 0.13280 0.03779 0.07726 -0.00175 AFIX 23 H3A 5 0.775131 0.361932 1.301599 11.00000 -1.20000 H3B 5 0.791088 0.477789 1.330028 11.00000 -1.20000 AFIX 0 C4 1 0.769150 0.491427 1.261918 11.00000 0.06929 0.12884 = 0.13428 0.03112 0.06521 0.00905 AFIX 23 H4A 5 0.749345 0.523001 1.257146 11.00000 -1.20000 H4B 5 0.761536 0.438234 1.235787 11.00000 -1.20000 AFIX 0 C5 1 0.784549 0.696436 1.277792 11.00000 0.11845 0.15593 = 0.16589 -0.02320 0.09566 0.03478 AFIX 33 H5A 5 0.797091 0.755803 1.275826 11.00000 -1.50000 H5B 5 0.793171 0.686716 1.310569 11.00000 -1.50000 H5C 5 0.761257 0.718275 1.258855 11.00000 -1.50000 AFIX 0 C6 1 0.772629 0.603924 1.208034 11.00000 0.09302 0.21819 = 0.06389 0.05691 0.03256 0.03254 AFIX 33 H6A 5 0.775188 0.534260 1.195643 11.00000 -1.50000 H6B 5 0.783813 0.666548 1.204963 11.00000 -1.50000 H6C 5 0.749135 0.621695 1.190315 11.00000 -1.50000 AFIX 0 C7 1 0.742936 0.506968 0.997277 11.00000 0.08159 0.17017 = 0.11883 0.04522 0.07746 0.03950 AFIX 33 H7A 5 0.756122 0.567574 1.019958 11.00000 -1.50000 H7B 5 0.752049 0.433182 1.012350 11.00000 -1.50000 H7C 5 0.720100 0.512694 0.986254 11.00000 -1.50000 AFIX 0 C8 1 0.731431 0.633410 0.937017 11.00000 0.07271 0.13083 = 0.11449 0.04296 0.06084 0.04557 AFIX 33 H8A 5 0.745700 0.690087 0.961148 11.00000 -1.50000 H8B 5 0.708880 0.641788 0.926930 11.00000 -1.50000 H8C 5 0.731555 0.644515 0.910055 11.00000 -1.50000 AFIX 0 C9 1 0.722732 0.429506 0.919893 11.00000 0.04965 0.22333 = 0.21258 -0.10953 0.05885 -0.06395 AFIX 23 H9A 5 0.706579 0.402918 0.924679 11.00000 -1.20000 H9B 5 0.710003 0.467709 0.888953 11.00000 -1.20000 AFIX 0 C10 1 0.737188 0.333535 0.916667 11.00000 0.11601 0.14860 = 0.24962 -0.10629 0.13082 -0.07394 AFIX 23 H10A 5 0.723184 0.308136 0.883538 11.00000 -1.20000 H10B 5 0.737088 0.272346 0.935477 11.00000 -1.20000 AFIX 0 C11 1 0.771756 0.359008 0.890752 11.00000 0.15167 0.11303 = 0.08158 -0.03468 0.06647 -0.03864 AFIX 33 H11A 5 0.794455 0.369367 0.901660 11.00000 -1.50000 H11B 5 0.758474 0.424901 0.872080 11.00000 -1.50000 H11C 5 0.762427 0.290473 0.871395 11.00000 -1.50000 AFIX 0 C12 1 0.789873 0.237158 0.957698 11.00000 0.16132 0.05251 = 0.14080 -0.01451 0.08278 -0.00897 AFIX 33 H12A 5 0.812478 0.241198 0.967690 11.00000 -1.50000 H12B 5 0.778426 0.172864 0.936303 11.00000 -1.50000 H12C 5 0.790393 0.227032 0.985253 11.00000 -1.50000 AFIX 0 C13 1 1.017924 0.962622 1.067881 11.00000 0.15729 0.07221 = 0.15409 0.00484 0.14103 -0.01155 AFIX 33 H13A 5 1.034509 0.918718 1.095885 11.00000 -1.50000 H13B 5 1.028936 1.012883 1.059571 11.00000 -1.50000 H13C 5 1.003232 0.910803 1.041745 11.00000 -1.50000 AFIX 0 C14 1 1.022972 1.107559 1.121086 11.00000 0.16593 0.07288 = 0.11402 -0.03028 0.09605 -0.05810 AFIX 33 H14A 5 1.038901 1.059212 1.147884 11.00000 -1.50000 H14B 5 1.010932 1.153628 1.128877 11.00000 -1.50000 H14C 5 1.034675 1.157399 1.113813 11.00000 -1.50000 AFIX 0 C15 1 0.973807 1.098666 1.035215 11.00000 0.13563 0.13339 = 0.10743 0.07165 0.07985 0.01061 AFIX 23 H15A 5 0.981358 1.178508 1.041676 11.00000 -1.20000 H15B 5 0.974592 1.071810 1.009761 11.00000 -1.20000 AFIX 0 C16 1 0.941018 1.098355 1.017857 11.00000 0.11948 0.23966 = 0.20979 0.18044 0.07727 0.04021 AFIX 23 H16A 5 0.927613 1.084528 0.983641 11.00000 -1.20000 H16B 5 0.935741 1.176062 1.021872 11.00000 -1.20000 AFIX 0 C17 1 0.912669 1.088279 1.051229 11.00000 0.18195 0.10462 = 0.13372 0.03240 0.10348 0.10224 AFIX 33 H17A 5 0.903447 1.035104 1.061467 11.00000 -1.50000 H17B 5 0.894866 1.133951 1.025064 11.00000 -1.50000 H17C 5 0.928579 1.138205 1.077380 11.00000 -1.50000 AFIX 0 C18 1 0.904312 0.947714 0.995702 11.00000 0.09987 0.13024 = 0.06647 0.00217 0.00404 0.01836 AFIX 33 H18A 5 0.895753 0.894229 1.006826 11.00000 -1.50000 H18B 5 0.914511 0.905613 0.983992 11.00000 -1.50000 H18C 5 0.886171 0.994065 0.970335 11.00000 -1.50000 AFIX 0 C19 1 0.857817 0.646869 1.245642 11.00000 0.05450 0.06863 = 0.04993 -0.00347 0.03452 -0.01073 AFIX 43 H19 5 0.851192 0.583059 1.225622 11.00000 -1.20000 AFIX 0 C20 1 0.879424 0.813652 1.279793 11.00000 0.07200 0.06825 = 0.07201 -0.00812 0.05625 -0.00961 AFIX 43 H20 5 0.890313 0.884857 1.288303 11.00000 -1.20000 AFIX 0 C21 1 0.865603 0.763739 1.297868 11.00000 0.07563 0.07908 = 0.06632 -0.00254 0.05502 0.00158 AFIX 43 H21 5 0.865062 0.795968 1.321640 11.00000 -1.20000 AFIX 0 C22 1 0.831697 0.624237 1.068888 11.00000 0.04333 0.07207 = 0.04738 -0.00165 0.02796 -0.00256 AFIX 43 H22 5 0.833510 0.559475 1.086038 11.00000 -1.20000 AFIX 0 C23 1 0.839497 0.799546 1.052762 11.00000 0.06042 0.06020 = 0.06157 0.01279 0.03986 0.01028 AFIX 43 H23 5 0.846962 0.875093 1.055719 11.00000 -1.20000 AFIX 0 C24 1 0.817538 0.739545 1.011547 11.00000 0.05893 0.06305 = 0.04960 0.00969 0.03088 0.00784 AFIX 43 H24 5 0.807267 0.768141 0.980818 11.00000 -1.20000 AFIX 0 C25 1 0.935053 0.856067 1.130508 11.00000 0.05351 0.04468 = 0.03920 0.00292 0.03109 -0.00367 AFIX 43 H25 5 0.941125 0.923636 1.148401 11.00000 -1.20000 AFIX 0 C26 1 0.914541 0.688434 1.101267 11.00000 0.07095 0.04086 = 0.08592 -0.01037 0.06127 -0.01157 AFIX 43 H26 5 0.903654 0.617746 1.094813 11.00000 -1.20000 AFIX 0 C27 1 0.930073 0.726130 1.082714 11.00000 0.05858 0.04801 = 0.05852 -0.00786 0.04313 -0.00629 AFIX 43 H27 5 0.931811 0.687119 1.061156 11.00000 -1.20000 AFIX 0 C28 1 0.951478 0.695394 1.321409 11.00000 0.06233 0.04782 = 0.06082 0.00856 0.03876 -0.00900 AFIX 43 H28 5 0.939914 0.626710 1.315828 11.00000 -1.20000 AFIX 0 C29 1 0.967011 0.865594 1.310928 11.00000 0.05397 0.04918 = 0.05510 0.00154 0.04246 -0.00075 AFIX 43 H29 5 0.967623 0.932102 1.296567 11.00000 -1.20000 AFIX 0 C30 1 0.979050 0.735901 1.364133 11.00000 0.05163 0.05947 = 0.03404 0.00420 0.02271 -0.00072 AFIX 43 H30 5 0.989825 0.697753 1.393321 11.00000 -1.20000 AFIX 0 C31 1 0.885615 0.746576 1.217134 11.00000 0.04940 0.05657 = 0.04683 0.00277 0.03334 -0.00965 C32 1 0.862590 0.734743 1.167887 11.00000 0.04851 0.06447 = 0.05912 0.00274 0.03776 -0.01293 AFIX 43 H32 5 0.840057 0.720767 1.153906 11.00000 -1.20000 AFIX 0 C33 1 0.872735 0.743430 1.140002 11.00000 0.04339 0.05094 = 0.04694 0.00572 0.03086 -0.00347 C34 1 0.905725 0.766148 1.159019 11.00000 0.05241 0.04180 = 0.04119 0.00061 0.03450 -0.01143 C35 1 0.929203 0.782819 1.207996 11.00000 0.05215 0.04943 = 0.06417 0.00314 0.04294 -0.00715 AFIX 43 H35 5 0.951370 0.801391 1.221246 11.00000 -1.20000 AFIX 0 C36 1 0.919108 0.771327 1.237328 11.00000 0.04439 0.05659 = 0.05101 0.00935 0.03314 -0.00162 C37 1 0.860109 0.394898 1.036187 11.00000 0.05422 0.05168 = 0.07750 0.00694 0.03964 0.00619 AFIX 43 H37 5 0.852335 0.357653 1.051212 11.00000 -1.20000 AFIX 0 C38 1 0.893753 0.382101 1.054669 11.00000 0.05078 0.05682 = 0.07070 0.00273 0.03514 0.00072 AFIX 43 H38 5 0.907853 0.334708 1.081134 11.00000 -1.20000 AFIX 0 C39 1 0.906030 0.437764 1.034541 11.00000 0.05550 0.03800 = 0.06392 -0.00204 0.03704 -0.00184 C40 1 0.883721 0.507413 0.994854 11.00000 0.05671 0.05538 = 0.07487 -0.00789 0.05061 -0.00428 AFIX 43 H40 5 0.891170 0.548004 0.980056 11.00000 -1.20000 AFIX 0 C41 1 0.850774 0.515905 0.977699 11.00000 0.04864 0.07459 = 0.05691 0.01121 0.03245 0.00295 AFIX 43 H41 5 0.836294 0.562996 0.951289 11.00000 -1.20000 AFIX 0 C42 1 0.942216 0.432585 1.054685 11.00000 0.04891 0.03665 = 0.05660 -0.00396 0.02944 -0.00210 C43 1 1.104338 0.405631 1.181160 11.00000 0.04097 0.05261 = 0.05911 0.00111 0.02199 0.00598 AFIX 43 H43 5 1.120402 0.368539 1.209955 11.00000 -1.20000 AFIX 0 C44 1 1.071684 0.385876 1.160839 11.00000 0.05612 0.05013 = 0.07508 0.00470 0.04443 0.00628 AFIX 43 H44 5 1.065738 0.336031 1.175356 11.00000 -1.20000 AFIX 0 C45 1 1.046247 0.441993 1.116843 11.00000 0.04753 0.03975 = 0.08137 -0.01176 0.04600 -0.00295 C46 1 1.057396 0.507452 1.096933 11.00000 0.06003 0.07529 = 0.06014 0.01057 0.03833 0.00700 AFIX 43 H46 5 1.041971 0.540340 1.066873 11.00000 -1.20000 AFIX 0 C47 1 1.091684 0.525716 1.121117 11.00000 0.05923 0.08649 = 0.06919 -0.01499 0.05057 -0.01493 AFIX 43 H47 5 1.098601 0.575393 1.107804 11.00000 -1.20000 AFIX 0 C48 1 0.952249 0.437135 1.026440 11.00000 0.05609 0.06290 = 0.04422 0.00251 0.02462 0.00032 AFIX 43 H48 5 0.936149 0.440950 0.993339 11.00000 -1.20000 AFIX 0 C49 1 0.986093 0.436182 1.046177 11.00000 0.05598 0.06022 = 0.07555 0.00500 0.04685 -0.00016 AFIX 43 H49 5 0.992360 0.438990 1.026120 11.00000 -1.20000 AFIX 0 C50 1 1.010831 0.431087 1.095541 11.00000 0.05168 0.03408 = 0.05916 -0.00390 0.03413 -0.00252 C51 1 1.000104 0.426734 1.123780 11.00000 0.04473 0.05796 = 0.06332 0.00327 0.03201 0.00195 AFIX 43 H51 5 1.016101 0.425116 1.156935 11.00000 -1.20000 AFIX 0 C52 1 0.966048 0.424708 1.103967 11.00000 0.06473 0.05407 = 0.06795 -0.01213 0.04466 -0.00276 AFIX 43 H52 5 0.959441 0.418168 1.123546 11.00000 -1.20000 AFIX 0 N1 2 0.821037 0.392811 1.318914 11.00000 0.05485 0.09621 = 0.08983 0.02358 0.05101 0.00310 N2 2 0.787799 0.587232 1.259652 11.00000 0.05323 0.11321 = 0.06843 0.01806 0.04016 0.00912 N3 2 0.743756 0.518329 0.956536 11.00000 0.04327 0.09606 = 0.07742 0.00253 0.03448 -0.00891 N4 2 0.771620 0.347144 0.932453 11.00000 0.05520 0.09779 = 0.08887 -0.02355 0.04548 -0.01170 N5 2 0.998218 1.032045 1.077717 11.00000 0.08832 0.04906 = 0.06485 -0.00794 0.05941 -0.01217 N6 2 0.929674 1.023385 1.035587 11.00000 0.07277 0.04578 = 0.05837 0.01906 0.04260 0.02066 N7 2 1.115068 0.474027 1.162981 11.00000 0.06912 0.04749 = 0.06421 -0.00296 0.05055 -0.00965 N8 2 0.838728 0.459761 0.997214 11.00000 0.04461 0.05921 = 0.06981 -0.00852 0.03825 -0.00706 N9 2 0.852316 0.659288 1.277140 11.00000 0.05416 0.08298 = 0.05589 -0.00244 0.04360 -0.00445 N10 2 0.874311 0.738479 1.246011 11.00000 0.04430 0.06059 = 0.05148 0.00128 0.03510 -0.00798 N11 2 0.812753 0.629814 1.022100 11.00000 0.04117 0.07098 = 0.04318 -0.00102 0.02288 0.00233 N12 2 0.848284 0.724782 1.089051 11.00000 0.04112 0.05378 = 0.04824 0.00381 0.02916 -0.00569 N13 2 0.942737 0.833682 1.102206 11.00000 0.05091 0.03368 = 0.04224 0.00318 0.03330 0.00192 N14 2 0.917640 0.771860 1.130934 11.00000 0.04409 0.04868 = 0.03778 -0.00149 0.02761 -0.00735 N15 2 0.988456 0.839434 1.357947 11.00000 0.04431 0.04137 = 0.03843 -0.00008 0.02680 -0.00460 N16 2 0.944449 0.778405 1.288242 11.00000 0.05033 0.04483 = 0.04157 0.00123 0.03020 -0.00731 PD1 4 0.836765 0.528983 1.298557 11.00000 0.04404 0.07582 = 0.05611 0.00738 0.03463 -0.00109 PD2 4 0.791774 0.491236 0.977102 11.00000 0.04157 0.06803 = 0.05789 -0.00484 0.03022 -0.00477 PD3 4 0.970823 0.931375 1.090222 11.00000 0.05460 0.03600 = 0.04442 0.00407 0.03612 -0.00032 HKLF 4 REM ds65 in C2/c REM R1 = 0.0594 for 8341 Fo > 4sig(Fo) and 0.1105 for all 14208 data REM 640 parameters refined using 1 restraints END WGHT 0.0757 0.0000 REM Highest difference peak 1.276, deepest hole -0.939, 1-sigma level 0.089 Q1 1 0.8537 0.4434 1.3078 11.00000 0.05 1.28 Q2 1 0.9717 0.8533 1.0917 11.00000 0.05 0.94 Q3 1 0.7861 0.5846 0.9686 11.00000 0.05 0.62 Q4 1 0.7924 0.4009 0.9786 11.00000 0.05 0.53 Q5 1 0.9587 1.0514 1.0989 11.00000 0.05 0.50 Q6 1 0.7743 0.5037 0.9369 11.00000 0.05 0.50 Q7 1 0.8075 0.5184 1.2876 11.00000 0.05 0.44 Q8 1 0.9862 0.9247 1.0915 11.00000 0.05 0.44 Q9 1 0.7648 0.5798 0.9397 11.00000 0.05 0.43 Q10 1 0.8118 0.6223 1.2800 11.00000 0.05 0.43 Q11 1 0.8344 0.6825 1.2910 11.00000 0.05 0.42 Q12 1 0.9531 1.1273 1.0395 11.00000 0.05 0.42 Q13 1 1.0070 0.8888 1.3804 11.00000 0.05 0.42 Q14 1 0.8374 0.3170 1.3288 11.00000 0.05 0.42 Q15 1 0.9706 0.9922 1.0887 11.00000 0.05 0.40 Q16 1 1.0574 1.0185 1.1583 11.00000 0.05 0.40 Q17 1 0.9635 0.9262 1.0418 11.00000 0.05 0.39 Q18 1 0.9596 0.9237 1.0996 11.00000 0.05 0.38 Q19 1 0.9445 1.1707 1.0688 11.00000 0.05 0.37 Q20 1 0.8215 0.5621 1.0095 11.00000 0.05 0.37 Q21 1 0.8374 0.5382 1.2596 11.00000 0.05 0.36 Q22 1 1.0345 0.9771 1.1211 11.00000 0.05 0.36 Q23 1 0.9574 0.9134 1.2790 11.00000 0.05 0.36 Q24 1 0.9658 1.0303 1.0491 11.00000 0.05 0.36 Q25 1 0.8668 0.5694 1.2923 11.00000 0.05 0.36 Q26 1 0.9506 1.0204 1.0390 11.00000 0.05 0.36 Q27 1 1.1295 0.5807 1.1611 11.00000 0.05 0.36 Q28 1 0.8540 0.2904 1.3297 11.00000 0.05 0.36 Q29 1 0.8223 0.5280 1.2508 11.00000 0.05 0.35 Q30 1 0.9590 0.8213 1.1008 11.00000 0.05 0.35 Q31 1 0.7648 0.4385 0.9423 11.00000 0.05 0.35 Q32 1 0.9409 1.0263 1.0600 11.00000 0.05 0.35 Q33 1 0.9742 1.1595 1.0774 11.00000 0.05 0.34 Q34 1 0.8497 0.6372 1.3207 11.00000 0.05 0.34 Q35 1 0.7738 0.4854 1.2094 11.00000 0.05 0.34 Q36 1 0.7798 0.4918 1.1823 11.00000 0.05 0.34 Q37 1 0.9211 0.8820 1.2371 11.00000 0.05 0.34 Q38 1 1.0246 0.8803 1.0705 11.00000 0.05 0.34 Q39 1 0.8319 0.6359 1.2715 11.00000 0.05 0.34 Q40 1 0.9996 1.0065 1.1223 11.00000 0.05 0.33 Q41 1 0.8226 0.5263 1.3214 11.00000 0.05 0.33 Q42 1 0.9627 1.1283 1.0230 11.00000 0.05 0.32 Q43 1 0.9202 0.6749 1.2276 11.00000 0.05 0.32 Q44 1 0.7679 0.3503 1.1872 11.00000 0.05 0.32 Q45 1 0.8943 0.6965 1.1484 11.00000 0.05 0.31 Q46 1 0.9437 0.5883 1.0707 11.00000 0.05 0.31 Q47 1 0.7318 0.5689 0.8897 11.00000 0.05 0.31 Q48 1 1.0445 0.4230 1.0760 11.00000 0.05 0.31 Q49 1 1.0715 0.5214 1.1194 11.00000 0.05 0.31 Q50 1 0.8431 0.2174 1.3214 11.00000 0.05 0.31 ; _shelx_res_checksum 76644 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.012 0.063 0.026 6894 3165 ' ' _platon_squeeze_details ; 12(N O3), 41(H2O) have been removed from formula unit by squeeze process. ; _database_code_depnum_ccdc_archive 'CCDC 951437'