# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_C60_2CryptandNa_110K _database_code_depnum_ccdc_archive 'CCDC 894601' _audit_creation_method ; SHELXL-97 CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60, 2(C18 H36 N2 Na O6)' _chemical_formula_sum 'C96 H72 N4 Na2 O12' _chemical_formula_weight 1519.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8970(10) _cell_length_b 17.499(2) _cell_length_c 17.785(2) _cell_angle_alpha 85.433(8) _cell_angle_beta 69.071(9) _cell_angle_gamma 70.433(9) _cell_volume 3528.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 3.0579 _cell_measurement_theta_max 25.1605 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_T_min 0.76663 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_detector_area_resol_mean 10.4752 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15684 _diffrn_reflns_av_R_equivalents 0.1016 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.18 _reflns_number_total 9182 _reflns_number_gt 5492 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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 'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+0.2845P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9182 _refine_ls_number_parameters 1391 _refine_ls_number_restraints 2983 _refine_ls_R_factor_all 0.1299 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2434 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.48110(14) 0.17822(10) 0.87495(10) 0.0387(4) Uani 1 1 d . . . O10 O 0.6452(3) 0.07046(18) 0.90342(18) 0.0456(8) Uani 1 1 d . . . N3 N 0.3510(3) 0.3245(2) 0.9978(2) 0.0374(9) Uani 1 1 d . . . O7 O 0.2653(2) 0.26485(17) 0.89212(17) 0.0407(7) Uani 1 1 d . . . O11 O 0.5741(3) 0.29515(19) 0.8610(2) 0.0511(9) Uani 1 1 d . . . O9 O 0.4436(3) 0.15290(18) 1.03038(18) 0.0443(8) Uani 1 1 d . . . O12 O 0.5774(3) 0.2117(2) 0.73423(19) 0.0563(9) Uani 1 1 d . . . N4 N 0.5957(3) 0.0493(2) 0.7676(2) 0.0486(10) Uani 1 1 d . . . O8 O 0.3576(3) 0.09959(18) 0.86428(19) 0.0456(8) Uani 1 1 d . . . C901 C 0.2279(4) 0.3537(3) 1.0036(3) 0.0401(11) Uani 1 1 d . . . H90A H 0.1917 0.4112 1.0235 0.048 Uiso 1 1 calc R . . H90B H 0.1847 0.3217 1.0429 0.048 Uiso 1 1 calc R . . C10 C 0.4061(4) 0.3867(3) 0.9669(3) 0.0461(12) Uani 1 1 d . . . H10A H 0.3884 0.4244 1.0119 0.055 Uiso 1 1 calc R . . H10B H 0.3725 0.4185 0.9275 0.055 Uiso 1 1 calc R . . C14 C 0.5590(4) 0.1363(3) 1.0311(3) 0.0545(13) Uani 1 1 d . . . H14A H 0.5573 0.1318 1.0874 0.065 Uiso 1 1 calc R . . H14B H 0.5887 0.1812 1.0071 0.065 Uiso 1 1 calc R . . C15 C 0.2003(4) 0.2142(3) 0.9357(3) 0.0447(12) Uani 1 1 d . . . H15A H 0.1150 0.2436 0.9507 0.054 Uiso 1 1 calc R . . H15B H 0.2177 0.1978 0.9856 0.054 Uiso 1 1 calc R . . C16 C 0.3619(4) 0.2968(3) 1.0745(3) 0.0425(11) Uani 1 1 d . . . H16A H 0.2983 0.3347 1.1182 0.051 Uiso 1 1 calc R . . H16B H 0.4379 0.2977 1.0752 0.051 Uiso 1 1 calc R . . C18 C 0.2169(4) 0.3464(3) 0.9234(3) 0.0441(11) Uani 1 1 d . . . H18A H 0.1328 0.3677 0.9293 0.053 Uiso 1 1 calc R . . H18B H 0.2577 0.3800 0.8847 0.053 Uiso 1 1 calc R . . C20 C 0.6374(5) 0.0598(3) 0.9848(3) 0.0530(13) Uani 1 1 d . . . H20A H 0.7164 0.0456 0.9886 0.064 Uiso 1 1 calc R . . H20B H 0.6057 0.0152 1.0067 0.064 Uiso 1 1 calc R . . C21 C 0.3556(4) 0.2118(3) 1.0907(3) 0.0441(11) Uani 1 1 d . . . H21A H 0.3640 0.1961 1.1434 0.053 Uiso 1 1 calc R . . H21B H 0.2772 0.2119 1.0940 0.053 Uiso 1 1 calc R . . C25 C 0.7122(4) -0.0025(3) 0.8571(3) 0.0505(13) Uani 1 1 d . . . H25A H 0.6772 -0.0454 0.8799 0.061 Uiso 1 1 calc R . . H25B H 0.7934 -0.0206 0.8576 0.061 Uiso 1 1 calc R . . C30 C 0.7140(4) 0.0119(3) 0.7717(3) 0.0582(14) Uani 1 1 d . . . H30A H 0.7614 0.0477 0.7466 0.070 Uiso 1 1 calc R . . H30B H 0.7528 -0.0405 0.7403 0.070 Uiso 1 1 calc R . . C32 C 0.6195(5) 0.2784(3) 0.7216(3) 0.0667(16) Uani 1 1 d . . . H32A H 0.6080 0.3065 0.6732 0.080 Uiso 1 1 calc R . . H32B H 0.7046 0.2589 0.7126 0.080 Uiso 1 1 calc R . . C36 C 0.2345(4) 0.1415(3) 0.8835(3) 0.0513(13) Uani 1 1 d . . . H36A H 0.1892 0.1055 0.9119 0.062 Uiso 1 1 calc R . . H36B H 0.2174 0.1580 0.8335 0.062 Uiso 1 1 calc R . . C37 C 0.5563(5) 0.3343(3) 0.7915(3) 0.0641(15) Uani 1 1 d . . . H37A H 0.5843 0.3816 0.7823 0.077 Uiso 1 1 calc R . . H37B H 0.4713 0.3541 0.8000 0.077 Uiso 1 1 calc R . . C47 C 0.6023(5) 0.0816(4) 0.6885(3) 0.0643(16) Uani 1 1 d . . . H47A H 0.5233 0.0979 0.6844 0.077 Uiso 1 1 calc R . . H47B H 0.6557 0.0381 0.6466 0.077 Uiso 1 1 calc R . . C49 C 0.5288(5) -0.0057(3) 0.7913(4) 0.0601(15) Uani 1 1 d . . . H49A H 0.5401 -0.0329 0.8401 0.072 Uiso 1 1 calc R . . H49B H 0.5599 -0.0481 0.7478 0.072 Uiso 1 1 calc R . . C52 C 0.6443(5) 0.1518(4) 0.6723(3) 0.0629(16) Uani 1 1 d . . . H52A H 0.7278 0.1342 0.6676 0.075 Uiso 1 1 calc R . . H52B H 0.6388 0.1745 0.6205 0.075 Uiso 1 1 calc R . . C54 C 0.3989(4) 0.0351(3) 0.8085(3) 0.0564(14) Uani 1 1 d . . . H54A H 0.3851 0.0553 0.7582 0.068 Uiso 1 1 calc R . . H54B H 0.3567 -0.0043 0.8304 0.068 Uiso 1 1 calc R . . C82 C 0.5389(4) 0.3493(3) 0.9265(3) 0.0572(14) Uani 1 1 d . . . H82A H 0.5725 0.3936 0.9075 0.069 Uiso 1 1 calc R . . H82B H 0.5720 0.3202 0.9671 0.069 Uiso 1 1 calc R . . Na2 Na 0.02310(14) 0.27481(10) 0.66889(10) 0.0411(4) Uani 1 1 d . . . O3 O -0.0587(3) 0.21379(19) 0.79933(19) 0.0513(9) Uani 1 1 d . . . N2 N 0.1805(3) 0.1598(2) 0.5279(2) 0.0399(9) Uani 1 1 d . . . O6 O 0.2537(3) 0.1797(2) 0.6627(2) 0.0540(9) Uani 1 1 d . . . O4 O -0.0470(3) 0.16467(18) 0.6535(2) 0.0459(8) Uani 1 1 d . . . O2 O 0.0298(3) 0.31987(18) 0.5329(2) 0.0503(9) Uani 1 1 d . . . O5 O 0.1500(3) 0.34946(19) 0.67723(18) 0.0447(8) Uani 1 1 d . . . O1 O -0.1609(3) 0.3957(2) 0.6722(2) 0.0590(10) Uani 1 1 d . . . N1 N -0.0760(3) 0.3796(2) 0.8016(2) 0.0425(9) Uani 1 1 d . . . C8 C 0.1300(4) 0.0957(3) 0.5384(3) 0.0518(13) Uani 1 1 d . . . H8A H 0.1619 0.0547 0.5732 0.062 Uiso 1 1 calc R . . H8B H 0.1530 0.0686 0.4853 0.062 Uiso 1 1 calc R . . C9 C 0.3012(4) 0.1289(3) 0.5262(3) 0.0473(12) Uani 1 1 d . . . H9A H 0.3406 0.1694 0.5024 0.057 Uiso 1 1 calc R . . H9B H 0.3439 0.0786 0.4913 0.057 Uiso 1 1 calc R . . C22 C 0.3236(4) 0.2301(3) 0.6551(3) 0.0460(12) Uani 1 1 d . . . H22A H 0.4029 0.2044 0.6150 0.055 Uiso 1 1 calc R . . H22B H 0.3325 0.2346 0.7075 0.055 Uiso 1 1 calc R . . C23 C 0.1732(4) 0.2048(3) 0.4560(3) 0.0517(13) Uani 1 1 d . . . H23A H 0.1143 0.1936 0.4390 0.062 Uiso 1 1 calc R . . H23B H 0.2502 0.1848 0.4118 0.062 Uiso 1 1 calc R . . C26 C -0.0344(5) 0.4031(3) 0.5346(3) 0.0618(15) Uani 1 1 d . . . H26A H -0.0353 0.4195 0.4802 0.074 Uiso 1 1 calc R . . H26B H 0.0016 0.4364 0.5530 0.074 Uiso 1 1 calc R . . C27 C -0.1351(5) 0.2636(4) 0.8683(3) 0.0639(15) Uani 1 1 d . . . H27A H -0.1401 0.2313 0.9170 0.077 Uiso 1 1 calc R . . H27B H -0.2149 0.2867 0.8654 0.077 Uiso 1 1 calc R . . C28 C 0.3082(4) 0.1109(3) 0.6086(3) 0.0481(12) Uani 1 1 d . . . H28A H 0.2705 0.0693 0.6316 0.058 Uiso 1 1 calc R . . H28B H 0.3919 0.0877 0.6033 0.058 Uiso 1 1 calc R . . C33 C 0.1410(4) 0.2926(3) 0.4680(3) 0.0501(13) Uani 1 1 d . . . H33A H 0.2016 0.3053 0.4816 0.060 Uiso 1 1 calc R . . H33B H 0.1349 0.3200 0.4182 0.060 Uiso 1 1 calc R . . C35 C -0.0894(5) 0.3307(4) 0.8732(3) 0.0612(15) Uani 1 1 d . . . H35A H -0.1441 0.3664 0.9213 0.073 Uiso 1 1 calc R . . H35B H -0.0123 0.3069 0.8801 0.073 Uiso 1 1 calc R . . C42 C -0.1844(5) 0.4640(3) 0.7198(3) 0.0619(15) Uani 1 1 d . . . H42A H -0.2605 0.5050 0.7227 0.074 Uiso 1 1 calc R . . H42B H -0.1218 0.4889 0.6965 0.074 Uiso 1 1 calc R . . C44 C -0.1574(5) 0.4148(4) 0.5924(4) 0.0742(18) Uani 1 1 d . . . H44A H -0.2069 0.4719 0.5924 0.089 Uiso 1 1 calc R . . H44B H -0.1908 0.3798 0.5739 0.089 Uiso 1 1 calc R . . C45 C 0.0059(4) 0.4222(3) 0.7955(3) 0.0463(12) Uani 1 1 d . . . H45A H -0.0073 0.4416 0.8501 0.056 Uiso 1 1 calc R . . H45B H -0.0094 0.4703 0.7627 0.056 Uiso 1 1 calc R . . C51 C -0.0261(5) 0.1078(3) 0.7130(3) 0.0616(15) Uani 1 1 d . . . H51A H 0.0582 0.0893 0.7066 0.074 Uiso 1 1 calc R . . H51B H -0.0471 0.0598 0.7067 0.074 Uiso 1 1 calc R . . C53 C -0.0976(5) 0.1474(3) 0.7922(4) 0.0627(16) Uani 1 1 d . . . H53A H -0.1817 0.1679 0.7979 0.075 Uiso 1 1 calc R . . H53B H -0.0881 0.1085 0.8348 0.075 Uiso 1 1 calc R . . C57 C -0.0043(4) 0.1279(3) 0.5764(3) 0.0523(13) Uani 1 1 d . . . H57A H -0.0354 0.1680 0.5406 0.063 Uiso 1 1 calc R . . H57B H -0.0347 0.0823 0.5795 0.063 Uiso 1 1 calc R . . C61 C 0.2715(4) 0.3125(3) 0.6300(3) 0.0499(13) Uani 1 1 d . . . H61A H 0.3159 0.3474 0.6344 0.060 Uiso 1 1 calc R . . H61B H 0.2797 0.3092 0.5727 0.060 Uiso 1 1 calc R . . C66 C 0.1318(4) 0.3689(3) 0.7580(3) 0.0427(11) Uani 1 1 d . . . H66A H 0.1854 0.3979 0.7590 0.051 Uiso 1 1 calc R . . H66B H 0.1473 0.3188 0.7881 0.051 Uiso 1 1 calc R . . C68 C -0.1885(4) 0.4354(4) 0.8020(3) 0.0601(15) Uani 1 1 d . . . H68A H -0.2124 0.4829 0.8385 0.072 Uiso 1 1 calc R . . H68B H -0.2486 0.4082 0.8231 0.072 Uiso 1 1 calc R . . C401 C 1.0282(10) 0.2035(5) 0.1465(4) 0.050(3) Uani 0.505(3) 1 d PDU A 1 C402 C 1.0029(8) 0.2901(4) 0.1372(5) 0.053(3) Uani 0.505(3) 1 d PDU A 1 C403 C 0.9258(4) 0.3177(4) 0.0909(5) 0.058(3) Uani 0.505(3) 1 d PDU A 1 C404 C 0.9008(4) 0.2477(2) 0.0733(5) 0.052(2) Uani 0.505(3) 1 d PDU A 1 C405 C 0.9642(5) 0.1775(5) 0.1070(5) 0.053(3) Uani 0.505(3) 1 d PDU A 1 C406 C 1.0374(9) 0.1706(4) 0.2172(6) 0.050(3) Uani 0.505(3) 1 d PDU A 1 C407 C 0.9829(6) 0.1098(6) 0.2526(3) 0.055(3) Uani 0.505(3) 1 d PDU A 1 C408 C 0.9357(4) 0.1241(5) 0.3393(4) 0.061(3) Uani 0.505(3) 1 d PDU A 1 C409 C 0.9614(5) 0.1933(3) 0.3580(5) 0.060(3) Uani 0.505(3) 1 d PDU A 1 C410 C 1.0230(9) 0.2223(4) 0.2824(3) 0.058(3) Uani 0.505(3) 1 d PDU A 1 C411 C 0.9905(9) 0.3388(4) 0.1984(6) 0.068(3) Uani 0.505(3) 1 d PDU A 1 C412 C 1.0016(9) 0.3038(5) 0.2729(3) 0.063(3) Uani 0.505(3) 1 d PDU A 1 C413 C 0.9143(5) 0.3612(3) 0.3375(5) 0.068(3) Uani 0.505(3) 1 d PDU A 1 C414 C 0.8521(4) 0.4331(5) 0.3052(3) 0.075(3) Uani 0.505(3) 1 d PDU A 1 C415 C 0.8978(4) 0.4167(6) 0.2188(4) 0.070(3) Uani 0.505(3) 1 d PDU A 1 C416 C 0.8392(5) 0.3918(3) 0.1095(4) 0.066(2) Uani 0.505(3) 1 d PDU A 1 C417 C 0.8242(5) 0.4424(4) 0.1757(3) 0.060(2) Uani 0.505(3) 1 d PDU A 1 C418 C 0.7004(4) 0.4855(5) 0.2166(3) 0.061(3) Uani 0.505(3) 1 d PDU A 1 C419 C 0.6394(6) 0.4570(4) 0.1764(3) 0.064(2) Uani 0.505(3) 1 d PDU A 1 C420 C 0.7233(4) 0.4006(3) 0.1099(4) 0.061(2) Uani 0.505(3) 1 d PDU A 1 C421 C 0.7909(6) 0.2559(3) 0.0746(4) 0.0632(18) Uani 0.505(3) 1 d PDU A 1 C422 C 0.6996(4) 0.3346(4) 0.0933(5) 0.066(2) Uani 0.505(3) 1 d PDU A 1 C423 C 0.5883(6) 0.3232(3) 0.1396(4) 0.068(2) Uani 0.505(3) 1 d PDU A 1 C424 C 0.6160(6) 0.2367(3) 0.1508(4) 0.068(2) Uani 0.505(3) 1 d PDU A 1 C425 C 0.7391(4) 0.1933(4) 0.1079(4) 0.069(2) Uani 0.505(3) 1 d PDU A 1 C426 C 0.9145(5) 0.1191(3) 0.1397(4) 0.056(2) Uani 0.505(3) 1 d PDU A 1 C427 C 0.7982(4) 0.1277(3) 0.1409(4) 0.065(2) Uani 0.505(3) 1 d PDU A 1 C428 C 0.7360(5) 0.0988(3) 0.2165(3) 0.0672(19) Uani 0.505(3) 1 d PDU A 1 C429 C 0.8138(4) 0.0713(5) 0.2622(3) 0.062(2) Uani 0.505(3) 1 d PDU A 1 C430 C 0.9232(6) 0.0849(4) 0.2151(2) 0.051(2) Uani 0.505(3) 1 d PDU A 1 C431 C 0.4410(10) 0.3657(5) 0.4138(5) 0.050(3) Uani 0.505(3) 1 d PDU A 1 C432 C 0.4665(8) 0.2790(4) 0.4226(5) 0.053(3) Uani 0.505(3) 1 d PDU A 1 C433 C 0.5445(5) 0.2526(4) 0.4683(6) 0.058(3) Uani 0.505(3) 1 d PDU A 1 C434 C 0.5687(4) 0.3218(2) 0.4886(5) 0.052(2) Uani 0.505(3) 1 d PDU A 1 C435 C 0.5069(6) 0.3907(5) 0.4524(5) 0.053(3) Uani 0.505(3) 1 d PDU A 1 C436 C 0.4307(9) 0.3991(4) 0.3435(6) 0.050(3) Uani 0.505(3) 1 d PDU A 1 C437 C 0.4877(6) 0.4583(6) 0.3069(3) 0.055(3) Uani 0.505(3) 1 d PDU A 1 C438 C 0.5342(4) 0.4465(5) 0.2199(3) 0.061(3) Uani 0.505(3) 1 d PDU A 1 C439 C 0.5085(5) 0.3771(3) 0.2017(6) 0.060(3) Uani 0.505(3) 1 d PDU A 1 C440 C 0.4476(9) 0.3476(5) 0.2774(3) 0.058(3) Uani 0.505(3) 1 d PDU A 1 C441 C 0.4808(9) 0.2305(4) 0.3606(6) 0.068(3) Uani 0.505(3) 1 d PDU A 1 C442 C 0.4691(10) 0.2660(5) 0.2864(3) 0.063(3) Uani 0.505(3) 1 d PDU A 1 C443 C 0.5570(5) 0.2089(4) 0.2217(5) 0.068(3) Uani 0.505(3) 1 d PDU A 1 C444 C 0.6186(4) 0.1376(5) 0.2551(3) 0.075(3) Uani 0.505(3) 1 d PDU A 1 C445 C 0.5722(4) 0.1519(6) 0.3418(4) 0.070(3) Uani 0.505(3) 1 d PDU A 1 C446 C 0.6303(6) 0.1782(3) 0.4508(4) 0.066(2) Uani 0.505(3) 1 d PDU A 1 C447 C 0.6459(5) 0.1270(4) 0.3848(3) 0.060(2) Uani 0.505(3) 1 d PDU A 1 C448 C 0.7698(4) 0.0841(5) 0.3441(3) 0.061(3) Uani 0.505(3) 1 d PDU A 1 C449 C 0.8315(6) 0.1126(4) 0.3836(3) 0.064(2) Uani 0.505(3) 1 d PDU A 1 C450 C 0.7468(4) 0.1694(3) 0.4494(5) 0.061(2) Uani 0.505(3) 1 d PDU A 1 C451 C 0.6787(5) 0.3135(3) 0.4870(4) 0.0632(18) Uani 0.505(3) 1 d PDU A 1 C452 C 0.7704(4) 0.2352(4) 0.4665(4) 0.066(2) Uani 0.505(3) 1 d PDU A 1 C453 C 0.8809(6) 0.2474(4) 0.4197(4) 0.068(2) Uani 0.505(3) 1 d PDU A 1 C454 C 0.8567(5) 0.3337(3) 0.4091(4) 0.068(2) Uani 0.505(3) 1 d PDU A 1 C455 C 0.7324(4) 0.3745(4) 0.4508(4) 0.069(2) Uani 0.505(3) 1 d PDU A 1 C456 C 0.5568(6) 0.4488(4) 0.4194(4) 0.056(2) Uani 0.505(3) 1 d PDU A 1 C457 C 0.6727(4) 0.4406(3) 0.4187(5) 0.065(2) Uani 0.505(3) 1 d PDU A 1 C458 C 0.7345(5) 0.4711(4) 0.3441(3) 0.0672(19) Uani 0.505(3) 1 d PDU A 1 C459 C 0.6562(4) 0.4972(5) 0.2986(3) 0.062(2) Uani 0.505(3) 1 d PDU A 1 C460 C 0.5462(6) 0.4841(4) 0.3449(2) 0.051(2) Uani 0.505(3) 1 d PDU A 1 C501 C 0.6452(8) 0.1139(7) 0.2879(6) 0.057(3) Uani 0.495(3) 1 d PDU A 2 C502 C 0.7687(9) 0.0760(7) 0.2751(6) 0.059(3) Uani 0.495(3) 1 d PDU A 2 C503 C 0.8381(8) 0.0878(6) 0.1948(6) 0.060(3) Uani 0.495(3) 1 d PDU A 2 C504 C 0.7537(9) 0.1357(7) 0.1542(7) 0.067(3) Uani 0.495(3) 1 d PDU A 2 C505 C 0.6361(9) 0.1492(7) 0.2117(7) 0.069(3) Uani 0.495(3) 1 d PDU A 2 C506 C 0.5690(9) 0.1502(8) 0.3607(7) 0.064(3) Uani 0.495(3) 1 d PDU A 2 C507 C 0.4745(11) 0.2281(7) 0.3628(8) 0.064(3) Uani 0.495(3) 1 d PDU A 2 C508 C 0.4592(11) 0.2798(7) 0.4280(7) 0.055(3) Uani 0.495(3) 1 d PDU A 2 C509 C 0.5425(9) 0.2342(7) 0.4662(8) 0.060(3) Uani 0.495(3) 1 d PDU A 2 C510 C 0.6084(9) 0.1552(7) 0.4251(6) 0.064(3) Uani 0.495(3) 1 d PDU A 2 C511 C 0.8089(8) 0.0825(6) 0.3374(6) 0.047(2) Uani 0.495(3) 1 d PDU A 2 C512 C 0.7244(8) 0.1230(6) 0.4136(6) 0.060(3) Uani 0.495(3) 1 d PDU A 2 C513 C 0.7825(10) 0.1657(7) 0.4432(7) 0.068(3) Uani 0.495(3) 1 d PDU A 2 C514 C 0.9029(8) 0.1496(6) 0.3864(6) 0.053(2) Uani 0.495(3) 1 d PDU A 2 C515 C 0.9167(8) 0.0972(6) 0.3218(6) 0.051(3) Uani 0.495(3) 1 d PDU A 2 C516 C 0.9421(8) 0.1041(6) 0.1783(6) 0.054(3) Uani 0.495(3) 1 d PDU A 2 C517 C 0.9840(10) 0.1086(8) 0.2440(6) 0.052(3) Uani 0.495(3) 1 d PDU A 2 C518 C 1.0362(12) 0.1721(7) 0.2270(7) 0.050(3) Uani 0.495(3) 1 d PDU A 2 C519 C 1.0280(11) 0.2069(7) 0.1506(7) 0.045(3) Uani 0.495(3) 1 d PDU A 2 C520 C 0.9710(9) 0.1653(7) 0.1210(7) 0.053(3) Uani 0.495(3) 1 d PDU A 2 C521 C 0.7816(9) 0.1926(7) 0.1023(7) 0.064(3) Uani 0.495(3) 1 d PDU A 2 C522 C 0.8907(9) 0.2079(7) 0.0842(7) 0.062(3) Uani 0.495(3) 1 d PDU A 2 C523 C 0.8680(9) 0.2939(6) 0.0750(6) 0.057(3) Uani 0.495(3) 1 d PDU A 2 C524 C 0.7426(9) 0.3314(7) 0.0868(7) 0.063(3) Uani 0.495(3) 1 d PDU A 2 C525 C 0.6885(8) 0.2695(6) 0.1044(5) 0.052(2) Uani 0.495(3) 1 d PDU A 2 C526 C 0.5481(9) 0.2212(7) 0.2144(6) 0.057(3) Uani 0.495(3) 1 d PDU A 2 C527 C 0.5777(8) 0.2813(6) 0.1593(6) 0.048(2) Uani 0.495(3) 1 d PDU A 2 C528 C 0.5089(9) 0.3600(6) 0.2027(7) 0.055(3) Uani 0.495(3) 1 d PDU A 2 C529 C 0.4409(11) 0.3483(7) 0.2846(6) 0.055(3) Uani 0.495(3) 1 d PDU A 2 C530 C 0.4654(12) 0.2616(7) 0.2939(6) 0.061(3) Uani 0.495(3) 1 d PDU A 2 C531 C 0.8192(9) 0.4547(7) 0.2838(7) 0.067(3) Uani 0.495(3) 1 d PDU A 2 C532 C 0.6943(9) 0.4910(7) 0.2967(7) 0.063(3) Uani 0.495(3) 1 d PDU A 2 C533 C 0.6265(8) 0.4802(6) 0.3764(7) 0.069(3) Uani 0.495(3) 1 d PDU A 2 C534 C 0.7092(10) 0.4340(8) 0.4178(7) 0.069(3) Uani 0.495(3) 1 d PDU A 2 C535 C 0.8272(9) 0.4208(7) 0.3602(7) 0.072(3) Uani 0.495(3) 1 d PDU A 2 C536 C 0.8969(9) 0.4178(8) 0.2110(7) 0.064(3) Uani 0.495(3) 1 d PDU A 2 C537 C 0.9906(12) 0.3405(7) 0.2078(8) 0.066(3) Uani 0.495(3) 1 d PDU A 2 C538 C 1.0043(11) 0.2883(6) 0.1429(7) 0.053(3) Uani 0.495(3) 1 d PDU A 2 C539 C 0.9218(9) 0.3338(7) 0.1040(7) 0.057(3) Uani 0.495(3) 1 d PDU A 2 C540 C 0.8560(9) 0.4137(7) 0.1457(7) 0.073(4) Uani 0.495(3) 1 d PDU A 2 C541 C 0.6568(9) 0.4861(6) 0.2338(6) 0.055(3) Uani 0.495(3) 1 d PDU A 2 C542 C 0.7393(9) 0.4479(6) 0.1570(6) 0.070(3) Uani 0.495(3) 1 d PDU A 2 C543 C 0.6807(10) 0.4052(7) 0.1272(7) 0.067(3) Uani 0.495(3) 1 d PDU A 2 C544 C 0.5610(8) 0.4205(6) 0.1839(6) 0.051(2) Uani 0.495(3) 1 d PDU A 2 C545 C 0.5478(9) 0.4710(6) 0.2496(6) 0.059(3) Uani 0.495(3) 1 d PDU A 2 C546 C 0.5243(9) 0.4639(6) 0.3915(6) 0.060(3) Uani 0.495(3) 1 d PDU A 2 C547 C 0.4818(9) 0.4611(7) 0.3269(6) 0.047(3) Uani 0.495(3) 1 d PDU A 2 C548 C 0.4301(12) 0.3974(7) 0.3446(8) 0.052(3) Uani 0.495(3) 1 d PDU A 2 C549 C 0.4389(12) 0.3621(7) 0.4193(7) 0.048(3) Uani 0.495(3) 1 d PDU A 2 C550 C 0.4946(9) 0.4030(7) 0.4502(7) 0.054(3) Uani 0.495(3) 1 d PDU A 2 C551 C 0.6830(9) 0.3770(7) 0.4681(7) 0.067(3) Uani 0.495(3) 1 d PDU A 2 C552 C 0.5741(9) 0.3608(6) 0.4851(7) 0.057(3) Uani 0.495(3) 1 d PDU A 2 C553 C 0.5965(9) 0.2760(6) 0.4938(7) 0.059(3) Uani 0.495(3) 1 d PDU A 2 C554 C 0.7214(9) 0.2385(7) 0.4816(7) 0.069(3) Uani 0.495(3) 1 d PDU A 2 C555 C 0.7763(8) 0.2989(6) 0.4641(5) 0.056(2) Uani 0.495(3) 1 d PDU A 2 C556 C 0.9163(9) 0.3484(7) 0.3544(7) 0.063(3) Uani 0.495(3) 1 d PDU A 2 C557 C 0.8866(8) 0.2877(6) 0.4108(6) 0.052(2) Uani 0.495(3) 1 d PDU A 2 C558 C 0.9554(9) 0.2091(7) 0.3693(7) 0.055(3) Uani 0.495(3) 1 d PDU A 2 C559 C 1.0229(12) 0.2211(7) 0.2893(6) 0.058(3) Uani 0.495(3) 1 d PDU A 2 C560 C 0.9984(13) 0.3063(8) 0.2779(7) 0.069(3) Uani 0.495(3) 1 d PDU A 2 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 Na1 0.0336(9) 0.0421(10) 0.0385(9) 0.0049(8) -0.0139(7) -0.0095(7) O10 0.0375(18) 0.0448(18) 0.0468(19) -0.0061(15) -0.0189(14) 0.0022(14) N3 0.030(2) 0.040(2) 0.047(2) 0.0033(18) -0.0200(17) -0.0104(16) O7 0.0378(18) 0.0445(18) 0.0394(17) 0.0025(14) -0.0125(14) -0.0142(14) O11 0.0401(19) 0.0454(19) 0.055(2) 0.0110(17) -0.0070(16) -0.0110(14) O9 0.0415(19) 0.0487(19) 0.0465(18) -0.0035(15) -0.0237(15) -0.0094(14) O12 0.059(2) 0.057(2) 0.0388(19) 0.0104(17) -0.0034(16) -0.0182(17) N4 0.043(2) 0.049(2) 0.050(2) 0.001(2) -0.0202(19) -0.0062(18) O8 0.0384(19) 0.0487(19) 0.0528(19) -0.0057(16) -0.0176(15) -0.0145(14) C901 0.027(2) 0.044(3) 0.049(3) -0.001(2) -0.013(2) -0.0122(19) C10 0.037(3) 0.044(3) 0.055(3) 0.002(2) -0.011(2) -0.018(2) C14 0.050(3) 0.065(3) 0.057(3) -0.007(3) -0.034(3) -0.012(2) C15 0.036(3) 0.053(3) 0.043(3) 0.005(2) -0.013(2) -0.013(2) C16 0.038(3) 0.048(3) 0.045(3) -0.002(2) -0.019(2) -0.012(2) C18 0.038(3) 0.043(3) 0.052(3) 0.006(2) -0.025(2) -0.005(2) C20 0.056(3) 0.061(3) 0.048(3) 0.004(3) -0.036(3) -0.008(2) C21 0.043(3) 0.047(3) 0.040(3) 0.000(2) -0.017(2) -0.009(2) C25 0.045(3) 0.046(3) 0.052(3) -0.005(2) -0.020(2) 0.000(2) C30 0.039(3) 0.068(3) 0.051(3) -0.018(3) -0.014(2) 0.006(2) C32 0.062(4) 0.065(4) 0.057(3) 0.026(3) -0.012(3) -0.017(3) C36 0.038(3) 0.064(3) 0.059(3) 0.002(3) -0.020(2) -0.023(2) C37 0.066(4) 0.052(3) 0.066(4) 0.023(3) -0.019(3) -0.018(3) C47 0.069(4) 0.076(4) 0.040(3) -0.008(3) -0.023(3) -0.007(3) C49 0.062(4) 0.040(3) 0.075(4) -0.017(3) -0.025(3) -0.008(2) C52 0.052(3) 0.088(4) 0.032(3) 0.006(3) -0.006(2) -0.013(3) C54 0.052(3) 0.055(3) 0.066(3) -0.016(3) -0.025(3) -0.014(2) C82 0.037(3) 0.056(3) 0.070(4) 0.001(3) -0.004(3) -0.021(2) Na2 0.0388(10) 0.0459(10) 0.0421(10) 0.0087(8) -0.0153(8) -0.0184(8) O3 0.050(2) 0.058(2) 0.0432(19) 0.0096(17) -0.0091(16) -0.0245(16) N2 0.034(2) 0.043(2) 0.046(2) 0.0120(18) -0.0198(17) -0.0133(16) O6 0.0419(19) 0.066(2) 0.054(2) -0.0032(18) -0.0078(16) -0.0267(16) O4 0.0379(18) 0.0398(18) 0.058(2) 0.0059(16) -0.0146(15) -0.0134(13) O2 0.046(2) 0.0427(19) 0.059(2) 0.0120(16) -0.0221(17) -0.0095(15) O5 0.0351(18) 0.063(2) 0.0423(18) -0.0008(15) -0.0144(14) -0.0224(15) O1 0.059(2) 0.060(2) 0.058(2) -0.0088(18) -0.0360(18) -0.0015(17) N1 0.035(2) 0.058(2) 0.036(2) 0.0041(19) -0.0100(17) -0.0209(18) C8 0.043(3) 0.053(3) 0.060(3) -0.004(3) -0.018(2) -0.014(2) C9 0.037(3) 0.048(3) 0.051(3) -0.002(2) -0.011(2) -0.012(2) C22 0.029(3) 0.057(3) 0.050(3) 0.002(2) -0.009(2) -0.016(2) C23 0.039(3) 0.071(4) 0.048(3) 0.009(3) -0.017(2) -0.022(2) C26 0.090(4) 0.050(3) 0.057(3) 0.011(3) -0.045(3) -0.018(3) C27 0.071(4) 0.088(4) 0.042(3) 0.008(3) -0.013(3) -0.047(3) C28 0.042(3) 0.052(3) 0.054(3) 0.008(3) -0.025(2) -0.013(2) C33 0.048(3) 0.066(4) 0.045(3) 0.024(3) -0.023(2) -0.028(2) C35 0.067(4) 0.088(4) 0.036(3) 0.003(3) -0.014(2) -0.038(3) C42 0.048(3) 0.064(3) 0.067(4) -0.020(3) -0.033(3) 0.009(2) C44 0.074(4) 0.078(4) 0.072(4) -0.016(3) -0.055(4) 0.009(3) C45 0.042(3) 0.055(3) 0.044(3) -0.001(2) -0.017(2) -0.016(2) C51 0.055(3) 0.041(3) 0.080(4) 0.017(3) -0.012(3) -0.021(2) C53 0.061(3) 0.041(3) 0.078(4) 0.022(3) -0.010(3) -0.028(3) C57 0.042(3) 0.056(3) 0.062(3) -0.004(3) -0.013(2) -0.025(2) C61 0.033(3) 0.073(4) 0.044(3) 0.001(3) -0.004(2) -0.028(2) C66 0.035(3) 0.053(3) 0.047(3) -0.002(2) -0.016(2) -0.021(2) C68 0.036(3) 0.089(4) 0.050(3) -0.016(3) -0.012(2) -0.013(3) C401 0.025(4) 0.060(4) 0.048(4) -0.006(4) 0.002(4) -0.006(4) C402 0.030(4) 0.065(4) 0.053(4) -0.002(4) 0.004(4) -0.023(4) C403 0.045(4) 0.077(5) 0.037(4) 0.011(4) 0.006(3) -0.026(4) C404 0.053(4) 0.075(5) 0.020(3) -0.010(5) 0.000(3) -0.024(4) C405 0.039(4) 0.062(4) 0.043(4) -0.016(4) 0.003(3) -0.012(4) C406 0.019(4) 0.057(4) 0.066(4) 0.000(4) -0.010(4) -0.008(3) C407 0.030(4) 0.041(4) 0.065(4) 0.005(4) -0.009(4) 0.013(3) C408 0.043(4) 0.062(5) 0.069(5) 0.021(4) -0.027(4) 0.000(4) C409 0.038(4) 0.081(4) 0.063(4) 0.011(4) -0.028(3) -0.013(4) C410 0.025(4) 0.076(4) 0.077(4) -0.006(4) -0.020(4) -0.015(4) C411 0.038(4) 0.078(4) 0.084(4) -0.007(4) 0.005(4) -0.038(4) C412 0.035(4) 0.088(4) 0.081(4) -0.010(4) -0.018(4) -0.038(4) C413 0.049(4) 0.086(4) 0.084(5) -0.021(4) -0.018(4) -0.041(4) C414 0.059(4) 0.077(5) 0.097(5) -0.023(5) -0.007(4) -0.049(4) C415 0.055(4) 0.064(4) 0.091(5) -0.003(4) 0.001(4) -0.047(4) C416 0.064(4) 0.061(4) 0.050(4) 0.027(4) 0.007(4) -0.025(3) C417 0.055(4) 0.044(4) 0.075(5) 0.010(3) 0.002(4) -0.037(3) C418 0.053(4) 0.031(3) 0.079(4) 0.022(3) 0.007(4) -0.025(3) C419 0.050(4) 0.052(4) 0.069(4) 0.042(3) -0.014(3) -0.006(3) C420 0.065(4) 0.070(4) 0.038(4) 0.032(4) -0.018(4) -0.018(4) C421 0.060(4) 0.096(4) 0.038(3) -0.007(4) -0.016(3) -0.030(3) C422 0.060(4) 0.108(5) 0.037(4) 0.016(4) -0.027(3) -0.029(4) C423 0.057(4) 0.104(5) 0.055(4) 0.000(4) -0.039(3) -0.018(4) C424 0.057(4) 0.097(5) 0.065(4) -0.022(4) -0.029(3) -0.030(4) C425 0.060(5) 0.101(5) 0.054(4) -0.028(4) -0.018(4) -0.032(4) C426 0.043(4) 0.048(4) 0.059(4) -0.028(3) 0.008(3) -0.013(3) C427 0.060(4) 0.070(4) 0.068(4) -0.037(4) -0.014(4) -0.026(4) C428 0.065(4) 0.050(4) 0.091(4) -0.031(3) -0.007(3) -0.038(3) C429 0.047(4) 0.033(3) 0.085(4) -0.007(4) 0.002(4) -0.012(3) C430 0.033(4) 0.024(3) 0.069(4) -0.002(3) 0.004(3) -0.001(3) C431 0.025(4) 0.060(4) 0.048(4) -0.006(4) 0.002(4) -0.006(4) C432 0.030(4) 0.065(4) 0.053(4) -0.002(4) 0.004(4) -0.023(4) C433 0.045(4) 0.077(5) 0.037(4) 0.011(4) 0.006(3) -0.026(4) C434 0.053(4) 0.075(5) 0.020(3) -0.010(5) 0.000(3) -0.024(4) C435 0.039(4) 0.062(4) 0.043(4) -0.016(4) 0.003(3) -0.012(4) C436 0.019(4) 0.057(4) 0.066(4) 0.000(4) -0.010(4) -0.008(3) C437 0.030(4) 0.041(4) 0.065(4) 0.005(4) -0.009(4) 0.013(3) C438 0.043(4) 0.062(5) 0.069(5) 0.021(4) -0.027(4) 0.000(4) C439 0.038(4) 0.081(4) 0.063(4) 0.011(4) -0.028(3) -0.013(4) C440 0.025(4) 0.076(4) 0.077(4) -0.006(4) -0.020(4) -0.015(4) C441 0.038(4) 0.078(4) 0.084(4) -0.007(4) 0.005(4) -0.038(4) C442 0.035(4) 0.088(4) 0.081(4) -0.010(4) -0.018(4) -0.038(4) C443 0.049(4) 0.086(4) 0.084(5) -0.021(4) -0.018(4) -0.041(4) C444 0.059(4) 0.077(5) 0.097(5) -0.023(5) -0.007(4) -0.049(4) C445 0.055(4) 0.064(4) 0.091(5) -0.003(4) 0.001(4) -0.047(4) C446 0.064(4) 0.061(4) 0.050(4) 0.027(4) 0.007(4) -0.025(3) C447 0.055(4) 0.044(4) 0.075(5) 0.010(3) 0.002(4) -0.037(3) C448 0.053(4) 0.031(3) 0.079(4) 0.022(3) 0.007(4) -0.025(3) C449 0.050(4) 0.052(4) 0.069(4) 0.042(3) -0.014(3) -0.006(3) C450 0.065(4) 0.070(4) 0.038(4) 0.032(4) -0.018(4) -0.018(4) C451 0.060(4) 0.096(4) 0.038(3) -0.007(4) -0.016(3) -0.030(3) C452 0.060(4) 0.108(5) 0.037(4) 0.016(4) -0.027(3) -0.029(4) C453 0.057(4) 0.104(5) 0.055(4) 0.000(4) -0.039(3) -0.018(4) C454 0.057(4) 0.097(5) 0.065(4) -0.022(4) -0.029(3) -0.030(4) C455 0.060(5) 0.101(5) 0.054(4) -0.028(4) -0.018(4) -0.032(4) C456 0.043(4) 0.048(4) 0.059(4) -0.028(3) 0.008(3) -0.013(3) C457 0.060(4) 0.070(4) 0.068(4) -0.037(4) -0.014(4) -0.026(4) C458 0.065(4) 0.050(4) 0.091(4) -0.031(3) -0.007(3) -0.038(3) C459 0.047(4) 0.033(3) 0.085(4) -0.007(4) 0.002(4) -0.012(3) C460 0.033(4) 0.024(3) 0.069(4) -0.002(3) 0.004(3) -0.001(3) C501 0.054(5) 0.057(5) 0.069(6) 0.009(5) -0.021(5) -0.034(4) C502 0.053(5) 0.027(4) 0.082(6) -0.014(5) -0.002(5) -0.016(4) C503 0.057(5) 0.035(4) 0.081(5) -0.028(4) -0.008(5) -0.019(4) C504 0.067(6) 0.065(6) 0.074(6) -0.022(5) -0.025(5) -0.023(5) C505 0.062(6) 0.077(6) 0.081(6) -0.009(6) -0.021(5) -0.039(5) C506 0.047(5) 0.067(5) 0.079(6) -0.001(5) 0.002(5) -0.048(5) C507 0.033(5) 0.074(5) 0.081(6) -0.016(5) 0.006(5) -0.038(4) C508 0.029(5) 0.067(5) 0.052(5) 0.007(5) 0.009(5) -0.020(5) C509 0.051(5) 0.062(5) 0.050(5) 0.012(5) 0.011(5) -0.031(4) C510 0.057(6) 0.062(6) 0.050(6) 0.017(5) 0.009(5) -0.025(5) C511 0.046(5) 0.020(4) 0.073(6) 0.020(4) -0.015(4) -0.020(4) C512 0.058(5) 0.053(5) 0.060(5) 0.037(4) -0.014(4) -0.022(4) C513 0.070(6) 0.089(6) 0.047(5) 0.031(5) -0.031(5) -0.022(5) C514 0.048(5) 0.065(5) 0.055(5) 0.015(5) -0.040(4) -0.010(4) C515 0.049(5) 0.034(5) 0.057(5) 0.026(4) -0.024(4) 0.001(4) C516 0.032(5) 0.037(5) 0.070(6) -0.013(5) 0.001(5) -0.001(4) C517 0.029(5) 0.042(5) 0.063(5) -0.001(5) -0.001(5) 0.001(4) C518 0.023(5) 0.058(5) 0.063(5) 0.006(5) -0.008(4) -0.012(4) C519 0.021(5) 0.056(5) 0.048(5) -0.009(5) 0.003(4) -0.016(4) C520 0.036(5) 0.058(5) 0.044(5) -0.020(5) 0.008(4) -0.010(4) C521 0.061(6) 0.099(6) 0.048(5) -0.030(5) -0.015(4) -0.043(5) C522 0.053(5) 0.088(6) 0.038(5) -0.013(5) -0.001(4) -0.026(5) C523 0.054(5) 0.087(6) 0.027(4) 0.013(5) -0.006(4) -0.031(5) C524 0.059(6) 0.108(6) 0.028(4) 0.024(5) -0.025(4) -0.031(5) C525 0.057(5) 0.089(5) 0.026(4) -0.005(4) -0.024(4) -0.030(4) C526 0.049(5) 0.089(6) 0.056(5) -0.019(5) -0.032(4) -0.032(5) C527 0.048(5) 0.068(6) 0.049(5) 0.001(4) -0.042(4) -0.017(4) C528 0.044(5) 0.076(6) 0.056(5) 0.002(5) -0.042(4) -0.009(4) C529 0.020(5) 0.073(5) 0.076(5) -0.009(5) -0.015(4) -0.017(4) C530 0.034(5) 0.084(6) 0.076(6) -0.013(5) -0.015(5) -0.034(5) C531 0.066(6) 0.058(5) 0.089(6) -0.012(5) -0.017(5) -0.042(5) C532 0.065(6) 0.034(5) 0.089(6) -0.010(5) -0.011(5) -0.030(4) C533 0.055(5) 0.049(5) 0.086(6) -0.022(5) 0.000(5) -0.019(4) C534 0.071(6) 0.074(6) 0.074(6) -0.027(5) -0.028(5) -0.029(5) C535 0.068(5) 0.081(6) 0.086(6) -0.018(5) -0.031(5) -0.040(5) C536 0.052(5) 0.055(5) 0.089(6) -0.007(5) -0.008(5) -0.040(5) C537 0.036(5) 0.079(6) 0.086(6) -0.004(5) -0.003(5) -0.040(5) C538 0.032(5) 0.063(5) 0.056(5) -0.004(5) 0.006(5) -0.029(4) C539 0.044(5) 0.073(6) 0.048(5) 0.010(5) 0.004(4) -0.035(4) C540 0.060(6) 0.064(6) 0.076(6) 0.028(5) 0.008(5) -0.035(5) C541 0.056(5) 0.023(4) 0.084(6) 0.024(5) -0.015(5) -0.025(4) C542 0.061(5) 0.064(5) 0.075(5) 0.037(5) -0.018(5) -0.021(4) C543 0.073(6) 0.072(6) 0.054(6) 0.044(5) -0.032(5) -0.020(5) C544 0.049(5) 0.049(5) 0.066(5) 0.032(5) -0.041(4) -0.013(4) C545 0.057(5) 0.032(5) 0.081(6) 0.022(5) -0.033(5) 0.000(4) C546 0.039(5) 0.043(5) 0.079(6) -0.025(5) 0.002(5) -0.008(4) C547 0.029(5) 0.033(5) 0.071(5) -0.008(5) -0.012(4) -0.006(4) C548 0.018(5) 0.061(5) 0.064(5) -0.007(5) -0.012(4) 0.001(4) C549 0.022(5) 0.062(5) 0.046(5) -0.008(5) -0.003(4) -0.004(4) C550 0.033(5) 0.064(5) 0.046(5) -0.025(5) 0.005(4) -0.007(4) C551 0.058(6) 0.104(6) 0.045(5) -0.026(5) -0.016(5) -0.029(5) C552 0.056(5) 0.079(6) 0.036(5) -0.021(5) -0.007(4) -0.027(5) C553 0.057(5) 0.086(6) 0.031(4) 0.005(5) -0.013(4) -0.023(5) C554 0.061(6) 0.107(6) 0.037(5) 0.018(5) -0.024(5) -0.024(5) C555 0.057(5) 0.093(6) 0.034(4) -0.007(4) -0.031(4) -0.025(4) C556 0.048(5) 0.089(6) 0.073(6) -0.015(5) -0.029(5) -0.035(5) C557 0.051(4) 0.070(5) 0.059(4) -0.011(4) -0.041(4) -0.024(4) C558 0.036(5) 0.081(6) 0.058(5) -0.006(5) -0.037(4) -0.011(4) C559 0.029(5) 0.075(5) 0.073(5) -0.004(5) -0.014(5) -0.022(5) C560 0.037(5) 0.095(6) 0.086(6) -0.004(5) -0.019(5) -0.037(5) _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 Na1 O12 2.486(3) . ? Na1 O8 2.488(3) . ? Na1 O10 2.496(3) . ? Na1 O7 2.603(3) . ? Na1 O11 2.652(4) . ? Na1 O9 2.658(3) . ? Na1 N4 2.712(4) . ? O10 C25 1.406(5) . ? O10 C20 1.417(6) . ? N3 C16 1.451(6) . ? N3 C10 1.462(6) . ? N3 C901 1.463(5) . ? O7 C15 1.419(5) . ? O7 C18 1.420(5) . ? O11 C82 1.404(6) . ? O11 C37 1.417(6) . ? O9 C21 1.422(5) . ? O9 C14 1.423(6) . ? O12 C52 1.398(6) . ? O12 C32 1.415(7) . ? N4 C49 1.442(7) . ? N4 C47 1.458(7) . ? N4 C30 1.472(6) . ? O8 C54 1.393(5) . ? O8 C36 1.431(6) . ? C901 C18 1.502(7) . ? C901 H90A 0.9900 . ? C901 H90B 0.9900 . ? C10 C82 1.525(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C14 C20 1.472(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C36 1.479(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.516(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C25 C30 1.513(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C32 C37 1.450(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C47 C52 1.472(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C49 C54 1.508(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? Na2 O4 2.456(3) . ? Na2 O5 2.459(3) . ? Na2 O2 2.464(4) . ? Na2 O3 2.499(3) . ? Na2 O1 2.583(4) . ? Na2 N1 2.744(4) . ? Na2 O6 2.848(4) . ? Na2 N2 2.981(4) . ? O3 C27 1.402(6) . ? O3 C53 1.441(6) . ? N2 C8 1.445(6) . ? N2 C9 1.457(6) . ? N2 C23 1.462(6) . ? O6 C28 1.417(6) . ? O6 C22 1.426(6) . ? O4 C57 1.401(6) . ? O4 C51 1.429(6) . ? O2 C26 1.410(6) . ? O2 C33 1.437(6) . ? O5 C66 1.420(5) . ? O5 C61 1.430(5) . ? O1 C42 1.405(6) . ? O1 C44 1.419(7) . ? N1 C68 1.451(6) . ? N1 C45 1.455(6) . ? N1 C35 1.468(6) . ? C8 C57 1.531(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C28 1.501(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C22 C61 1.481(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C33 1.463(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C26 C44 1.506(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C35 1.499(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C42 C68 1.494(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C66 1.504(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C51 C53 1.454(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C401 C406 1.368(3) . ? C401 C402 1.448(2) . ? C401 C405 1.449(2) . ? C402 C411 1.368(3) . ? C402 C403 1.449(2) . ? C403 C416 1.368(3) . ? C403 C404 1.450(2) . ? C404 C421 1.367(3) . ? C404 C405 1.449(2) . ? C405 C426 1.368(3) . ? C406 C410 1.449(2) . ? C406 C407 1.450(2) . ? C407 C430 1.367(3) . ? C407 C408 1.448(2) . ? C408 C449 1.367(3) . ? C408 C409 1.448(2) . ? C409 C453 1.367(3) . ? C409 C410 1.448(2) . ? C410 C412 1.367(3) . ? C411 C415 1.449(2) . ? C411 C412 1.449(2) . ? C412 C413 1.449(2) . ? C413 C454 1.367(3) . ? C413 C414 1.449(2) . ? C414 C458 1.367(3) . ? C414 C415 1.449(2) . ? C415 C417 1.367(3) . ? C416 C420 1.449(2) . ? C416 C417 1.449(2) . ? C417 C418 1.449(2) . ? C418 C459 1.368(3) . ? C418 C419 1.448(2) . ? C419 C438 1.367(3) . ? C419 C420 1.449(2) . ? C420 C422 1.368(3) . ? C421 C422 1.449(2) . ? C421 C425 1.449(2) . ? C422 C423 1.449(2) . ? C423 C439 1.368(3) . ? C423 C424 1.449(2) . ? C424 C443 1.367(3) . ? C424 C425 1.449(2) . ? C425 C427 1.367(3) . ? C426 C427 1.449(2) . ? C426 C430 1.450(2) . ? C427 C428 1.449(2) . ? C428 C444 1.367(3) . ? C428 C429 1.448(2) . ? C429 C448 1.367(3) . ? C429 C430 1.448(2) . ? C431 C436 1.367(3) . ? C431 C435 1.449(3) . ? C431 C432 1.449(2) . ? C432 C441 1.367(3) . ? C432 C433 1.449(2) . ? C433 C446 1.367(3) . ? C433 C434 1.449(2) . ? C434 C451 1.366(3) . ? C434 C435 1.449(2) . ? C435 C456 1.367(3) . ? C436 C440 1.449(2) . ? C436 C437 1.450(2) . ? C437 C460 1.368(3) . ? C437 C438 1.449(2) . ? C438 C439 1.449(2) . ? C439 C440 1.449(2) . ? C440 C442 1.367(3) . ? C441 C442 1.449(2) . ? C441 C445 1.449(2) . ? C442 C443 1.449(2) . ? C443 C444 1.449(2) . ? C444 C445 1.448(2) . ? C445 C447 1.367(3) . ? C446 C450 1.448(2) . ? C446 C447 1.449(2) . ? C447 C448 1.449(2) . ? C448 C449 1.448(2) . ? C449 C450 1.448(2) . ? C450 C452 1.367(3) . ? C451 C452 1.448(2) . ? C451 C455 1.449(2) . ? C452 C453 1.448(2) . ? C453 C454 1.448(2) . ? C454 C455 1.449(2) . ? C455 C457 1.367(3) . ? C456 C457 1.448(2) . ? C456 C460 1.449(2) . ? C457 C458 1.449(2) . ? C458 C459 1.448(2) . ? C459 C460 1.448(2) . ? C501 C506 1.361(12) . ? C501 C502 1.445(12) . ? C501 C505 1.470(12) . ? C502 C511 1.407(12) . ? C502 C503 1.432(12) . ? C503 C516 1.388(11) . ? C503 C504 1.505(12) . ? C504 C521 1.351(12) . ? C504 C505 1.447(12) . ? C505 C526 1.375(12) . ? C506 C510 1.428(13) . ? C506 C507 1.485(12) . ? C507 C530 1.341(12) . ? C507 C508 1.446(12) . ? C508 C549 1.380(11) . ? C508 C509 1.455(12) . ? C509 C553 1.379(12) . ? C509 C510 1.448(12) . ? C510 C512 1.354(12) . ? C511 C515 1.424(12) . ? C511 C512 1.451(11) . ? C512 C513 1.454(12) . ? C513 C554 1.338(12) . ? C513 C514 1.464(12) . ? C514 C558 1.382(12) . ? C514 C515 1.452(12) . ? C515 C517 1.385(11) . ? C516 C520 1.465(12) . ? C516 C517 1.469(13) . ? C517 C518 1.444(11) . ? C518 C559 1.381(12) . ? C518 C519 1.468(11) . ? C519 C538 1.360(11) . ? C519 C520 1.430(11) . ? C520 C522 1.394(12) . ? C521 C522 1.439(12) . ? C521 C525 1.465(12) . ? C522 C523 1.441(12) . ? C523 C539 1.369(12) . ? C523 C524 1.470(12) . ? C524 C543 1.367(12) . ? C524 C525 1.433(12) . ? C525 C527 1.370(11) . ? C526 C527 1.432(12) . ? C526 C530 1.488(11) . ? C527 C528 1.463(12) . ? C528 C544 1.394(12) . ? C528 C529 1.447(11) . ? C529 C548 1.363(11) . ? C529 C530 1.450(12) . ? C531 C536 1.367(12) . ? C531 C532 1.457(13) . ? C531 C535 1.464(13) . ? C532 C541 1.387(12) . ? C532 C533 1.412(12) . ? C533 C546 1.371(12) . ? C533 C534 1.491(13) . ? C534 C551 1.333(12) . ? C534 C535 1.451(12) . ? C535 C556 1.378(12) . ? C536 C540 1.453(13) . ? C536 C537 1.470(12) . ? C537 C560 1.361(12) . ? C537 C538 1.452(12) . ? C538 C539 1.455(12) . ? C539 C540 1.464(12) . ? C540 C542 1.366(12) . ? C541 C542 1.441(12) . ? C541 C545 1.442(12) . ? C542 C543 1.461(13) . ? C543 C544 1.458(12) . ? C544 C545 1.447(12) . ? C545 C547 1.368(11) . ? C546 C547 1.447(13) . ? C546 C550 1.478(12) . ? C547 C548 1.442(11) . ? C548 C549 1.447(11) . ? C549 C550 1.421(11) . ? C550 C552 1.362(12) . ? C551 C552 1.448(12) . ? C551 C555 1.474(12) . ? C552 C553 1.421(12) . ? C553 C554 1.462(12) . ? C554 C555 1.418(12) . ? C555 C557 1.356(11) . ? C556 C557 1.452(12) . ? C556 C560 1.458(12) . ? C557 C558 1.449(12) . ? C558 C559 1.421(12) . ? C559 C560 1.431(12) . ? 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 O12 Na1 O8 104.89(13) . . ? O12 Na1 O10 102.85(12) . . ? O8 Na1 O10 102.07(12) . . ? O12 Na1 O7 98.10(12) . . ? O8 Na1 O7 65.17(10) . . ? O10 Na1 O7 157.85(12) . . ? O12 Na1 O11 64.92(12) . . ? O8 Na1 O11 161.68(13) . . ? O10 Na1 O11 95.25(12) . . ? O7 Na1 O11 100.10(11) . . ? O12 Na1 O9 159.29(13) . . ? O8 Na1 O9 94.52(11) . . ? O10 Na1 O9 65.31(10) . . ? O7 Na1 O9 96.57(10) . . ? O11 Na1 O9 98.14(11) . . ? O12 Na1 N4 65.13(12) . . ? O8 Na1 N4 64.88(12) . . ? O10 Na1 N4 64.62(12) . . ? O7 Na1 N4 119.61(12) . . ? O11 Na1 N4 118.91(12) . . ? O9 Na1 N4 118.93(12) . . ? C25 O10 C20 110.9(4) . . ? C25 O10 Na1 124.3(3) . . ? C20 O10 Na1 117.9(3) . . ? C16 N3 C10 111.7(4) . . ? C16 N3 C901 111.1(3) . . ? C10 N3 C901 110.9(3) . . ? C15 O7 C18 113.9(3) . . ? C15 O7 Na1 103.1(2) . . ? C18 O7 Na1 121.0(3) . . ? C82 O11 C37 113.3(4) . . ? C82 O11 Na1 120.4(3) . . ? C37 O11 Na1 102.7(3) . . ? C21 O9 C14 113.6(3) . . ? C21 O9 Na1 120.9(3) . . ? C14 O9 Na1 100.3(3) . . ? C52 O12 C32 111.5(4) . . ? C52 O12 Na1 122.1(3) . . ? C32 O12 Na1 118.6(3) . . ? C49 N4 C47 113.2(5) . . ? C49 N4 C30 111.6(4) . . ? C47 N4 C30 110.8(4) . . ? C49 N4 Na1 107.1(3) . . ? C47 N4 Na1 106.4(3) . . ? C30 N4 Na1 107.5(3) . . ? C54 O8 C36 111.9(3) . . ? C54 O8 Na1 123.3(3) . . ? C36 O8 Na1 117.7(2) . . ? N3 C901 C18 111.4(4) . . ? N3 C901 H90A 109.4 . . ? C18 C901 H90A 109.4 . . ? N3 C901 H90B 109.4 . . ? C18 C901 H90B 109.4 . . ? H90A C901 H90B 108.0 . . ? N3 C10 C82 111.5(4) . . ? N3 C10 H10A 109.3 . . ? C82 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C82 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? O9 C14 C20 109.6(4) . . ? O9 C14 H14A 109.7 . . ? C20 C14 H14A 109.7 . . ? O9 C14 H14B 109.7 . . ? C20 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? O7 C15 C36 108.1(4) . . ? O7 C15 H15A 110.1 . . ? C36 C15 H15A 110.1 . . ? O7 C15 H15B 110.1 . . ? C36 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N3 C16 C21 112.6(4) . . ? N3 C16 H16A 109.1 . . ? C21 C16 H16A 109.1 . . ? N3 C16 H16B 109.1 . . ? C21 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? O7 C18 C901 112.1(4) . . ? O7 C18 H18A 109.2 . . ? C901 C18 H18A 109.2 . . ? O7 C18 H18B 109.2 . . ? C901 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? O10 C20 C14 108.2(4) . . ? O10 C20 H20A 110.1 . . ? C14 C20 H20A 110.1 . . ? O10 C20 H20B 110.1 . . ? C14 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O9 C21 C16 113.1(4) . . ? O9 C21 H21A 109.0 . . ? C16 C21 H21A 109.0 . . ? O9 C21 H21B 109.0 . . ? C16 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O10 C25 C30 108.5(4) . . ? O10 C25 H25A 110.0 . . ? C30 C25 H25A 110.0 . . ? O10 C25 H25B 110.0 . . ? C30 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? N4 C30 C25 112.8(4) . . ? N4 C30 H30A 109.0 . . ? C25 C30 H30A 109.0 . . ? N4 C30 H30B 109.0 . . ? C25 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? O12 C32 C37 109.5(4) . . ? O12 C32 H32A 109.8 . . ? C37 C32 H32A 109.8 . . ? O12 C32 H32B 109.8 . . ? C37 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? O8 C36 C15 108.6(4) . . ? O8 C36 H36A 110.0 . . ? C15 C36 H36A 110.0 . . ? O8 C36 H36B 110.0 . . ? C15 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O11 C37 C32 110.3(4) . . ? O11 C37 H37A 109.6 . . ? C32 C37 H37A 109.6 . . ? O11 C37 H37B 109.6 . . ? C32 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? N4 C47 C52 113.4(5) . . ? N4 C47 H47A 108.9 . . ? C52 C47 H47A 108.9 . . ? N4 C47 H47B 108.9 . . ? C52 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? N4 C49 C54 113.7(4) . . ? N4 C49 H49A 108.8 . . ? C54 C49 H49A 108.8 . . ? N4 C49 H49B 108.8 . . ? C54 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? O12 C52 C47 110.6(4) . . ? O12 C52 H52A 109.5 . . ? C47 C52 H52A 109.5 . . ? O12 C52 H52B 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? O8 C54 C49 108.7(4) . . ? O8 C54 H54A 109.9 . . ? C49 C54 H54A 109.9 . . ? O8 C54 H54B 109.9 . . ? C49 C54 H54B 109.9 . . ? H54A C54 H54B 108.3 . . ? O11 C82 C10 114.2(4) . . ? O11 C82 H82A 108.7 . . ? C10 C82 H82A 108.7 . . ? O11 C82 H82B 108.7 . . ? C10 C82 H82B 108.7 . . ? H82A C82 H82B 107.6 . . ? O4 Na2 O5 162.16(13) . . ? O4 Na2 O2 90.98(12) . . ? O5 Na2 O2 93.50(12) . . ? O4 Na2 O3 66.96(12) . . ? O5 Na2 O3 111.94(13) . . ? O2 Na2 O3 153.65(14) . . ? O4 Na2 O1 98.16(12) . . ? O5 Na2 O1 99.52(13) . . ? O2 Na2 O1 67.79(11) . . ? O3 Na2 O1 100.00(13) . . ? O4 Na2 N1 124.26(12) . . ? O5 Na2 N1 66.61(11) . . ? O2 Na2 N1 123.01(13) . . ? O3 Na2 N1 65.33(11) . . ? O1 Na2 N1 64.35(12) . . ? O4 Na2 O6 98.81(11) . . ? O5 Na2 O6 63.43(11) . . ? O2 Na2 O6 109.25(11) . . ? O3 Na2 O6 89.07(11) . . ? O1 Na2 O6 162.83(13) . . ? N1 Na2 O6 107.45(12) . . ? O4 Na2 N2 65.22(11) . . ? O5 Na2 N2 102.10(11) . . ? O2 Na2 N2 61.27(11) . . ? O3 Na2 N2 116.78(12) . . ? O1 Na2 N2 125.28(12) . . ? N1 Na2 N2 167.36(12) . . ? O6 Na2 N2 60.90(10) . . ? C27 O3 C53 111.3(4) . . ? C27 O3 Na2 120.4(3) . . ? C53 O3 Na2 114.5(3) . . ? C8 N2 C9 111.5(4) . . ? C8 N2 C23 111.7(4) . . ? C9 N2 C23 111.0(3) . . ? C8 N2 Na2 104.2(3) . . ? C9 N2 Na2 111.6(3) . . ? C23 N2 Na2 106.5(3) . . ? C28 O6 C22 115.0(3) . . ? C28 O6 Na2 114.8(3) . . ? C22 O6 Na2 110.7(3) . . ? C57 O4 C51 112.8(4) . . ? C57 O4 Na2 117.1(3) . . ? C51 O4 Na2 106.6(3) . . ? C26 O2 C33 115.3(4) . . ? C26 O2 Na2 111.3(3) . . ? C33 O2 Na2 117.7(3) . . ? C66 O5 C61 112.8(3) . . ? C66 O5 Na2 112.5(2) . . ? C61 O5 Na2 113.9(3) . . ? C42 O1 C44 113.0(4) . . ? C42 O1 Na2 115.4(3) . . ? C44 O1 Na2 109.9(3) . . ? C68 N1 C45 111.4(4) . . ? C68 N1 C35 111.4(4) . . ? C45 N1 C35 110.1(4) . . ? C68 N1 Na2 109.3(3) . . ? C45 N1 Na2 106.9(2) . . ? C35 N1 Na2 107.6(3) . . ? N2 C8 C57 111.8(4) . . ? N2 C8 H8A 109.3 . . ? C57 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C57 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? N2 C9 C28 112.5(4) . . ? N2 C9 H9A 109.1 . . ? C28 C9 H9A 109.1 . . ? N2 C9 H9B 109.1 . . ? C28 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? O6 C22 C61 112.4(4) . . ? O6 C22 H22A 109.1 . . ? C61 C22 H22A 109.1 . . ? O6 C22 H22B 109.1 . . ? C61 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? N2 C23 C33 113.6(4) . . ? N2 C23 H23A 108.9 . . ? C33 C23 H23A 108.9 . . ? N2 C23 H23B 108.9 . . ? C33 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O2 C26 C44 106.7(4) . . ? O2 C26 H26A 110.4 . . ? C44 C26 H26A 110.4 . . ? O2 C26 H26B 110.4 . . ? C44 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? O3 C27 C35 109.0(4) . . ? O3 C27 H27A 109.9 . . ? C35 C27 H27A 109.9 . . ? O3 C27 H27B 109.9 . . ? C35 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O6 C28 C9 113.8(4) . . ? O6 C28 H28A 108.8 . . ? C9 C28 H28A 108.8 . . ? O6 C28 H28B 108.8 . . ? C9 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? O2 C33 C23 107.7(4) . . ? O2 C33 H33A 110.2 . . ? C23 C33 H33A 110.2 . . ? O2 C33 H33B 110.2 . . ? C23 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? N1 C35 C27 112.9(4) . . ? N1 C35 H35A 109.0 . . ? C27 C35 H35A 109.0 . . ? N1 C35 H35B 109.0 . . ? C27 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? O1 C42 C68 107.1(5) . . ? O1 C42 H42A 110.3 . . ? C68 C42 H42A 110.3 . . ? O1 C42 H42B 110.3 . . ? C68 C42 H42B 110.3 . . ? H42A C42 H42B 108.5 . . ? O1 C44 C26 112.4(5) . . ? O1 C44 H44A 109.1 . . ? C26 C44 H44A 109.1 . . ? O1 C44 H44B 109.1 . . ? C26 C44 H44B 109.1 . . ? H44A C44 H44B 107.9 . . ? N1 C45 C66 112.0(4) . . ? N1 C45 H45A 109.2 . . ? C66 C45 H45A 109.2 . . ? N1 C45 H45B 109.2 . . ? C66 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? O4 C51 C53 108.4(4) . . ? O4 C51 H51A 110.0 . . ? C53 C51 H51A 110.0 . . ? O4 C51 H51B 110.0 . . ? C53 C51 H51B 110.0 . . ? H51A C51 H51B 108.4 . . ? O3 C53 C51 107.4(4) . . ? O3 C53 H53A 110.2 . . ? C51 C53 H53A 110.2 . . ? O3 C53 H53B 110.2 . . ? C51 C53 H53B 110.2 . . ? H53A C53 H53B 108.5 . . ? O4 C57 C8 114.3(4) . . ? O4 C57 H57A 108.7 . . ? C8 C57 H57A 108.7 . . ? O4 C57 H57B 108.7 . . ? C8 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? O5 C61 C22 113.0(4) . . ? O5 C61 H61A 109.0 . . ? C22 C61 H61A 109.0 . . ? O5 C61 H61B 109.0 . . ? C22 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? O5 C66 C45 107.3(4) . . ? O5 C66 H66A 110.2 . . ? C45 C66 H66A 110.2 . . ? O5 C66 H66B 110.2 . . ? C45 C66 H66B 110.2 . . ? H66A C66 H66B 108.5 . . ? N1 C68 C42 112.2(4) . . ? N1 C68 H68A 109.2 . . ? C42 C68 H68A 109.2 . . ? N1 C68 H68B 109.2 . . ? C42 C68 H68B 109.2 . . ? H68A C68 H68B 107.9 . . ? C406 C401 C402 120.00(11) . . ? C406 C401 C405 120.02(11) . . ? C402 C401 C405 107.2(10) . . ? C411 C402 C401 120.01(11) . . ? C411 C402 C403 119.99(11) . . ? C401 C402 C403 109.1(9) . . ? C416 C403 C402 120.00(11) . . ? C416 C403 C404 119.95(11) . . ? C402 C403 C404 107.1(8) . . ? C421 C404 C405 120.01(11) . . ? C421 C404 C403 119.97(11) . . ? C405 C404 C403 108.4(7) . . ? C426 C405 C401 120.02(11) . . ? C426 C405 C404 120.00(11) . . ? C401 C405 C404 108.2(8) . . ? C401 C406 C410 119.97(11) . . ? C401 C406 C407 119.97(11) . . ? C410 C406 C407 107.5(10) . . ? C430 C407 C408 119.98(11) . . ? C430 C407 C406 120.01(11) . . ? C408 C407 C406 108.1(9) . . ? C449 C408 C407 120.02(11) . . ? C449 C408 C409 120.00(11) . . ? C407 C408 C409 108.3(8) . . ? C453 C409 C410 119.99(11) . . ? C453 C409 C408 119.96(11) . . ? C410 C409 C408 107.4(9) . . ? C412 C410 C409 120.00(11) . . ? C412 C410 C406 120.01(11) . . ? C409 C410 C406 108.6(10) . . ? C402 C411 C415 119.99(11) . . ? C402 C411 C412 119.97(11) . . ? C415 C411 C412 107.7(10) . . ? C410 C412 C411 120.01(11) . . ? C410 C412 C413 119.98(12) . . ? C411 C412 C413 106.7(10) . . ? C454 C413 C414 119.95(11) . . ? C454 C413 C412 119.98(11) . . ? C414 C413 C412 110.4(9) . . ? C458 C414 C415 120.00(11) . . ? C458 C414 C413 119.98(11) . . ? C415 C414 C413 105.3(8) . . ? C417 C415 C414 119.96(11) . . ? C417 C415 C411 120.00(11) . . ? C414 C415 C411 109.8(9) . . ? C403 C416 C420 120.05(11) . . ? C403 C416 C417 120.00(11) . . ? C420 C416 C417 107.5(6) . . ? C415 C417 C418 119.98(11) . . ? C415 C417 C416 120.00(11) . . ? C418 C417 C416 109.8(6) . . ? C459 C418 C419 119.94(12) . . ? C459 C418 C417 119.97(12) . . ? C419 C418 C417 105.5(6) . . ? C438 C419 C418 119.98(11) . . ? C438 C419 C420 120.04(11) . . ? C418 C419 C420 110.2(6) . . ? C422 C420 C416 119.99(11) . . ? C422 C420 C419 119.91(11) . . ? C416 C420 C419 106.9(6) . . ? C404 C421 C422 120.07(11) . . ? C404 C421 C425 119.99(11) . . ? C422 C421 C425 109.3(6) . . ? C420 C422 C423 119.97(11) . . ? C420 C422 C421 119.95(11) . . ? C423 C422 C421 108.8(7) . . ? C439 C423 C422 120.04(11) . . ? C439 C423 C424 119.96(12) . . ? C422 C423 C424 105.4(7) . . ? C443 C424 C423 119.98(11) . . ? C443 C424 C425 119.96(11) . . ? C423 C424 C425 111.4(6) . . ? C427 C425 C424 119.97(12) . . ? C427 C425 C421 119.97(11) . . ? C424 C425 C421 105.0(7) . . ? C405 C426 C427 119.96(11) . . ? C405 C426 C430 119.94(11) . . ? C427 C426 C430 107.4(6) . . ? C425 C427 C426 120.02(11) . . ? C425 C427 C428 119.95(11) . . ? C426 C427 C428 108.2(6) . . ? C444 C428 C429 120.00(11) . . ? C444 C428 C427 120.00(11) . . ? C429 C428 C427 108.2(6) . . ? C448 C429 C428 120.00(11) . . ? C448 C429 C430 120.03(11) . . ? C428 C429 C430 107.4(6) . . ? C407 C430 C429 119.98(11) . . ? C407 C430 C426 120.02(11) . . ? C429 C430 C426 108.7(6) . . ? C436 C431 C435 120.07(17) . . ? C436 C431 C432 120.01(11) . . ? C435 C431 C432 106.9(10) . . ? C441 C432 C433 119.99(11) . . ? C441 C432 C431 119.98(11) . . ? C433 C432 C431 107.9(9) . . ? C446 C433 C432 120.01(11) . . ? C446 C433 C434 119.93(11) . . ? C432 C433 C434 109.2(8) . . ? C451 C434 C433 119.98(11) . . ? C451 C434 C435 119.96(11) . . ? C433 C434 C435 106.0(8) . . ? C456 C435 C431 119.90(17) . . ? C456 C435 C434 119.95(11) . . ? C431 C435 C434 109.9(8) . . ? C431 C436 C440 120.00(11) . . ? C431 C436 C437 119.97(12) . . ? C440 C436 C437 105.6(10) . . ? C460 C437 C438 119.94(11) . . ? C460 C437 C436 119.89(14) . . ? C438 C437 C436 110.3(8) . . ? C419 C438 C437 119.96(12) . . ? C419 C438 C439 119.99(11) . . ? C437 C438 C439 106.7(8) . . ? C423 C439 C440 119.97(11) . . ? C423 C439 C438 119.94(11) . . ? C440 C439 C438 107.8(9) . . ? C442 C440 C436 119.95(11) . . ? C442 C440 C439 119.98(11) . . ? C436 C440 C439 109.6(10) . . ? C432 C441 C442 120.00(11) . . ? C432 C441 C445 119.98(11) . . ? C442 C441 C445 109.0(10) . . ? C440 C442 C441 120.00(12) . . ? C440 C442 C443 119.97(12) . . ? C441 C442 C443 106.3(10) . . ? C424 C443 C444 119.98(11) . . ? C424 C443 C442 119.97(11) . . ? C444 C443 C442 109.6(9) . . ? C428 C444 C445 120.00(11) . . ? C428 C444 C443 120.01(11) . . ? C445 C444 C443 107.0(8) . . ? C447 C445 C444 120.00(11) . . ? C447 C445 C441 120.00(11) . . ? C444 C445 C441 107.9(9) . . ? C433 C446 C450 120.02(11) . . ? C433 C446 C447 119.97(11) . . ? C450 C446 C447 106.8(6) . . ? C445 C447 C448 119.97(11) . . ? C445 C447 C446 119.99(11) . . ? C448 C447 C446 109.9(6) . . ? C429 C448 C449 119.98(11) . . ? C429 C448 C447 119.99(11) . . ? C449 C448 C447 106.0(6) . . ? C408 C449 C448 119.98(11) . . ? C408 C449 C450 120.03(11) . . ? C448 C449 C450 109.3(6) . . ? C452 C450 C446 120.01(11) . . ? C452 C450 C449 119.96(11) . . ? C446 C450 C449 107.9(6) . . ? C434 C451 C452 120.05(11) . . ? C434 C451 C455 120.07(11) . . ? C452 C451 C455 107.4(6) . . ? C450 C452 C453 120.02(11) . . ? C450 C452 C451 119.95(11) . . ? C453 C452 C451 108.8(6) . . ? C409 C453 C452 120.02(11) . . ? C409 C453 C454 120.00(11) . . ? C452 C453 C454 107.4(7) . . ? C413 C454 C453 120.00(11) . . ? C413 C454 C455 120.00(11) . . ? C453 C454 C455 108.2(6) . . ? C457 C455 C454 120.00(11) . . ? C457 C455 C451 119.95(11) . . ? C454 C455 C451 108.2(6) . . ? C435 C456 C457 120.04(11) . . ? C435 C456 C460 120.07(16) . . ? C457 C456 C460 108.1(6) . . ? C455 C457 C456 119.99(11) . . ? C455 C457 C458 119.97(11) . . ? C456 C457 C458 108.4(6) . . ? C414 C458 C459 119.99(11) . . ? C414 C458 C457 120.00(11) . . ? C459 C458 C457 107.2(6) . . ? C418 C459 C460 120.00(11) . . ? C418 C459 C458 119.95(11) . . ? C460 C459 C458 108.9(6) . . ? C437 C460 C459 120.02(11) . . ? C437 C460 C456 119.98(11) . . ? C459 C460 C456 107.4(6) . . ? C506 C501 C502 120.1(9) . . ? C506 C501 C505 121.9(10) . . ? C502 C501 C505 107.4(8) . . ? C511 C502 C503 117.5(9) . . ? C511 C502 C501 118.6(8) . . ? C503 C502 C501 110.1(9) . . ? C516 C503 C502 121.6(10) . . ? C516 C503 C504 118.7(9) . . ? C502 C503 C504 106.8(8) . . ? C521 C504 C505 122.1(10) . . ? C521 C504 C503 119.3(10) . . ? C505 C504 C503 107.3(9) . . ? C526 C505 C504 120.2(10) . . ? C526 C505 C501 118.9(9) . . ? C504 C505 C501 108.4(9) . . ? C501 C506 C510 121.7(9) . . ? C501 C506 C507 118.7(11) . . ? C510 C506 C507 107.3(9) . . ? C530 C507 C508 118.9(9) . . ? C530 C507 C506 120.3(12) . . ? C508 C507 C506 108.4(9) . . ? C549 C508 C507 120.9(9) . . ? C549 C508 C509 119.3(12) . . ? C507 C508 C509 106.7(8) . . ? C553 C509 C510 120.8(10) . . ? C553 C509 C508 117.9(11) . . ? C510 C509 C508 109.2(9) . . ? C512 C510 C506 119.3(9) . . ? C512 C510 C509 119.0(10) . . ? C506 C510 C509 108.5(9) . . ? C502 C511 C515 121.9(9) . . ? C502 C511 C512 119.1(9) . . ? C515 C511 C512 109.2(9) . . ? C510 C512 C511 121.1(10) . . ? C510 C512 C513 121.0(9) . . ? C511 C512 C513 106.5(8) . . ? C554 C513 C512 120.0(10) . . ? C554 C513 C514 120.3(10) . . ? C512 C513 C514 108.9(9) . . ? C558 C514 C515 119.9(9) . . ? C558 C514 C513 121.4(9) . . ? C515 C514 C513 106.3(8) . . ? C517 C515 C511 120.6(9) . . ? C517 C515 C514 118.1(9) . . ? C511 C515 C514 109.0(8) . . ? C503 C516 C520 120.9(9) . . ? C503 C516 C517 120.0(9) . . ? C520 C516 C517 107.6(8) . . ? C515 C517 C518 121.3(11) . . ? C515 C517 C516 118.4(9) . . ? C518 C517 C516 107.5(8) . . ? C559 C518 C517 119.9(12) . . ? C559 C518 C519 120.4(8) . . ? C517 C518 C519 108.3(8) . . ? C538 C519 C520 120.1(12) . . ? C538 C519 C518 118.9(8) . . ? C520 C519 C518 108.2(8) . . ? C522 C520 C519 120.3(11) . . ? C522 C520 C516 118.5(9) . . ? C519 C520 C516 108.3(8) . . ? C504 C521 C522 121.7(10) . . ? C504 C521 C525 118.3(9) . . ? C522 C521 C525 109.1(9) . . ? C520 C522 C521 120.9(10) . . ? C520 C522 C523 119.1(10) . . ? C521 C522 C523 107.9(9) . . ? C539 C523 C522 120.6(10) . . ? C539 C523 C524 119.4(9) . . ? C522 C523 C524 107.5(9) . . ? C543 C524 C525 118.3(9) . . ? C543 C524 C523 119.8(10) . . ? C525 C524 C523 108.8(9) . . ? C527 C525 C524 122.8(9) . . ? C527 C525 C521 118.9(9) . . ? C524 C525 C521 106.6(8) . . ? C505 C526 C527 117.7(9) . . ? C505 C526 C530 119.4(11) . . ? C527 C526 C530 109.3(8) . . ? C525 C527 C526 122.8(9) . . ? C525 C527 C528 120.1(9) . . ? C526 C527 C528 106.4(8) . . ? C544 C528 C529 122.0(11) . . ? C544 C528 C527 116.7(9) . . ? C529 C528 C527 109.9(8) . . ? C548 C529 C528 118.2(12) . . ? C548 C529 C530 120.9(9) . . ? C528 C529 C530 107.6(8) . . ? C507 C530 C529 120.9(9) . . ? C507 C530 C526 120.8(12) . . ? C529 C530 C526 106.8(8) . . ? C536 C531 C532 120.5(10) . . ? C536 C531 C535 122.2(11) . . ? C532 C531 C535 106.5(9) . . ? C541 C532 C533 120.0(10) . . ? C541 C532 C531 118.3(9) . . ? C533 C532 C531 110.2(10) . . ? C546 C533 C532 119.9(10) . . ? C546 C533 C534 119.4(10) . . ? C532 C533 C534 107.7(9) . . ? C551 C534 C535 121.4(10) . . ? C551 C534 C533 119.4(10) . . ? C535 C534 C533 106.8(9) . . ? C556 C535 C534 121.4(10) . . ? C556 C535 C531 115.9(10) . . ? C534 C535 C531 108.8(9) . . ? C531 C536 C540 120.4(10) . . ? C531 C536 C537 120.1(12) . . ? C540 C536 C537 107.1(9) . . ? C560 C537 C538 118.4(9) . . ? C560 C537 C536 119.2(13) . . ? C538 C537 C536 108.9(9) . . ? C519 C538 C537 121.2(9) . . ? C519 C538 C539 120.6(12) . . ? C537 C538 C539 107.3(8) . . ? C523 C539 C538 119.3(11) . . ? C523 C539 C540 120.7(9) . . ? C538 C539 C540 108.5(9) . . ? C542 C540 C536 119.6(10) . . ? C542 C540 C539 119.6(10) . . ? C536 C540 C539 108.1(9) . . ? C532 C541 C542 121.0(9) . . ? C532 C541 C545 120.2(9) . . ? C542 C541 C545 109.0(9) . . ? C540 C542 C541 120.2(10) . . ? C540 C542 C543 120.2(10) . . ? C541 C542 C543 106.5(9) . . ? C524 C543 C544 120.0(10) . . ? C524 C543 C542 120.4(10) . . ? C544 C543 C542 109.2(9) . . ? C528 C544 C545 117.9(9) . . ? C528 C544 C543 121.9(9) . . ? C545 C544 C543 106.4(9) . . ? C547 C545 C541 119.6(9) . . ? C547 C545 C544 120.3(9) . . ? C541 C545 C544 108.9(8) . . ? C533 C546 C547 120.8(9) . . ? C533 C546 C550 120.2(10) . . ? C547 C546 C550 108.8(8) . . ? C545 C547 C548 120.4(10) . . ? C545 C547 C546 119.3(9) . . ? C548 C547 C546 106.4(8) . . ? C529 C548 C547 121.1(12) . . ? C529 C548 C549 118.7(8) . . ? C547 C548 C549 109.3(8) . . ? C508 C549 C550 120.8(12) . . ? C508 C549 C548 119.6(8) . . ? C550 C549 C548 108.7(8) . . ? C552 C550 C549 120.4(11) . . ? C552 C550 C546 118.3(9) . . ? C549 C550 C546 106.8(8) . . ? C534 C551 C552 121.2(10) . . ? C534 C551 C555 118.8(9) . . ? C552 C551 C555 108.0(9) . . ? C550 C552 C553 119.3(9) . . ? C550 C552 C551 121.4(10) . . ? C553 C552 C551 108.3(9) . . ? C509 C553 C552 122.1(10) . . ? C509 C553 C554 118.6(9) . . ? C552 C553 C554 107.5(9) . . ? C513 C554 C555 117.9(10) . . ? C513 C554 C553 120.6(10) . . ? C555 C554 C553 109.5(9) . . ? C557 C555 C554 124.1(9) . . ? C557 C555 C551 119.3(9) . . ? C554 C555 C551 106.5(9) . . ? C535 C556 C557 116.4(9) . . ? C535 C556 C560 123.3(11) . . ? C557 C556 C560 107.8(9) . . ? C555 C557 C558 119.2(9) . . ? C555 C557 C556 122.7(9) . . ? C558 C557 C556 107.0(8) . . ? C514 C558 C559 121.6(11) . . ? C514 C558 C557 117.1(8) . . ? C559 C558 C557 108.6(8) . . ? C518 C559 C558 119.2(12) . . ? C518 C559 C560 118.3(9) . . ? C558 C559 C560 109.1(8) . . ? C537 C560 C559 122.7(9) . . ? C537 C560 C556 119.4(12) . . ? C559 C560 C556 107.4(9) . . ? _diffrn_measured_fraction_theta_max 0.724 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.724 _refine_diff_density_max 0.369 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.061 data_C60_2DB18crown6_Na_BN_DCB _database_code_depnum_ccdc_archive 'CCDC 894602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60, 2(C34 H34 N2 Na O6), C6 H4 Cl2, C7 H5 N ' _chemical_formula_sum 'C141 H77 Cl2 N5 Na2 O12' _chemical_formula_weight 2149.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 26.826(3) _cell_length_b 16.3245(14) _cell_length_c 24.427(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.108(7) _cell_angle_gamma 90.00 _cell_volume 10681.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 175(2) _cell_measurement_reflns_used 11416 _cell_measurement_theta_min 1.5173 _cell_measurement_theta_max 27.0408 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4440 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_T_min 0.9190 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 175(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_detector_area_resol_mean 10.4752 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46143 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.10 _reflns_number_total 20261 _reflns_number_gt 10013 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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 'calc w=1/[\s^2^(Fo^2^)+(0.1450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(2) _refine_ls_number_reflns 20261 _refine_ls_number_parameters 1437 _refine_ls_number_restraints 1225 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2401 _refine_ls_wR_factor_gt 0.1981 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1B C 0.3507(3) 0.8673(4) 0.1143(3) 0.072(3) Uani 1 1 d G . . H1B H 0.3220 0.8381 0.1006 0.086 Uiso 1 1 calc R . . C4B C 0.3968(3) 0.8284(3) 0.1189(3) 0.070(3) Uani 1 1 d G . . H4B H 0.3997 0.7727 0.1082 0.084 Uiso 1 1 calc R . . C3B C 0.4388(3) 0.8711(3) 0.1389(3) 0.051(2) Uani 1 1 d G . . H3B H 0.4703 0.8445 0.1420 0.061 Uiso 1 1 calc R . . C2B C 0.4346(3) 0.9526(3) 0.1545(3) 0.041(2) Uani 1 1 d G . . C19B C 0.3884(3) 0.9915(3) 0.1499(3) 0.046(2) Uani 1 1 d G . . C20B C 0.3465(3) 0.9488(4) 0.1299(3) 0.054(2) Uani 1 1 d G . . H20B H 0.3149 0.9754 0.1268 0.065 Uiso 1 1 calc R . . C9B C 0.4839(3) 1.1704(3) 0.3854(2) 0.041(2) Uani 1 1 d G . . C10B C 0.5002(3) 1.1465(4) 0.4380(3) 0.051(2) Uani 1 1 d G . . H10B H 0.5303 1.1161 0.4435 0.062 Uiso 1 1 calc R . . C11B C 0.4726(3) 1.1671(4) 0.4825(2) 0.067(3) Uani 1 1 d G . . H11B H 0.4838 1.1507 0.5184 0.080 Uiso 1 1 calc R . . C12B C 0.4287(3) 1.2116(4) 0.4745(2) 0.059(2) Uani 1 1 d G . . H12B H 0.4098 1.2257 0.5049 0.071 Uiso 1 1 calc R . . C13B C 0.4123(3) 1.2356(4) 0.4219(3) 0.061(3) Uani 1 1 d G . . H13B H 0.3823 1.2660 0.4165 0.074 Uiso 1 1 calc R . . C14B C 0.4399(3) 1.2150(4) 0.3774(2) 0.045(2) Uani 1 1 d G . . Na1 Na 0.4507(2) 1.12232(19) 0.2520(2) 0.0456(8) Uani 1 1 d . . . O9 O 0.3691(3) 1.2040(3) 0.2321(3) 0.0497(16) Uani 1 1 d . . . O11 O 0.5068(3) 1.1576(4) 0.3384(3) 0.0475(14) Uani 1 1 d . . . O10 O 0.4267(3) 1.2358(3) 0.3259(3) 0.0451(14) Uani 1 1 d . . . O8 O 0.3887(3) 1.0716(3) 0.1645(3) 0.0437(14) Uani 1 1 d . . . O7 O 0.4723(3) 1.0009(3) 0.1733(3) 0.0476(14) Uani 1 1 d . . . O12 O 0.5372(3) 1.0501(4) 0.2593(3) 0.0514(15) Uani 1 1 d . . . C5B C 0.5198(4) 0.9637(6) 0.1844(4) 0.048(2) Uani 1 1 d . . . H5B1 H 0.5327 0.9416 0.1501 0.058 Uiso 1 1 calc R . . H5B2 H 0.5169 0.9179 0.2106 0.058 Uiso 1 1 calc R . . C6B C 0.5537(4) 1.0252(6) 0.2075(5) 0.068(3) Uani 1 1 d . . . H6B1 H 0.5879 1.0025 0.2119 0.082 Uiso 1 1 calc R . . H6B2 H 0.5544 1.0730 0.1826 0.082 Uiso 1 1 calc R . . C7B C 0.5721(4) 1.1015(6) 0.2878(4) 0.060(3) Uani 1 1 d . . . H7B1 H 0.5742 1.1550 0.2690 0.072 Uiso 1 1 calc R . . H7B2 H 0.6056 1.0759 0.2898 0.072 Uiso 1 1 calc R . . C8B C 0.5535(4) 1.1129(6) 0.3447(4) 0.059(3) Uani 1 1 d . . . H8B1 H 0.5482 1.0590 0.3621 0.071 Uiso 1 1 calc R . . H8B2 H 0.5782 1.1441 0.3679 0.071 Uiso 1 1 calc R . . C15B C 0.3783(4) 1.2755(6) 0.3148(4) 0.049(2) Uani 1 1 d . . . H15A H 0.3511 1.2419 0.3290 0.059 Uiso 1 1 calc R . . H15B H 0.3778 1.3302 0.3323 0.059 Uiso 1 1 calc R . . C16B C 0.3720(3) 1.2832(5) 0.2558(4) 0.045(2) Uani 1 1 d . . . H16A H 0.3411 1.3141 0.2459 0.055 Uiso 1 1 calc R . . H16B H 0.4005 1.3135 0.2417 0.055 Uiso 1 1 calc R . . C17B C 0.3520(4) 1.2006(6) 0.1763(4) 0.057(3) Uani 1 1 d . . . H17A H 0.3775 1.2242 0.1531 0.068 Uiso 1 1 calc R . . H17B H 0.3210 1.2331 0.1707 0.068 Uiso 1 1 calc R . . C18B C 0.3425(4) 1.1163(5) 0.1607(4) 0.058(3) Uani 1 1 d . . . H18A H 0.3185 1.0915 0.1853 0.070 Uiso 1 1 calc R . . H18B H 0.3277 1.1140 0.1227 0.070 Uiso 1 1 calc R . . C5S C 0.5120(3) 1.3048(4) 0.1100(3) 0.055(2) Uani 1 1 d G . . C6S C 0.5469(3) 1.2731(3) 0.0756(3) 0.077(3) Uani 1 1 d G . . H6S H 0.5637 1.2234 0.0849 0.092 Uiso 1 1 calc R . . C4S C 0.5571(3) 1.3141(5) 0.0276(3) 0.100(4) Uani 1 1 d G . . H4S H 0.5809 1.2925 0.0041 0.120 Uiso 1 1 calc R . . C3S C 0.5325(4) 1.3868(5) 0.0140(3) 0.113(5) Uani 1 1 d G . . H3S H 0.5395 1.4149 -0.0188 0.136 Uiso 1 1 calc R . . C2S C 0.4976(4) 1.4185(4) 0.0484(3) 0.090(3) Uani 1 1 d G . . H2S H 0.4808 1.4682 0.0391 0.109 Uiso 1 1 calc R . . C1S C 0.4874(3) 1.3775(4) 0.0964(3) 0.094(4) Uani 1 1 d G . . H1S H 0.4635 1.3991 0.1198 0.113 Uiso 1 1 calc R . . N1 N 0.4868(4) 1.2237(6) 0.1930(4) 0.083(3) Uani 1 1 d . . . C7S C 0.4971(4) 1.2600(6) 0.1562(5) 0.056(2) Uani 1 1 d . . . C15S C 0.3191(4) 0.7714(4) 0.2616(3) 0.085(3) Uani 1 1 d G . . H15S H 0.3085 0.7425 0.2293 0.103 Uiso 1 1 calc R . . C14S C 0.3487(3) 0.8409(4) 0.2581(3) 0.078(3) Uani 1 1 d G . . H14S H 0.3583 0.8595 0.2234 0.093 Uiso 1 1 calc R . . C16S C 0.3641(3) 0.8832(4) 0.3054(3) 0.070(3) Uani 1 1 d G . . C11S C 0.3500(4) 0.8560(5) 0.3562(3) 0.101(4) Uani 1 1 d G . . H11S H 0.3605 0.8849 0.3886 0.121 Uiso 1 1 calc R . . C12S C 0.3204(4) 0.7865(5) 0.3597(3) 0.135(5) Uani 1 1 d GU . . H12S H 0.3107 0.7680 0.3945 0.162 Uiso 1 1 calc R . . C13S C 0.3049(4) 0.7442(4) 0.3124(4) 0.132(5) Uani 1 1 d G . . H13S H 0.2847 0.6967 0.3148 0.159 Uiso 1 1 calc R . . N2 N 0.4146(5) 1.0090(7) 0.2999(4) 0.091(3) Uani 1 1 d . . . C17A C 0.3920(5) 0.9527(6) 0.3011(4) 0.065(3) Uani 1 1 d . . . C1D C 0.0078(3) 0.1644(5) 0.0741(2) 0.084(4) Uani 1 1 d G . . H1D H -0.0036 0.1469 0.0385 0.101 Uiso 1 1 calc R . . C2D C 0.0514(3) 0.2101(5) 0.0811(3) 0.110(5) Uani 1 1 d G . . H2D H 0.0698 0.2239 0.0503 0.132 Uiso 1 1 calc R . . C3D C 0.0680(3) 0.2357(4) 0.1332(3) 0.058(3) Uani 1 1 d G . . H3D H 0.0978 0.2669 0.1380 0.070 Uiso 1 1 calc R . . C4D C 0.0411(3) 0.2155(3) 0.1783(2) 0.040(2) Uani 1 1 d G . . C19D C -0.0025(3) 0.1698(4) 0.1714(2) 0.042(2) Uani 1 1 d G . . C20D C -0.0191(3) 0.1442(4) 0.1193(3) 0.060(3) Uani 1 1 d G . . H20D H -0.0489 0.1130 0.1145 0.072 Uiso 1 1 calc R . . C9D C 0.0928(3) -0.0080(2) 0.4080(3) 0.041(2) Uani 1 1 d G . . C10D C 0.1349(3) -0.0500(3) 0.4284(3) 0.061(3) Uani 1 1 d G . . H10D H 0.1662 -0.0228 0.4321 0.073 Uiso 1 1 calc R . . C11D C 0.1312(3) -0.1318(3) 0.4434(3) 0.056(3) Uani 1 1 d G . . H11D H 0.1599 -0.1606 0.4573 0.068 Uiso 1 1 calc R . . C12D C 0.0854(3) -0.1716(2) 0.4379(3) 0.048(2) Uani 1 1 d G . . H12D H 0.0828 -0.2276 0.4482 0.058 Uiso 1 1 calc R . . C13D C 0.0433(3) -0.1296(3) 0.4175(3) 0.044(2) Uani 1 1 d G . . H13D H 0.0120 -0.1568 0.4138 0.053 Uiso 1 1 calc R . . C14D C 0.0470(3) -0.0478(3) 0.4025(3) 0.040(2) Uani 1 1 d G . . O6 O 0.0921(3) 0.0731(3) 0.3907(3) 0.0469(15) Uani 1 1 d . . . Na2 Na 0.0290(2) 0.12235(19) 0.3040(2) 0.0455(8) Uani 1 1 d . . . O4 O 0.0538(3) 0.2365(4) 0.2320(3) 0.0434(14) Uani 1 1 d . . . O5 O 0.1111(3) 0.2032(3) 0.3245(3) 0.0430(14) Uani 1 1 d . . . O3 O -0.0266(3) 0.1515(4) 0.2177(3) 0.0428(13) Uani 1 1 d . . . O1 O 0.0079(3) 0.0000(3) 0.3813(3) 0.0436(14) Uani 1 1 d . . . O2 O -0.0574(3) 0.0489(3) 0.2979(3) 0.0480(15) Uani 1 1 d . . . C5D C 0.0992(4) 0.2776(5) 0.2428(4) 0.048(2) Uani 1 1 d . . . H5D1 H 0.0978 0.3328 0.2260 0.057 Uiso 1 1 calc R . . H5D2 H 0.1268 0.2467 0.2273 0.057 Uiso 1 1 calc R . . C6D C 0.1075(4) 0.2843(5) 0.3041(4) 0.052(2) Uani 1 1 d . . . H6D1 H 0.1387 0.3149 0.3136 0.062 Uiso 1 1 calc R . . H6D2 H 0.0793 0.3134 0.3199 0.062 Uiso 1 1 calc R . . C7D C 0.1290(4) 0.2035(5) 0.3800(4) 0.051(2) Uani 1 1 d . . . H7D1 H 0.1039 0.2283 0.4033 0.061 Uiso 1 1 calc R . . H7D2 H 0.1602 0.2359 0.3843 0.061 Uiso 1 1 calc R . . C8D C 0.1388(4) 0.1146(5) 0.3968(4) 0.055(3) Uani 1 1 d . . . H8D1 H 0.1633 0.0893 0.3730 0.066 Uiso 1 1 calc R . . H8D2 H 0.1522 0.1117 0.4353 0.066 Uiso 1 1 calc R . . C15D C -0.0395(4) -0.0399(5) 0.3735(5) 0.056(2) Uani 1 1 d . . . H15C H -0.0512 -0.0598 0.4088 0.067 Uiso 1 1 calc R . . H15D H -0.0372 -0.0871 0.3482 0.067 Uiso 1 1 calc R . . C16D C -0.0750(3) 0.0250(5) 0.3487(4) 0.045(2) Uani 1 1 d . . . H16C H -0.1091 0.0023 0.3435 0.054 Uiso 1 1 calc R . . H16D H -0.0761 0.0729 0.3735 0.054 Uiso 1 1 calc R . . C17D C -0.0911(3) 0.1033(6) 0.2678(4) 0.058(3) Uani 1 1 d . . . H17C H -0.0917 0.1574 0.2861 0.069 Uiso 1 1 calc R . . H17D H -0.1253 0.0804 0.2662 0.069 Uiso 1 1 calc R . . C18D C -0.0735(4) 0.1121(6) 0.2124(4) 0.056(2) Uani 1 1 d . . . H18C H -0.0702 0.0577 0.1951 0.067 Uiso 1 1 calc R . . H18D H -0.0974 0.1453 0.1894 0.067 Uiso 1 1 calc R . . C43S C -0.0070(3) 0.3794(4) 0.4604(3) 0.079(3) Uani 1 1 d G . . H43S H 0.0177 0.4003 0.4377 0.095 Uiso 1 1 calc R . . C42S C -0.0300(3) 0.3050(4) 0.4480(3) 0.058(2) Uani 1 1 d G . . C38S C -0.0661(3) 0.2745(4) 0.4813(3) 0.065(3) Uani 1 1 d G . . H38S H -0.0819 0.2236 0.4728 0.078 Uiso 1 1 calc R . . C41S C -0.0791(3) 0.3185(5) 0.5271(3) 0.099(4) Uani 1 1 d G . . H41S H -0.1037 0.2976 0.5499 0.119 Uiso 1 1 calc R . . C39S C -0.0560(4) 0.3929(5) 0.5396(3) 0.110(4) Uani 1 1 d GU . . H39S H -0.0649 0.4229 0.5709 0.132 Uiso 1 1 calc R . . C40S C -0.0200(3) 0.4234(4) 0.5063(4) 0.120(5) Uani 1 1 d G . . H40S H -0.0042 0.4743 0.5148 0.144 Uiso 1 1 calc R . . N3 N -0.0082(4) 0.2203(5) 0.3645(4) 0.067(2) Uani 1 1 d . . . C44S C -0.0192(4) 0.2584(7) 0.4008(4) 0.057(2) Uani 1 1 d . . . C32S C 0.1582(4) -0.2324(4) 0.3002(3) 0.086(3) Uani 1 1 d G . . H32S H 0.1664 -0.2610 0.3333 0.103 Uiso 1 1 calc R . . C31S C 0.1281(3) -0.1632(5) 0.3006(3) 0.084(3) Uani 1 1 d G . . H31S H 0.1157 -0.1444 0.3341 0.101 Uiso 1 1 calc R . . C36S C 0.1161(3) -0.1214(4) 0.2521(3) 0.068(3) Uani 1 1 d G . . C35S C 0.1342(4) -0.1489(5) 0.2031(3) 0.123(5) Uani 1 1 d G . . H35S H 0.1260 -0.1204 0.1700 0.148 Uiso 1 1 calc R . . C34S C 0.1643(4) -0.2182(5) 0.2027(3) 0.131(5) Uani 1 1 d GU . . H34S H 0.1767 -0.2370 0.1692 0.157 Uiso 1 1 calc R . . C33S C 0.1763(3) -0.2599(4) 0.2512(4) 0.083(3) Uani 1 1 d G . . H33S H 0.1969 -0.3073 0.2509 0.100 Uiso 1 1 calc R . . C37S C 0.0861(6) -0.0440(10) 0.2505(5) 0.105(5) Uani 1 1 d . . . N4 N 0.0640(4) 0.0145(6) 0.2579(4) 0.080(3) Uani 1 1 d . . . C401 C 0.8400(3) 0.1293(4) 0.5745(2) 0.0550(12) Uani 0.797(4) 1 d PDU A 1 C402 C 0.8647(3) 0.0657(2) 0.5442(2) 0.0650(12) Uani 0.797(4) 1 d PDU A 1 C403 C 0.8672(3) -0.0097(3) 0.5758(2) 0.0621(13) Uani 0.797(4) 1 d PDU A 1 C404 C 0.8415(3) 0.0072(3) 0.6254(3) 0.0688(14) Uani 0.797(4) 1 d PDU A 1 C405 C 0.8252(2) 0.0921(3) 0.6251(3) 0.0531(11) Uani 0.797(4) 1 d PDU A 1 C406 C 0.8090(3) 0.1845(3) 0.5472(2) 0.0650(14) Uani 0.797(4) 1 d PDU A 1 C407 C 0.7611(2) 0.2048(4) 0.5686(3) 0.0633(13) Uani 0.797(4) 1 d PDU A 1 C408 C 0.7242(3) 0.2146(4) 0.5232(2) 0.0728(15) Uani 0.797(4) 1 d PDU A 1 C409 C 0.7490(2) 0.1989(4) 0.4728(3) 0.0689(14) Uani 0.797(4) 1 d PDU A 1 C410 C 0.8008(3) 0.1795(3) 0.4880(3) 0.0690(15) Uani 0.797(4) 1 d PDU A 1 C411 C 0.8581(3) 0.0625(3) 0.4880(2) 0.0728(13) Uani 0.797(4) 1 d PDU A 1 C412 C 0.8255(2) 0.1213(4) 0.4591(2) 0.0812(16) Uani 0.797(4) 1 d PDU A 1 C413 C 0.7995(2) 0.0780(3) 0.4141(3) 0.0751(15) Uani 0.797(4) 1 d PDU A 1 C414 C 0.8159(2) -0.0068(3) 0.4150(3) 0.0854(16) Uani 0.797(4) 1 d PDU A 1 C415 C 0.8527(3) -0.0159(3) 0.4604(2) 0.0712(14) Uani 0.797(4) 1 d PDU A 1 C416 C 0.8607(3) -0.0840(3) 0.5497(2) 0.0696(13) Uani 0.797(4) 1 d PDU A 1 C417 C 0.8547(3) -0.0873(3) 0.4904(3) 0.0728(14) Uani 0.797(4) 1 d PDU A 1 C418 C 0.8186(2) -0.1519(4) 0.4782(3) 0.0873(18) Uani 0.797(4) 1 d PDU A 1 C419 C 0.8037(2) -0.1903(5) 0.5285(2) 0.0740(14) Uani 0.797(4) 1 d PDU A 1 C420 C 0.8301(2) -0.1468(3) 0.5731(3) 0.0669(13) Uani 0.797(4) 1 d PDU A 1 C421 C 0.8125(3) -0.0524(2) 0.6476(3) 0.0647(13) Uani 0.797(4) 1 d PDU A 1 C422 C 0.8069(3) -0.1317(3) 0.6210(2) 0.0642(13) Uani 0.797(4) 1 d PDU A 1 C423 C 0.7558(2) -0.1589(4) 0.6266(2) 0.0654(13) Uani 0.797(4) 1 d PDU A 1 C424 C 0.7301(3) -0.0967(3) 0.6568(3) 0.0637(13) Uani 0.797(4) 1 d PDU A 1 C425 C 0.7650(2) -0.0307(3) 0.6698(3) 0.0652(12) Uani 0.797(4) 1 d PDU A 1 C426 C 0.7802(3) 0.1126(3) 0.6459(3) 0.0673(14) Uani 0.797(4) 1 d PDU A 1 C427 C 0.7489(2) 0.0493(3) 0.6679(4) 0.0780(17) Uani 0.797(4) 1 d PDU A 1 C428 C 0.6966(3) 0.0675(3) 0.6551(3) 0.0757(14) Uani 0.797(4) 1 d PDU A 1 C429 C 0.6969(3) 0.1419(4) 0.6224(2) 0.0804(17) Uani 0.797(4) 1 d PDU A 1 C430 C 0.7476(2) 0.1712(5) 0.6171(2) 0.0631(14) Uani 0.797(4) 1 d PDU A 1 C431 C 0.6410(3) -0.1281(5) 0.4819(2) 0.0550(12) Uani 0.797(4) 1 d PDU A 1 C432 C 0.6146(3) -0.0669(2) 0.5125(2) 0.0650(12) Uani 0.797(4) 1 d PDU A 1 C433 C 0.6132(3) 0.0078(3) 0.4801(2) 0.0621(13) Uani 0.797(4) 1 d PDU A 1 C434 C 0.6384(3) -0.0080(3) 0.4300(3) 0.0688(14) Uani 0.797(4) 1 d PDU A 1 C435 C 0.6554(3) -0.0925(3) 0.4306(3) 0.0531(11) Uani 0.797(4) 1 d PDU A 1 C436 C 0.6722(3) -0.1831(3) 0.5092(2) 0.0650(14) Uani 0.797(4) 1 d PDU A 1 C437 C 0.7192(2) -0.2055(4) 0.4867(3) 0.0633(13) Uani 0.797(4) 1 d PDU A 1 C438 C 0.7550(3) -0.2140(4) 0.5333(2) 0.0728(15) Uani 0.797(4) 1 d PDU A 1 C439 C 0.7310(2) -0.2001(4) 0.5843(3) 0.0689(14) Uani 0.797(4) 1 d PDU A 1 C440 C 0.6796(3) -0.1791(3) 0.5685(3) 0.0690(15) Uani 0.797(4) 1 d PDU A 1 C441 C 0.6221(3) -0.0626(3) 0.5685(2) 0.0728(13) Uani 0.797(4) 1 d PDU A 1 C442 C 0.6552(2) -0.1206(5) 0.5974(2) 0.0812(16) Uani 0.797(4) 1 d PDU A 1 C443 C 0.6808(2) -0.0793(3) 0.6432(3) 0.0751(15) Uani 0.797(4) 1 d PDU A 1 C444 C 0.6640(2) 0.0051(3) 0.6405(3) 0.0854(16) Uani 0.797(4) 1 d PDU A 1 C445 C 0.6272(3) 0.0164(3) 0.5954(2) 0.0712(14) Uani 0.797(4) 1 d PDU A 1 C446 C 0.6183(3) 0.0826(3) 0.5056(2) 0.0696(13) Uani 0.797(4) 1 d PDU A 1 C447 C 0.6274(3) 0.0869(3) 0.5646(3) 0.0728(14) Uani 0.797(4) 1 d PDU A 1 C448 C 0.6618(2) 0.1527(4) 0.5799(3) 0.0873(18) Uani 0.797(4) 1 d PDU A 1 C449 C 0.6760(2) 0.1879(5) 0.5285(2) 0.0740(14) Uani 0.797(4) 1 d PDU A 1 C450 C 0.6497(2) 0.1454(3) 0.4833(3) 0.0669(13) Uani 0.797(4) 1 d PDU A 1 C451 C 0.6669(3) 0.0523(3) 0.4079(3) 0.0647(13) Uani 0.797(4) 1 d PDU A 1 C452 C 0.6731(3) 0.1308(3) 0.4355(2) 0.0642(13) Uani 0.797(4) 1 d PDU A 1 C453 C 0.7243(2) 0.1577(4) 0.4303(2) 0.0654(13) Uani 0.797(4) 1 d PDU A 1 C454 C 0.7506(3) 0.0969(3) 0.3995(3) 0.0637(13) Uani 0.797(4) 1 d PDU A 1 C455 C 0.7150(2) 0.0318(3) 0.3864(3) 0.0652(12) Uani 0.797(4) 1 d PDU A 1 C456 C 0.7007(3) -0.1120(3) 0.4100(3) 0.0673(14) Uani 0.797(4) 1 d PDU A 1 C457 C 0.7307(2) -0.0485(3) 0.3860(3) 0.0780(17) Uani 0.797(4) 1 d PDU A 1 C458 C 0.7821(3) -0.0685(3) 0.4029(3) 0.0757(14) Uani 0.797(4) 1 d PDU A 1 C459 C 0.7848(3) -0.1444(4) 0.4342(2) 0.0804(17) Uani 0.797(4) 1 d PDU A 1 C460 C 0.7334(2) -0.1704(5) 0.4390(2) 0.0631(14) Uani 0.797(4) 1 d PDU A 1 C701 C 0.8712(12) 0.0082(12) 0.5464(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C702 C 0.8637(11) -0.0528(12) 0.5040(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C703 C 0.8444(10) -0.1287(14) 0.5235(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C704 C 0.8442(10) -0.1164(14) 0.5822(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C705 C 0.8582(11) -0.0342(12) 0.5966(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C706 C 0.8587(12) 0.0929(14) 0.5367(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C707 C 0.8332(12) 0.1396(19) 0.5794(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C708 C 0.7961(10) 0.190(2) 0.5538(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C709 C 0.7989(9) 0.178(2) 0.4936(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C710 C 0.8383(10) 0.1204(14) 0.4871(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C711 C 0.8440(11) -0.0228(12) 0.4553(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C712 C 0.8320(9) 0.0613(12) 0.4436(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C713 C 0.7849(9) 0.0660(13) 0.4131(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C714 C 0.7708(8) -0.0134(12) 0.3928(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C715 C 0.8063(9) -0.0722(12) 0.4244(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C716 C 0.8065(9) -0.1740(18) 0.4948(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C717 C 0.7900(9) -0.1459(17) 0.4424(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C718 C 0.7352(8) -0.164(2) 0.4391(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C719 C 0.7201(8) -0.204(2) 0.4864(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C720 C 0.7675(9) -0.214(2) 0.5219(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C721 C 0.8044(9) -0.1544(16) 0.6042(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C722 C 0.7650(8) -0.2017(17) 0.5764(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C723 C 0.7216(8) -0.1811(18) 0.6049(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C724 C 0.7330(8) -0.1268(16) 0.6490(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C725 C 0.7842(8) -0.1015(14) 0.6474(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C726 C 0.8393(10) 0.0143(13) 0.6365(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C727 C 0.7958(9) -0.0199(12) 0.6615(13) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C728 C 0.7585(8) 0.0375(13) 0.6790(13) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C729 C 0.7768(9) 0.1113(16) 0.6528(14) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C730 C 0.8260(11) 0.0975(15) 0.6269(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C731 C 0.6093(11) -0.0204(11) 0.5272(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C732 C 0.6220(12) 0.0377(12) 0.5701(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C733 C 0.6319(11) 0.1166(14) 0.5452(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C734 C 0.6320(11) 0.1062(15) 0.4885(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C735 C 0.6176(13) 0.0221(13) 0.4750(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C736 C 0.6254(10) -0.1055(13) 0.5329(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C737 C 0.6459(13) -0.1403(19) 0.4846(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C738 C 0.6793(10) -0.1974(19) 0.5118(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C739 C 0.6770(9) -0.1891(18) 0.5732(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C740 C 0.6470(11) -0.1229(16) 0.5868(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C741 C 0.6392(10) 0.0169(12) 0.6202(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C742 C 0.6555(10) -0.0671(12) 0.6278(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C743 C 0.6985(8) -0.0695(12) 0.6615(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C744 C 0.7096(8) 0.0144(12) 0.6690(13) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C745 C 0.6751(9) 0.0733(12) 0.6424(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C746 C 0.6666(9) 0.1672(18) 0.5717(9) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C747 C 0.6883(9) 0.1476(16) 0.6244(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C748 C 0.7425(8) 0.161(2) 0.6288(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C749 C 0.7541(8) 0.204(2) 0.5803(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C750 C 0.7068(8) 0.2016(18) 0.5463(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C751 C 0.6677(9) 0.1461(18) 0.4598(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C752 C 0.7066(8) 0.1985(16) 0.4889(8) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C753 C 0.7527(8) 0.180(2) 0.4633(10) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C754 C 0.7463(8) 0.1235(16) 0.4165(12) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C755 C 0.6923(8) 0.1070(15) 0.4134(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C756 C 0.6380(11) -0.0133(13) 0.4307(11) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C757 C 0.6764(9) 0.0246(13) 0.3988(13) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C758 C 0.7179(8) -0.0292(14) 0.3901(14) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C759 C 0.7040(10) -0.1100(15) 0.4117(13) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 C760 C 0.6542(11) -0.0963(16) 0.4379(13) 0.0573(17) Uiso 0.203(4) 1 d PD A 2 Cl3 Cl 0.2401(3) 1.25418(17) 0.2757(4) 0.0966(13) Uani 0.648(6) 1 d PDU B 1 Cl4 Cl 0.2712(3) 1.1439(5) 0.3656(4) 0.174(3) Uani 0.648(6) 1 d PDU B 1 C501 C 0.2131(4) 1.0937(6) 0.2131(4) 0.065(3) Uani 0.648(6) 1 d PGDU B 1 H501 H 0.1999 1.1203 0.1809 0.078 Uiso 0.648(6) 1 calc PR B 1 C502 C 0.2285(5) 1.1396(4) 0.2589(4) 0.126(9) Uani 0.648(6) 1 d PGDU B 1 C503 C 0.2479(4) 1.1006(6) 0.3059(4) 0.084(4) Uani 0.648(6) 1 d PGDU B 1 C504 C 0.2519(4) 1.0157(6) 0.3072(4) 0.095(4) Uani 0.648(6) 1 d PGDU B 1 H504 H 0.2651 0.9891 0.3394 0.114 Uiso 0.648(6) 1 calc PR B 1 C505 C 0.2365(6) 0.9698(4) 0.2614(5) 0.135(6) Uani 0.648(6) 1 d PGDU B 1 H505 H 0.2392 0.9118 0.2623 0.162 Uiso 0.648(6) 1 calc PR B 1 C506 C 0.2171(5) 1.0088(6) 0.2144(4) 0.111(8) Uani 0.648(6) 1 d PGDU B 1 H506 H 0.2065 0.9774 0.1831 0.133 Uiso 0.648(6) 1 calc PR B 1 Cl5 Cl 0.2644(6) 1.0415(11) 0.3454(5) 0.177(5) Uani 0.352(6) 1 d PDU B 2 Cl6 Cl 0.2447(7) 1.2206(12) 0.3113(8) 0.229(7) Uani 0.352(6) 1 d PDU B 2 C801 C 0.2325(9) 1.0073(11) 0.2212(8) 0.055(6) Uani 0.352(6) 1 d PDU B 2 H801 H 0.2387 0.9501 0.2187 0.066 Uiso 0.352(6) 1 calc PR B 2 C802 C 0.2421(15) 1.0600(11) 0.2692(8) 0.104(9) Uani 0.352(6) 1 d PDU B 2 C803 C 0.2415(11) 1.1445(9) 0.2681(8) 0.069(6) Uani 0.352(6) 1 d PDU B 2 C804 C 0.2296(7) 1.1868(11) 0.2191(8) 0.071(5) Uani 0.352(6) 1 d PDU B 2 H804 H 0.2391 1.2421 0.2137 0.085 Uiso 0.352(6) 1 calc PR B 2 C805 C 0.2055(9) 1.1462(12) 0.1831(9) 0.065(3) Uani 0.352(6) 1 d PDU B 2 H805 H 0.1824 1.1737 0.1586 0.078 Uiso 0.352(6) 1 calc PR B 2 C806 C 0.2115(10) 1.0607(13) 0.1780(10) 0.107(9) Uani 0.352(6) 1 d PDU B 2 H806 H 0.2012 1.0363 0.1440 0.128 Uiso 0.352(6) 1 calc PR B 2 N5 N 0.1772(3) 0.9007(6) 0.0574(2) 0.088(3) Uani 0.734(9) 1 d PDU C 1 C307 C 0.2087(3) 0.9271(5) 0.04020(18) 0.125(5) Uani 0.734(9) 1 d PDU C 1 C301 C 0.2604(4) 1.0476(3) 0.0201(3) 0.127(6) Uani 0.734(9) 1 d PGDU C 1 H301 H 0.2369 1.0816 0.0369 0.153 Uiso 0.734(9) 1 calc PR C 1 C302 C 0.3036(4) 1.0815(4) 0.0008(3) 0.105(6) Uani 0.734(9) 1 d PGDU C 1 H302 H 0.3096 1.1386 0.0044 0.126 Uiso 0.734(9) 1 calc PR C 1 C303 C 0.3380(3) 1.0318(5) -0.0238(4) 0.128(5) Uani 0.734(9) 1 d PGDU C 1 H303 H 0.3676 1.0550 -0.0370 0.153 Uiso 0.734(9) 1 calc PR C 1 C304 C 0.3292(3) 0.9482(4) -0.0291(4) 0.114(4) Uani 0.734(9) 1 d PGDU C 1 H304 H 0.3527 0.9142 -0.0460 0.136 Uiso 0.734(9) 1 calc PR C 1 C305 C 0.2860(3) 0.9143(3) -0.0099(3) 0.078(3) Uani 0.734(9) 1 d PGDU C 1 H305 H 0.2799 0.8572 -0.0135 0.094 Uiso 0.734(9) 1 calc PR C 1 C306 C 0.2515(3) 0.9640(3) 0.0148(3) 0.120(5) Uani 0.734(9) 1 d PGDU C 1 N6 N 0.1433(8) 1.0880(12) 0.0896(11) 0.098(5) Uiso 0.266(9) 1 d PD C 2 C607 C 0.1771(9) 1.0647(10) 0.0763(12) 0.098(5) Uiso 0.266(9) 1 d PD C 2 C601 C 0.2515(10) 1.0859(11) 0.0228(15) 0.098(5) Uiso 0.266(9) 1 d PD C 2 H601 H 0.2498 1.1430 0.0300 0.118 Uiso 0.266(9) 1 calc PR C 2 C602 C 0.2885(10) 1.0544(14) -0.0093(14) 0.098(5) Uiso 0.266(9) 1 d PD C 2 H602 H 0.3082 1.0899 -0.0301 0.118 Uiso 0.266(9) 1 calc PR C 2 C603 C 0.2959(9) 0.9700(15) -0.0103(13) 0.098(5) Uiso 0.266(9) 1 d PD C 2 H603 H 0.3272 0.9479 -0.0193 0.118 Uiso 0.266(9) 1 calc PR C 2 C604 C 0.2565(11) 0.9182(13) 0.0021(14) 0.098(5) Uiso 0.266(9) 1 d PD C 2 H604 H 0.2529 0.8652 -0.0137 0.118 Uiso 0.266(9) 1 calc PR C 2 C605 C 0.2229(12) 0.9480(9) 0.0389(15) 0.098(5) Uiso 0.266(9) 1 d PD C 2 H605 H 0.2042 0.9114 0.0601 0.118 Uiso 0.266(9) 1 calc PR C 2 C606 C 0.2172(10) 1.0324(9) 0.0440(14) 0.098(5) Uiso 0.266(9) 1 d PD C 2 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 C1B 0.073(7) 0.064(7) 0.076(7) 0.001(5) -0.019(6) 0.009(5) C4B 0.097(9) 0.055(7) 0.058(6) -0.004(5) 0.007(6) -0.009(6) C3B 0.064(6) 0.038(5) 0.050(6) -0.004(4) 0.006(5) -0.003(4) C2B 0.049(5) 0.039(5) 0.035(4) 0.008(4) 0.002(4) 0.003(4) C19B 0.057(6) 0.044(6) 0.037(5) 0.000(4) -0.006(4) -0.007(4) C20B 0.047(6) 0.055(6) 0.059(6) -0.004(5) -0.015(5) -0.004(4) C9B 0.040(5) 0.041(5) 0.041(5) -0.011(4) -0.014(4) 0.002(4) C10B 0.041(5) 0.054(5) 0.057(6) -0.013(4) -0.018(4) 0.010(4) C11B 0.088(8) 0.072(7) 0.040(5) -0.001(5) -0.005(5) 0.024(6) C12B 0.060(6) 0.071(6) 0.047(6) -0.002(4) 0.016(4) 0.017(4) C13B 0.057(6) 0.077(7) 0.051(6) -0.014(5) 0.008(4) 0.028(5) C14B 0.045(5) 0.059(6) 0.031(5) -0.018(4) 0.001(4) 0.008(4) Na1 0.041(2) 0.053(2) 0.0423(19) 0.0054(14) 0.0017(15) 0.0041(14) O9 0.047(4) 0.037(3) 0.063(4) -0.001(3) -0.024(3) 0.012(3) O11 0.039(3) 0.058(3) 0.046(3) -0.010(3) 0.001(3) 0.020(3) O10 0.032(3) 0.050(4) 0.052(4) -0.003(3) -0.003(3) 0.016(2) O8 0.044(4) 0.042(4) 0.045(3) -0.005(3) -0.001(3) 0.005(3) O7 0.056(4) 0.040(3) 0.048(3) -0.006(3) 0.013(3) -0.002(3) O12 0.031(3) 0.081(4) 0.042(3) -0.010(3) 0.005(3) -0.003(3) C5B 0.040(5) 0.059(6) 0.047(5) -0.010(4) 0.004(4) 0.010(4) C6B 0.063(6) 0.068(7) 0.078(7) -0.016(5) 0.043(5) 0.021(5) C7B 0.042(5) 0.066(6) 0.074(7) -0.015(5) 0.012(5) 0.012(5) C8B 0.023(4) 0.093(8) 0.060(6) -0.020(5) -0.011(4) 0.019(4) C15B 0.042(5) 0.051(5) 0.055(6) -0.008(4) 0.004(4) 0.022(4) C16B 0.027(4) 0.041(5) 0.067(6) -0.014(4) -0.006(4) 0.009(3) C17B 0.061(6) 0.058(6) 0.050(6) 0.000(5) -0.013(5) 0.023(5) C18B 0.057(6) 0.049(6) 0.066(6) 0.010(4) -0.024(5) 0.002(4) C5S 0.040(5) 0.044(5) 0.084(7) 0.027(5) 0.017(5) 0.013(4) C6S 0.062(7) 0.059(7) 0.111(9) 0.023(6) 0.021(6) 0.003(5) C4S 0.056(6) 0.103(9) 0.146(11) 0.043(8) 0.044(6) 0.038(6) C3S 0.085(8) 0.111(9) 0.148(11) 0.081(8) 0.049(7) 0.020(6) C2S 0.094(9) 0.073(7) 0.107(9) 0.026(6) 0.027(7) 0.007(6) C1S 0.117(9) 0.076(8) 0.095(8) 0.042(6) 0.073(7) 0.042(6) N1 0.080(7) 0.100(7) 0.071(6) 0.032(5) 0.019(5) 0.008(5) C7S 0.046(6) 0.052(6) 0.069(7) 0.011(5) 0.012(5) -0.003(4) C15S 0.072(7) 0.073(7) 0.111(9) -0.003(6) 0.003(6) -0.002(5) C14S 0.081(7) 0.072(7) 0.085(7) 0.006(5) 0.048(5) -0.028(5) C16S 0.045(5) 0.071(7) 0.097(8) 0.049(6) 0.023(5) 0.023(5) C11S 0.092(7) 0.116(9) 0.094(8) 0.068(7) 0.000(6) -0.027(6) C12S 0.157(9) 0.126(8) 0.123(8) 0.051(7) 0.017(7) -0.056(7) C13S 0.133(12) 0.116(11) 0.150(12) 0.081(9) 0.038(9) -0.032(9) N2 0.104(8) 0.092(8) 0.079(7) -0.001(5) 0.039(5) -0.012(6) C17A 0.079(7) 0.047(5) 0.070(6) 0.012(4) 0.025(5) -0.013(5) C1D 0.113(10) 0.103(9) 0.035(6) 0.014(6) -0.007(6) -0.028(7) C2D 0.130(11) 0.155(12) 0.044(6) 0.030(7) -0.004(6) -0.068(9) C3D 0.057(6) 0.064(6) 0.051(6) 0.018(5) -0.009(5) -0.019(5) C4D 0.035(5) 0.032(4) 0.050(5) 0.000(4) -0.014(4) -0.003(3) C19D 0.041(5) 0.049(5) 0.037(5) 0.011(4) 0.003(4) -0.009(4) C20D 0.075(7) 0.063(6) 0.042(5) 0.001(5) -0.005(5) -0.027(5) C9D 0.053(5) 0.030(5) 0.041(5) 0.001(4) -0.003(4) -0.008(4) C10D 0.066(7) 0.052(6) 0.061(6) 0.010(5) -0.015(5) -0.001(5) C11D 0.081(7) 0.040(5) 0.046(5) 0.009(4) -0.013(5) 0.024(5) C12D 0.069(6) 0.031(5) 0.044(5) 0.006(4) -0.006(4) 0.003(4) C13D 0.051(6) 0.042(5) 0.041(5) -0.001(4) 0.009(4) -0.008(4) C14D 0.046(5) 0.044(5) 0.031(4) 0.008(4) 0.003(4) 0.010(4) O6 0.045(4) 0.034(3) 0.060(4) 0.004(3) -0.013(3) -0.002(2) Na2 0.0371(19) 0.049(2) 0.051(2) -0.0032(14) 0.0022(15) -0.0008(14) O4 0.039(3) 0.057(4) 0.033(3) 0.006(3) -0.005(2) -0.014(3) O5 0.060(4) 0.038(3) 0.030(3) 0.003(2) -0.002(3) -0.009(3) O3 0.027(3) 0.056(3) 0.045(3) 0.004(3) -0.004(2) -0.010(2) O1 0.031(3) 0.045(3) 0.055(4) 0.007(3) 0.002(2) -0.002(2) O2 0.031(3) 0.051(3) 0.063(4) 0.021(3) 0.012(3) -0.005(3) C5D 0.031(4) 0.042(5) 0.069(6) 0.011(4) -0.014(4) -0.010(3) C6D 0.061(6) 0.037(5) 0.055(5) -0.005(4) -0.015(4) -0.016(4) C7D 0.057(6) 0.039(5) 0.055(6) -0.004(4) -0.017(4) -0.010(4) C8D 0.051(6) 0.054(6) 0.057(6) 0.021(4) -0.014(4) -0.020(4) C15D 0.039(5) 0.049(5) 0.083(7) 0.011(5) 0.027(5) -0.003(4) C16D 0.023(4) 0.057(5) 0.056(5) 0.004(4) 0.004(3) 0.005(3) C17D 0.011(4) 0.088(7) 0.072(6) 0.024(5) -0.007(4) 0.004(4) C18D 0.047(6) 0.061(6) 0.059(6) 0.008(5) -0.009(5) -0.017(4) C43S 0.037(5) 0.058(6) 0.144(10) -0.017(6) 0.018(5) -0.009(4) C42S 0.057(6) 0.059(6) 0.060(6) -0.002(5) 0.016(5) 0.005(5) C38S 0.057(6) 0.070(7) 0.070(6) -0.020(5) 0.026(5) -0.037(5) C41S 0.108(9) 0.115(10) 0.081(7) -0.034(7) 0.056(6) -0.016(7) C39S 0.108(8) 0.113(8) 0.114(8) -0.040(6) 0.047(6) -0.026(6) C40S 0.088(9) 0.101(9) 0.175(13) -0.089(9) 0.060(8) -0.046(7) N3 0.065(6) 0.054(5) 0.082(6) -0.009(4) 0.015(4) 0.012(4) C44S 0.054(6) 0.056(6) 0.063(6) -0.012(5) 0.011(5) -0.003(5) C32S 0.112(9) 0.057(6) 0.091(8) -0.027(5) 0.023(6) -0.010(6) C31S 0.122(9) 0.081(7) 0.051(6) -0.018(5) 0.008(5) -0.027(6) C36S 0.079(7) 0.053(6) 0.075(7) -0.030(5) 0.020(5) 0.014(5) C35S 0.207(15) 0.110(9) 0.056(6) -0.013(6) 0.031(7) 0.050(10) C34S 0.180(9) 0.116(7) 0.099(7) -0.050(6) 0.033(6) 0.057(7) C33S 0.063(6) 0.073(6) 0.112(8) -0.012(6) -0.009(5) 0.012(5) C37S 0.083(9) 0.139(12) 0.093(9) -0.060(8) 0.017(7) -0.026(8) N4 0.079(6) 0.064(6) 0.097(7) -0.036(5) 0.007(5) 0.023(5) C401 0.035(2) 0.045(2) 0.083(3) -0.009(2) -0.0151(19) -0.0204(17) C402 0.0226(19) 0.069(3) 0.103(3) 0.005(3) -0.0004(19) -0.0155(19) C403 0.0215(19) 0.051(2) 0.110(3) 0.012(2) -0.032(2) -0.0015(16) C404 0.054(2) 0.075(3) 0.073(3) 0.000(2) -0.043(2) -0.004(2) C405 0.055(2) 0.038(2) 0.062(3) -0.0054(17) -0.0338(19) -0.0118(16) C406 0.058(3) 0.036(2) 0.099(3) 0.004(2) -0.016(2) -0.023(2) C407 0.081(3) 0.0319(19) 0.076(3) -0.018(2) -0.011(2) -0.0040(19) C408 0.090(3) 0.0228(18) 0.105(4) 0.009(2) -0.005(3) 0.009(2) C409 0.104(3) 0.030(2) 0.072(3) 0.0204(19) -0.011(3) -0.016(2) C410 0.090(3) 0.049(2) 0.066(3) 0.029(2) -0.014(2) -0.049(2) C411 0.034(2) 0.100(3) 0.087(3) 0.004(3) 0.026(2) -0.023(2) C412 0.061(3) 0.091(3) 0.093(4) 0.040(3) 0.013(3) -0.035(3) C413 0.061(3) 0.118(4) 0.049(3) 0.028(2) 0.021(2) -0.032(3) C414 0.084(3) 0.111(4) 0.066(3) -0.001(3) 0.047(3) -0.005(3) C415 0.036(3) 0.112(4) 0.068(3) -0.007(3) 0.033(2) 0.002(2) C416 0.027(2) 0.071(3) 0.111(4) 0.008(3) -0.001(2) 0.0200(18) C417 0.032(2) 0.062(3) 0.127(4) -0.028(3) 0.031(2) 0.009(2) C418 0.073(3) 0.077(3) 0.114(4) -0.029(3) 0.025(3) 0.030(3) C419 0.063(3) 0.041(2) 0.115(4) -0.013(2) -0.020(3) 0.0278(19) C420 0.040(2) 0.038(2) 0.120(4) 0.014(2) -0.025(2) 0.0138(17) C421 0.079(3) 0.052(2) 0.059(3) 0.019(2) -0.041(2) -0.012(2) C422 0.073(3) 0.050(2) 0.066(3) 0.014(2) -0.031(2) 0.020(2) C423 0.084(3) 0.044(2) 0.064(3) 0.0378(19) -0.032(2) -0.020(2) C424 0.083(3) 0.071(3) 0.038(2) 0.024(2) 0.008(2) -0.014(2) C425 0.099(3) 0.065(3) 0.0309(19) 0.0085(18) -0.005(2) 0.002(2) C426 0.087(3) 0.074(3) 0.040(2) -0.024(2) -0.002(2) -0.036(2) C427 0.098(4) 0.104(4) 0.033(2) -0.019(2) 0.003(2) -0.010(3) C428 0.064(3) 0.118(4) 0.047(3) -0.031(3) 0.018(2) 0.010(3) C429 0.077(3) 0.076(3) 0.091(4) -0.051(3) 0.029(3) 0.012(2) C430 0.059(2) 0.056(3) 0.074(3) -0.045(2) -0.004(2) -0.0005(19) C431 0.035(2) 0.045(2) 0.083(3) -0.009(2) -0.0151(19) -0.0204(17) C432 0.0226(19) 0.069(3) 0.103(3) 0.005(3) -0.0004(19) -0.0155(19) C433 0.0215(19) 0.051(2) 0.110(3) 0.012(2) -0.032(2) -0.0015(16) C434 0.054(2) 0.075(3) 0.073(3) 0.000(2) -0.043(2) -0.004(2) C435 0.055(2) 0.038(2) 0.062(3) -0.0054(17) -0.0338(19) -0.0118(16) C436 0.058(3) 0.036(2) 0.099(3) 0.004(2) -0.016(2) -0.023(2) C437 0.081(3) 0.0319(19) 0.076(3) -0.018(2) -0.011(2) -0.0040(19) C438 0.090(3) 0.0228(18) 0.105(4) 0.009(2) -0.005(3) 0.009(2) C439 0.104(3) 0.030(2) 0.072(3) 0.0204(19) -0.011(3) -0.016(2) C440 0.090(3) 0.049(2) 0.066(3) 0.029(2) -0.014(2) -0.049(2) C441 0.034(2) 0.100(3) 0.087(3) 0.004(3) 0.026(2) -0.023(2) C442 0.061(3) 0.091(3) 0.093(4) 0.040(3) 0.013(3) -0.035(3) C443 0.061(3) 0.118(4) 0.049(3) 0.028(2) 0.021(2) -0.032(3) C444 0.084(3) 0.111(4) 0.066(3) -0.001(3) 0.047(3) -0.005(3) C445 0.036(3) 0.112(4) 0.068(3) -0.007(3) 0.033(2) 0.002(2) C446 0.027(2) 0.071(3) 0.111(4) 0.008(3) -0.001(2) 0.0200(18) C447 0.032(2) 0.062(3) 0.127(4) -0.028(3) 0.031(2) 0.009(2) C448 0.073(3) 0.077(3) 0.114(4) -0.029(3) 0.025(3) 0.030(3) C449 0.063(3) 0.041(2) 0.115(4) -0.013(2) -0.020(3) 0.0278(19) C450 0.040(2) 0.038(2) 0.120(4) 0.014(2) -0.025(2) 0.0138(17) C451 0.079(3) 0.052(2) 0.059(3) 0.019(2) -0.041(2) -0.012(2) C452 0.073(3) 0.050(2) 0.066(3) 0.014(2) -0.031(2) 0.020(2) C453 0.084(3) 0.044(2) 0.064(3) 0.0378(19) -0.032(2) -0.020(2) C454 0.083(3) 0.071(3) 0.038(2) 0.024(2) 0.008(2) -0.014(2) C455 0.099(3) 0.065(3) 0.0309(19) 0.0085(18) -0.005(2) 0.002(2) C456 0.087(3) 0.074(3) 0.040(2) -0.024(2) -0.002(2) -0.036(2) C457 0.098(4) 0.104(4) 0.033(2) -0.019(2) 0.003(2) -0.010(3) C458 0.064(3) 0.118(4) 0.047(3) -0.031(3) 0.018(2) 0.010(3) C459 0.077(3) 0.076(3) 0.091(4) -0.051(3) 0.029(3) 0.012(2) C460 0.059(2) 0.056(3) 0.074(3) -0.045(2) -0.004(2) -0.0005(19) Cl3 0.0523(14) 0.0895(18) 0.149(3) 0.022(4) 0.0177(16) 0.002(3) Cl4 0.119(4) 0.221(6) 0.184(5) -0.001(5) 0.021(4) -0.037(4) C501 0.063(5) 0.071(5) 0.061(5) 0.009(4) 0.018(4) 0.013(4) C502 0.080(11) 0.140(12) 0.157(13) 0.022(9) 0.019(8) 0.031(8) C503 0.055(6) 0.101(8) 0.100(8) 0.044(7) 0.029(6) 0.011(6) C504 0.075(7) 0.096(8) 0.115(9) -0.018(7) 0.020(7) 0.027(6) C505 0.105(9) 0.142(9) 0.158(12) 0.011(8) 0.009(9) 0.004(9) C506 0.084(11) 0.137(11) 0.112(10) 0.014(8) 0.005(8) -0.047(8) Cl5 0.141(8) 0.238(10) 0.151(8) -0.019(7) 0.002(6) 0.107(7) Cl6 0.188(10) 0.269(11) 0.232(11) -0.031(9) 0.037(9) 0.003(9) C801 0.022(7) 0.061(9) 0.085(11) -0.003(8) 0.028(7) -0.002(6) C802 0.087(11) 0.125(12) 0.099(13) 0.001(10) -0.006(10) -0.012(10) C803 0.025(7) 0.068(10) 0.119(12) 0.013(9) 0.036(8) 0.006(8) C804 0.040(8) 0.081(9) 0.094(10) 0.026(8) 0.037(7) 0.032(7) C805 0.063(5) 0.071(5) 0.061(5) 0.009(4) 0.018(4) 0.013(4) C806 0.092(12) 0.112(12) 0.119(13) -0.004(10) 0.015(9) -0.008(9) N5 0.116(6) 0.078(5) 0.069(5) 0.020(4) -0.008(5) -0.021(5) C307 0.144(10) 0.124(9) 0.100(8) 0.015(7) -0.058(7) -0.043(8) C301 0.137(10) 0.157(10) 0.080(7) 0.011(7) -0.067(7) 0.003(8) C302 0.118(9) 0.121(9) 0.074(8) 0.006(7) -0.021(7) -0.038(7) C303 0.151(9) 0.118(8) 0.110(8) 0.002(7) -0.032(7) 0.007(7) C304 0.146(8) 0.102(7) 0.092(7) -0.006(6) -0.013(6) 0.079(7) C305 0.138(8) 0.021(4) 0.073(6) 0.020(4) -0.028(6) 0.000(5) C306 0.117(9) 0.153(9) 0.083(7) 0.040(7) -0.050(6) -0.008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1B C4B 1.3900 . ? C1B C20B 1.3900 . ? C1B H1B 0.9500 . ? C4B C3B 1.3900 . ? C4B H4B 0.9500 . ? C3B C2B 1.3900 . ? C3B H3B 0.9500 . ? C2B O7 1.344(7) . ? C2B C19B 1.3900 . ? C19B O8 1.355(7) . ? C19B C20B 1.3900 . ? C20B H20B 0.9500 . ? C9B O11 1.349(6) . ? C9B C10B 1.3900 . ? C9B C14B 1.3900 . ? C10B C11B 1.3900 . ? C10B H10B 0.9500 . ? C11B C12B 1.3900 . ? C11B H11B 0.9500 . ? C12B C13B 1.3900 . ? C12B H12B 0.9500 . ? C13B C14B 1.3900 . ? C13B H13B 0.9500 . ? C14B O10 1.333(6) . ? Na1 N2 2.419(11) . ? Na1 N1 2.428(10) . ? Na1 O9 2.588(6) . ? Na1 O11 2.589(6) . ? Na1 O12 2.601(6) . ? Na1 O10 2.690(6) . ? Na1 O8 2.765(6) . ? Na1 O7 2.842(6) . ? O9 C16B 1.416(9) . ? O9 C17B 1.416(9) . ? O11 C8B 1.452(9) . ? O10 C15B 1.463(9) . ? O8 C18B 1.437(10) . ? O7 C5B 1.425(10) . ? O12 C7B 1.411(11) . ? O12 C6B 1.422(10) . ? C5B C6B 1.448(13) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7B C8B 1.513(13) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C15B C16B 1.445(12) . ? C15B H15A 0.9900 . ? C15B H15B 0.9900 . ? C16B H16A 0.9900 . ? C16B H16B 0.9900 . ? C17B C18B 1.446(12) . ? C17B H17A 0.9900 . ? C17B H17B 0.9900 . ? C18B H18A 0.9900 . ? C18B H18B 0.9900 . ? C5S C6S 1.3900 . ? C5S C1S 1.3900 . ? C5S C7S 1.420(11) . ? C6S C4S 1.3900 . ? C6S H6S 0.9500 . ? C4S C3S 1.3900 . ? C4S H4S 0.9500 . ? C3S C2S 1.3900 . ? C3S H3S 0.9500 . ? C2S C1S 1.3900 . ? C2S H2S 0.9500 . ? C1S H1S 0.9500 . ? N1 C7S 1.125(11) . ? C15S C14S 1.3900 . ? C15S C13S 1.3900 . ? C15S H15S 0.9500 . ? C14S C16S 1.3900 . ? C14S H14S 0.9500 . ? C16S C17A 1.366(11) . ? C16S C11S 1.3900 . ? C11S C12S 1.3900 . ? C11S H11S 0.9500 . ? C12S C13S 1.3900 . ? C12S H12S 0.9500 . ? C13S H13S 0.9500 . ? N2 C17A 1.103(12) . ? C1D C2D 1.3900 . ? C1D C20D 1.3900 . ? C1D H1D 0.9500 . ? C2D C3D 1.3900 . ? C2D H2D 0.9500 . ? C3D C4D 1.3900 . ? C3D H3D 0.9500 . ? C4D O4 1.380(6) . ? C4D C19D 1.3900 . ? C19D O3 1.367(6) . ? C19D C20D 1.3900 . ? C20D H20D 0.9500 . ? C9D O6 1.390(6) . ? C9D C10D 1.3900 . ? C9D C14D 1.3900 . ? C10D C11D 1.3900 . ? C10D H10D 0.9500 . ? C11D C12D 1.3900 . ? C11D H11D 0.9500 . ? C12D C13D 1.3900 . ? C12D H12D 0.9500 . ? C13D C14D 1.3900 . ? C13D H13D 0.9500 . ? C14D O1 1.386(6) . ? O6 C8D 1.424(9) . ? O6 Na2 2.758(6) . ? Na2 N4 2.315(9) . ? Na2 N3 2.429(9) . ? Na2 O3 2.561(6) . ? Na2 O5 2.592(6) . ? Na2 O2 2.606(6) . ? Na2 O4 2.672(6) . ? Na2 O1 2.829(6) . ? O4 C5D 1.401(8) . ? O5 C7D 1.414(9) . ? O5 C6D 1.416(9) . ? O3 C18D 1.412(10) . ? O1 C15D 1.430(10) . ? O2 C16D 1.408(9) . ? O2 C17D 1.441(9) . ? C5D C6D 1.505(11) . ? C5D H5D1 0.9900 . ? C5D H5D2 0.9900 . ? C6D H6D1 0.9900 . ? C6D H6D2 0.9900 . ? C7D C8D 1.528(12) . ? C7D H7D1 0.9900 . ? C7D H7D2 0.9900 . ? C8D H8D1 0.9900 . ? C8D H8D2 0.9900 . ? C15D C16D 1.528(11) . ? C15D H15C 0.9900 . ? C15D H15D 0.9900 . ? C16D H16C 0.9900 . ? C16D H16D 0.9900 . ? C17D C18D 1.463(13) . ? C17D H17C 0.9900 . ? C17D H17D 0.9900 . ? C18D H18C 0.9900 . ? C18D H18D 0.9900 . ? C43S C42S 1.3900 . ? C43S C40S 1.3900 . ? C43S H43S 0.9500 . ? C42S C38S 1.3900 . ? C42S C44S 1.423(11) . ? C38S C41S 1.3900 . ? C38S H38S 0.9500 . ? C41S C39S 1.3900 . ? C41S H41S 0.9500 . ? C39S C40S 1.3900 . ? C39S H39S 0.9500 . ? C40S H40S 0.9500 . ? N3 C44S 1.135(11) . ? C32S C31S 1.3900 . ? C32S C33S 1.3900 . ? C32S H32S 0.9500 . ? C31S C36S 1.3900 . ? C31S H31S 0.9500 . ? C36S C35S 1.3900 . ? C36S C37S 1.498(18) . ? C35S C34S 1.3900 . ? C35S H35S 0.9500 . ? C34S C33S 1.3900 . ? C34S H34S 0.9500 . ? C33S H33S 0.9500 . ? C37S N4 1.143(16) . ? C401 C406 1.374(2) . ? C401 C405 1.451(2) . ? C401 C402 1.456(2) . ? C402 C411 1.374(2) . ? C402 C403 1.453(2) . ? C403 C416 1.376(2) . ? C403 C404 1.452(2) . ? C404 C421 1.375(2) . ? C404 C405 1.453(2) . ? C405 C426 1.376(2) . ? C406 C407 1.451(2) . ? C406 C410 1.453(2) . ? C407 C430 1.374(2) . ? C407 C408 1.455(2) . ? C408 C449 1.375(2) . ? C408 C409 1.453(2) . ? C409 C453 1.376(2) . ? C409 C410 1.453(2) . ? C410 C412 1.376(2) . ? C411 C415 1.451(2) . ? C411 C412 1.455(2) . ? C412 C413 1.451(2) . ? C413 C454 1.377(2) . ? C413 C414 1.452(2) . ? C414 C458 1.376(2) . ? C414 C415 1.452(2) . ? C415 C417 1.376(2) . ? C416 C417 1.450(2) . ? C416 C420 1.451(2) . ? C417 C418 1.453(2) . ? C418 C459 1.374(2) . ? C418 C419 1.453(2) . ? C419 C438 1.375(2) . ? C419 C420 1.453(2) . ? C420 C422 1.375(2) . ? C421 C422 1.453(2) . ? C421 C425 1.454(2) . ? C422 C423 1.454(2) . ? C423 C439 1.375(2) . ? C423 C424 1.450(2) . ? C424 C443 1.375(2) . ? C424 C425 1.452(2) . ? C425 C427 1.376(2) . ? C426 C430 1.451(2) . ? C426 C427 1.453(2) . ? C427 C428 1.451(2) . ? C428 C444 1.376(2) . ? C428 C429 1.454(2) . ? C429 C448 1.374(2) . ? C429 C430 1.455(2) . ? C431 C436 1.374(2) . ? C431 C435 1.453(2) . ? C431 C432 1.455(2) . ? C432 C441 1.374(2) . ? C432 C433 1.452(2) . ? C433 C446 1.375(2) . ? C433 C434 1.453(2) . ? C434 C451 1.375(2) . ? C434 C435 1.454(2) . ? C435 C456 1.378(2) . ? C436 C437 1.448(2) . ? C436 C440 1.453(2) . ? C437 C460 1.372(2) . ? C437 C438 1.455(2) . ? C438 C439 1.452(2) . ? C439 C440 1.452(2) . ? C440 C442 1.374(2) . ? C441 C445 1.449(2) . ? C441 C442 1.454(2) . ? C442 C443 1.449(2) . ? C443 C444 1.450(2) . ? C444 C445 1.451(2) . ? C445 C447 1.375(2) . ? C446 C447 1.449(2) . ? C446 C450 1.451(2) . ? C447 C448 1.452(2) . ? C448 C449 1.453(2) . ? C449 C450 1.454(2) . ? C450 C452 1.377(2) . ? C451 C452 1.453(2) . ? C451 C455 1.457(2) . ? C452 C453 1.455(2) . ? C453 C454 1.451(2) . ? C454 C455 1.453(2) . ? C455 C457 1.377(2) . ? C456 C460 1.451(2) . ? C456 C457 1.454(2) . ? C457 C458 1.454(2) . ? C458 C459 1.454(2) . ? C459 C460 1.455(2) . ? C701 C706 1.440(18) . ? C701 C702 1.444(18) . ? C701 C705 1.467(18) . ? C702 C711 1.364(17) . ? C702 C703 1.435(18) . ? C703 C716 1.411(18) . ? C703 C704 1.449(18) . ? C704 C721 1.369(18) . ? C704 C705 1.433(18) . ? C705 C726 1.371(18) . ? C706 C710 1.377(18) . ? C706 C707 1.488(18) . ? C707 C730 1.372(18) . ? C707 C708 1.416(18) . ? C708 C749 1.348(18) . ? C708 C709 1.488(18) . ? C709 C753 1.409(18) . ? C709 C710 1.433(18) . ? C710 C712 1.437(18) . ? C711 C712 1.436(18) . ? C711 C715 1.470(18) . ? C712 C713 1.433(18) . ? C713 C754 1.404(18) . ? C713 C714 1.430(18) . ? C714 C758 1.442(18) . ? C714 C715 1.531(18) . ? C715 C717 1.361(18) . ? C716 C717 1.409(18) . ? C716 C720 1.429(18) . ? C717 C718 1.496(18) . ? C718 C759 1.369(18) . ? C718 C719 1.407(18) . ? C719 C738 1.293(18) . ? C719 C720 1.508(18) . ? C720 C722 1.351(18) . ? C721 C722 1.449(18) . ? C721 C725 1.488(18) . ? C722 C723 1.429(18) . ? C723 C739 1.394(18) . ? C723 C724 1.417(18) . ? C724 C743 1.361(18) . ? C724 C725 1.437(18) . ? C725 C727 1.407(17) . ? C726 C730 1.420(18) . ? C726 C727 1.459(18) . ? C727 C728 1.451(18) . ? C728 C744 1.375(18) . ? C728 C729 1.462(18) . ? C729 C748 1.342(18) . ? C729 C730 1.510(18) . ? C731 C732 1.442(18) . ? C731 C736 1.458(17) . ? C731 C735 1.478(18) . ? C732 C741 1.330(18) . ? C732 C733 1.454(18) . ? C733 C746 1.379(18) . ? C733 C734 1.397(18) . ? C734 C751 1.380(18) . ? C734 C735 1.459(18) . ? C735 C756 1.368(18) . ? C736 C740 1.435(18) . ? C736 C737 1.446(18) . ? C737 C760 1.375(18) . ? C737 C738 1.430(19) . ? C738 C739 1.511(18) . ? C739 C740 1.398(18) . ? C740 C742 1.365(18) . ? C741 C745 1.418(18) . ? C741 C742 1.447(18) . ? C742 C743 1.381(18) . ? C743 C744 1.412(18) . ? C744 C745 1.461(18) . ? C745 C747 1.344(18) . ? C746 C750 1.391(18) . ? C746 C747 1.422(18) . ? C747 C748 1.469(18) . ? C748 C749 1.424(18) . ? C749 C750 1.479(18) . ? C750 C752 1.402(17) . ? C751 C755 1.487(18) . ? C751 C752 1.497(18) . ? C752 C753 1.449(18) . ? C753 C754 1.467(18) . ? C754 C755 1.470(18) . ? C755 C757 1.449(18) . ? C756 C760 1.432(18) . ? C756 C757 1.462(18) . ? C757 C758 1.442(18) . ? C758 C759 1.477(18) . ? C759 C760 1.529(18) . ? Cl3 C502 1.937(9) . ? Cl4 C503 1.708(10) . ? C501 C502 1.3900 . ? C501 C506 1.3900 . ? C501 H501 0.9500 . ? C502 C503 1.3900 . ? C503 C504 1.3900 . ? C504 C505 1.3900 . ? C504 H504 0.9500 . ? C505 C506 1.3900 . ? C505 H505 0.9500 . ? C506 H506 0.9500 . ? Cl5 C802 1.947(17) . ? Cl6 C803 1.631(17) . ? C801 C806 1.459(18) . ? C801 C802 1.467(18) . ? C801 H801 0.9500 . ? C802 C803 1.378(17) . ? C803 C804 1.404(17) . ? C804 C805 1.253(18) . ? C804 H804 0.9500 . ? C805 C806 1.411(18) . ? C805 H805 0.9500 . ? C806 H806 0.9500 . ? N5 C307 1.056(14) . ? C307 C306 1.466(16) . ? C301 C302 1.3900 . ? C301 C306 1.3900 . ? C301 H301 0.9500 . ? C302 C303 1.3900 . ? C302 H302 0.9500 . ? C303 C304 1.3900 . ? C303 H303 0.9500 . ? C304 C305 1.3900 . ? C304 H304 0.9500 . ? C305 C306 1.3900 . ? C305 H305 0.9500 . ? N6 C607 1.050(15) . ? C607 C606 1.466(17) . ? C601 C606 1.390(5) . ? C601 C602 1.395(5) . ? C601 H601 0.9500 . ? C602 C603 1.393(5) . ? C602 H602 0.9500 . ? C603 C604 1.399(5) . ? C603 H603 0.9500 . ? C604 C605 1.396(5) . ? C604 H604 0.9500 . ? C605 C606 1.392(5) . ? C605 H605 0.9500 . ? 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 C4B C1B C20B 120.0 . . ? C4B C1B H1B 120.0 . . ? C20B C1B H1B 120.0 . . ? C3B C4B C1B 120.0 . . ? C3B C4B H4B 120.0 . . ? C1B C4B H4B 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? O7 C2B C3B 125.7(4) . . ? O7 C2B C19B 114.2(4) . . ? C3B C2B C19B 120.0 . . ? O8 C19B C20B 124.6(4) . . ? O8 C19B C2B 115.3(4) . . ? C20B C19B C2B 120.0 . . ? C19B C20B C1B 120.0 . . ? C19B C20B H20B 120.0 . . ? C1B C20B H20B 120.0 . . ? O11 C9B C10B 127.4(4) . . ? O11 C9B C14B 112.5(4) . . ? C10B C9B C14B 120.0 . . ? C9B C10B C11B 120.0 . . ? C9B C10B H10B 120.0 . . ? C11B C10B H10B 120.0 . . ? C12B C11B C10B 120.0 . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C13B C12B C11B 120.0 . . ? C13B C12B H12B 120.0 . . ? C11B C12B H12B 120.0 . . ? C12B C13B C14B 120.0 . . ? C12B C13B H13B 120.0 . . ? C14B C13B H13B 120.0 . . ? O10 C14B C13B 123.4(4) . . ? O10 C14B C9B 116.6(4) . . ? C13B C14B C9B 120.0 . . ? N2 Na1 N1 172.1(4) . . ? N2 Na1 O9 97.3(3) . . ? N1 Na1 O9 84.1(3) . . ? N2 Na1 O11 90.4(3) . . ? N1 Na1 O11 95.7(3) . . ? O9 Na1 O11 119.1(2) . . ? N2 Na1 O12 90.0(3) . . ? N1 Na1 O12 88.1(3) . . ? O9 Na1 O12 171.8(2) . . ? O11 Na1 O12 64.43(18) . . ? N2 Na1 O10 94.9(3) . . ? N1 Na1 O10 92.7(3) . . ? O9 Na1 O10 62.54(18) . . ? O11 Na1 O10 56.62(17) . . ? O12 Na1 O10 120.83(19) . . ? N2 Na1 O8 84.5(3) . . ? N1 Na1 O8 89.3(3) . . ? O9 Na1 O8 62.70(17) . . ? O11 Na1 O8 174.8(2) . . ? O12 Na1 O8 114.5(2) . . ? O10 Na1 O8 124.67(19) . . ? N2 Na1 O7 84.0(3) . . ? N1 Na1 O7 88.4(3) . . ? O9 Na1 O7 115.7(2) . . ? O11 Na1 O7 125.2(2) . . ? O12 Na1 O7 61.08(18) . . ? O10 Na1 O7 177.8(2) . . ? O8 Na1 O7 53.42(18) . . ? C16B O9 C17B 116.0(6) . . ? C16B O9 Na1 111.5(4) . . ? C17B O9 Na1 112.7(5) . . ? C9B O11 C8B 114.7(6) . . ? C9B O11 Na1 117.2(4) . . ? C8B O11 Na1 115.8(5) . . ? C14B O10 C15B 118.5(5) . . ? C14B O10 Na1 113.3(4) . . ? C15B O10 Na1 115.1(4) . . ? C19B O8 C18B 118.8(6) . . ? C19B O8 Na1 119.1(4) . . ? C18B O8 Na1 112.2(5) . . ? C2B O7 C5B 117.7(6) . . ? C2B O7 Na1 117.6(4) . . ? C5B O7 Na1 112.4(5) . . ? C7B O12 C6B 112.3(7) . . ? C7B O12 Na1 109.2(5) . . ? C6B O12 Na1 112.8(5) . . ? O7 C5B C6B 108.3(7) . . ? O7 C5B H5B1 110.0 . . ? C6B C5B H5B1 110.0 . . ? O7 C5B H5B2 110.0 . . ? C6B C5B H5B2 110.0 . . ? H5B1 C5B H5B2 108.4 . . ? O12 C6B C5B 109.0(8) . . ? O12 C6B H6B1 109.9 . . ? C5B C6B H6B1 109.9 . . ? O12 C6B H6B2 109.9 . . ? C5B C6B H6B2 109.9 . . ? H6B1 C6B H6B2 108.3 . . ? O12 C7B C8B 106.6(7) . . ? O12 C7B H7B1 110.4 . . ? C8B C7B H7B1 110.4 . . ? O12 C7B H7B2 110.4 . . ? C8B C7B H7B2 110.4 . . ? H7B1 C7B H7B2 108.6 . . ? O11 C8B C7B 106.8(7) . . ? O11 C8B H8B1 110.4 . . ? C7B C8B H8B1 110.4 . . ? O11 C8B H8B2 110.4 . . ? C7B C8B H8B2 110.4 . . ? H8B1 C8B H8B2 108.6 . . ? C16B C15B O10 106.1(6) . . ? C16B C15B H15A 110.5 . . ? O10 C15B H15A 110.5 . . ? C16B C15B H15B 110.5 . . ? O10 C15B H15B 110.5 . . ? H15A C15B H15B 108.7 . . ? O9 C16B C15B 109.2(7) . . ? O9 C16B H16A 109.8 . . ? C15B C16B H16A 109.8 . . ? O9 C16B H16B 109.8 . . ? C15B C16B H16B 109.8 . . ? H16A C16B H16B 108.3 . . ? O9 C17B C18B 109.6(7) . . ? O9 C17B H17A 109.8 . . ? C18B C17B H17A 109.8 . . ? O9 C17B H17B 109.7 . . ? C18B C17B H17B 109.7 . . ? H17A C17B H17B 108.2 . . ? O8 C18B C17B 109.0(7) . . ? O8 C18B H18A 109.9 . . ? C17B C18B H18A 109.9 . . ? O8 C18B H18B 109.9 . . ? C17B C18B H18B 109.9 . . ? H18A C18B H18B 108.3 . . ? C6S C5S C1S 120.0 . . ? C6S C5S C7S 121.0(6) . . ? C1S C5S C7S 118.6(6) . . ? C4S C6S C5S 120.0 . . ? C4S C6S H6S 120.0 . . ? C5S C6S H6S 120.0 . . ? C6S C4S C3S 120.0 . . ? C6S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C1S C2S C3S 120.0 . . ? C1S C2S H2S 120.0 . . ? C3S C2S H2S 120.0 . . ? C2S C1S C5S 120.0 . . ? C2S C1S H1S 120.0 . . ? C5S C1S H1S 120.0 . . ? C7S N1 Na1 163.1(10) . . ? N1 C7S C5S 178.0(10) . . ? C14S C15S C13S 120.0 . . ? C14S C15S H15S 120.0 . . ? C13S C15S H15S 120.0 . . ? C16S C14S C15S 120.0 . . ? C16S C14S H14S 120.0 . . ? C15S C14S H14S 120.0 . . ? C17A C16S C11S 120.8(6) . . ? C17A C16S C14S 119.2(6) . . ? C11S C16S C14S 120.0 . . ? C12S C11S C16S 120.0 . . ? C12S C11S H11S 120.0 . . ? C16S C11S H11S 120.0 . . ? C11S C12S C13S 120.0 . . ? C11S C12S H12S 120.0 . . ? C13S C12S H12S 120.0 . . ? C12S C13S C15S 120.0 . . ? C12S C13S H13S 120.0 . . ? C15S C13S H13S 120.0 . . ? C17A N2 Na1 152.4(9) . . ? N2 C17A C16S 177.2(10) . . ? C2D C1D C20D 120.0 . . ? C2D C1D H1D 120.0 . . ? C20D C1D H1D 120.0 . . ? C1D C2D C3D 120.0 . . ? C1D C2D H2D 120.0 . . ? C3D C2D H2D 120.0 . . ? C4D C3D C2D 120.0 . . ? C4D C3D H3D 120.0 . . ? C2D C3D H3D 120.0 . . ? O4 C4D C3D 125.5(4) . . ? O4 C4D C19D 114.5(4) . . ? C3D C4D C19D 120.0 . . ? O3 C19D C4D 116.7(4) . . ? O3 C19D C20D 123.3(4) . . ? C4D C19D C20D 120.0 . . ? C19D C20D C1D 120.0 . . ? C19D C20D H20D 120.0 . . ? C1D C20D H20D 120.0 . . ? O6 C9D C10D 125.2(4) . . ? O6 C9D C14D 114.8(4) . . ? C10D C9D C14D 120.0 . . ? C11D C10D C9D 120.0 . . ? C11D C10D H10D 120.0 . . ? C9D C10D H10D 120.0 . . ? C10D C11D C12D 120.0 . . ? C10D C11D H11D 120.0 . . ? C12D C11D H11D 120.0 . . ? C13D C12D C11D 120.0 . . ? C13D C12D H12D 120.0 . . ? C11D C12D H12D 120.0 . . ? C12D C13D C14D 120.0 . . ? C12D C13D H13D 120.0 . . ? C14D C13D H13D 120.0 . . ? O1 C14D C13D 125.1(4) . . ? O1 C14D C9D 114.9(4) . . ? C13D C14D C9D 120.0 . . ? C9D O6 C8D 115.1(5) . . ? C9D O6 Na2 120.6(4) . . ? C8D O6 Na2 116.2(4) . . ? N4 Na2 N3 170.8(3) . . ? N4 Na2 O3 88.6(3) . . ? N3 Na2 O3 97.9(3) . . ? N4 Na2 O5 96.8(3) . . ? N3 Na2 O5 85.4(2) . . ? O3 Na2 O5 121.0(2) . . ? N4 Na2 O2 90.3(3) . . ? N3 Na2 O2 86.8(3) . . ? O3 Na2 O2 63.98(18) . . ? O5 Na2 O2 171.3(2) . . ? N4 Na2 O4 95.1(3) . . ? N3 Na2 O4 93.8(3) . . ? O3 Na2 O4 58.91(17) . . ? O5 Na2 O4 62.11(17) . . ? O2 Na2 O4 122.39(19) . . ? N4 Na2 O6 84.5(3) . . ? N3 Na2 O6 88.9(3) . . ? O3 Na2 O6 172.9(2) . . ? O5 Na2 O6 61.39(17) . . ? O2 Na2 O6 114.6(2) . . ? O4 Na2 O6 122.99(19) . . ? N4 Na2 O1 83.6(3) . . ? N3 Na2 O1 87.4(3) . . ? O3 Na2 O1 123.5(2) . . ? O5 Na2 O1 115.48(19) . . ? O2 Na2 O1 60.21(17) . . ? O4 Na2 O1 177.2(2) . . ? O6 Na2 O1 54.43(16) . . ? C4D O4 C5D 117.8(6) . . ? C4D O4 Na2 113.2(4) . . ? C5D O4 Na2 117.0(4) . . ? C7D O5 C6D 110.3(5) . . ? C7D O5 Na2 115.3(5) . . ? C6D O5 Na2 111.6(4) . . ? C19D O3 C18D 118.9(6) . . ? C19D O3 Na2 116.1(4) . . ? C18D O3 Na2 117.8(5) . . ? C14D O1 C15D 116.3(5) . . ? C14D O1 Na2 118.1(4) . . ? C15D O1 Na2 116.1(5) . . ? C16D O2 C17D 112.9(6) . . ? C16D O2 Na2 114.7(4) . . ? C17D O2 Na2 106.2(5) . . ? O4 C5D C6D 107.7(7) . . ? O4 C5D H5D1 110.2 . . ? C6D C5D H5D1 110.2 . . ? O4 C5D H5D2 110.2 . . ? C6D C5D H5D2 110.2 . . ? H5D1 C5D H5D2 108.5 . . ? O5 C6D C5D 106.5(6) . . ? O5 C6D H6D1 110.4 . . ? C5D C6D H6D1 110.4 . . ? O5 C6D H6D2 110.4 . . ? C5D C6D H6D2 110.4 . . ? H6D1 C6D H6D2 108.6 . . ? O5 C7D C8D 107.4(6) . . ? O5 C7D H7D1 110.2 . . ? C8D C7D H7D1 110.2 . . ? O5 C7D H7D2 110.2 . . ? C8D C7D H7D2 110.2 . . ? H7D1 C7D H7D2 108.5 . . ? O6 C8D C7D 106.6(7) . . ? O6 C8D H8D1 110.4 . . ? C7D C8D H8D1 110.4 . . ? O6 C8D H8D2 110.4 . . ? C7D C8D H8D2 110.4 . . ? H8D1 C8D H8D2 108.6 . . ? O1 C15D C16D 105.5(7) . . ? O1 C15D H15C 110.6 . . ? C16D C15D H15C 110.6 . . ? O1 C15D H15D 110.6 . . ? C16D C15D H15D 110.6 . . ? H15C C15D H15D 108.8 . . ? O2 C16D C15D 108.0(6) . . ? O2 C16D H16C 110.1 . . ? C15D C16D H16C 110.1 . . ? O2 C16D H16D 110.1 . . ? C15D C16D H16D 110.1 . . ? H16C C16D H16D 108.4 . . ? O2 C17D C18D 107.8(7) . . ? O2 C17D H17C 110.1 . . ? C18D C17D H17C 110.1 . . ? O2 C17D H17D 110.1 . . ? C18D C17D H17D 110.1 . . ? H17C C17D H17D 108.5 . . ? O3 C18D C17D 106.9(7) . . ? O3 C18D H18C 110.3 . . ? C17D C18D H18C 110.3 . . ? O3 C18D H18D 110.3 . . ? C17D C18D H18D 110.3 . . ? H18C C18D H18D 108.6 . . ? C42S C43S C40S 120.0 . . ? C42S C43S H43S 120.0 . . ? C40S C43S H43S 120.0 . . ? C38S C42S C43S 120.0 . . ? C38S C42S C44S 117.5(6) . . ? C43S C42S C44S 122.5(6) . . ? C42S C38S C41S 120.0 . . ? C42S C38S H38S 120.0 . . ? C41S C38S H38S 120.0 . . ? C38S C41S C39S 120.0 . . ? C38S C41S H41S 120.0 . . ? C39S C41S H41S 120.0 . . ? C40S C39S C41S 120.0 . . ? C40S C39S H39S 120.0 . . ? C41S C39S H39S 120.0 . . ? C39S C40S C43S 120.0 . . ? C39S C40S H40S 120.0 . . ? C43S C40S H40S 120.0 . . ? C44S N3 Na2 165.7(8) . . ? N3 C44S C42S 176.4(11) . . ? C31S C32S C33S 120.0 . . ? C31S C32S H32S 120.0 . . ? C33S C32S H32S 120.0 . . ? C32S C31S C36S 120.0 . . ? C32S C31S H31S 120.0 . . ? C36S C31S H31S 120.0 . . ? C31S C36S C35S 120.0 . . ? C31S C36S C37S 122.4(7) . . ? C35S C36S C37S 117.6(7) . . ? C34S C35S C36S 120.0 . . ? C34S C35S H35S 120.0 . . ? C36S C35S H35S 120.0 . . ? C35S C34S C33S 120.0 . . ? C35S C34S H34S 120.0 . . ? C33S C34S H34S 120.0 . . ? C34S C33S C32S 120.0 . . ? C34S C33S H33S 120.0 . . ? C32S C33S H33S 120.0 . . ? N4 C37S C36S 169.4(12) . . ? C37S N4 Na2 159.9(10) . . ? C406 C401 C405 120.07(12) . . ? C406 C401 C402 119.98(13) . . ? C405 C401 C402 106.7(6) . . ? C411 C402 C403 119.90(12) . . ? C411 C402 C401 119.87(12) . . ? C403 C402 C401 110.0(6) . . ? C416 C403 C404 119.93(13) . . ? C416 C403 C402 119.96(13) . . ? C404 C403 C402 105.8(6) . . ? C421 C404 C403 119.95(12) . . ? C421 C404 C405 119.99(12) . . ? C403 C404 C405 109.5(6) . . ? C426 C405 C401 119.92(12) . . ? C426 C405 C404 120.01(12) . . ? C401 C405 C404 107.9(6) . . ? C401 C406 C407 120.01(13) . . ? C401 C406 C410 120.11(13) . . ? C407 C406 C410 106.4(6) . . ? C430 C407 C406 119.94(12) . . ? C430 C407 C408 120.09(12) . . ? C406 C407 C408 109.3(6) . . ? C449 C408 C409 119.94(12) . . ? C449 C408 C407 119.86(13) . . ? C409 C408 C407 107.5(6) . . ? C453 C409 C408 120.05(12) . . ? C453 C409 C410 119.98(12) . . ? C408 C409 C410 107.4(6) . . ? C412 C410 C406 119.92(12) . . ? C412 C410 C409 120.01(12) . . ? C406 C410 C409 109.4(6) . . ? C402 C411 C415 120.06(12) . . ? C402 C411 C412 120.08(12) . . ? C415 C411 C412 108.3(6) . . ? C410 C412 C413 119.98(13) . . ? C410 C412 C411 119.96(13) . . ? C413 C412 C411 107.3(6) . . ? C454 C413 C412 119.99(12) . . ? C454 C413 C414 119.97(12) . . ? C412 C413 C414 108.7(6) . . ? C458 C414 C413 120.04(13) . . ? C458 C414 C415 120.10(13) . . ? C413 C414 C415 107.6(6) . . ? C417 C415 C411 120.02(12) . . ? C417 C415 C414 119.96(12) . . ? C411 C415 C414 108.0(6) . . ? C403 C416 C417 119.98(12) . . ? C403 C416 C420 120.06(12) . . ? C417 C416 C420 109.4(6) . . ? C415 C417 C416 119.95(13) . . ? C415 C417 C418 119.93(13) . . ? C416 C417 C418 105.6(6) . . ? C459 C418 C417 119.98(12) . . ? C459 C418 C419 120.08(12) . . ? C417 C418 C419 110.5(6) . . ? C438 C419 C418 119.96(13) . . ? C438 C419 C420 119.98(13) . . ? C418 C419 C420 106.2(6) . . ? C422 C420 C416 119.95(12) . . ? C422 C420 C419 120.12(12) . . ? C416 C420 C419 108.2(6) . . ? C404 C421 C422 120.04(12) . . ? C404 C421 C425 120.02(12) . . ? C422 C421 C425 108.3(6) . . ? C420 C422 C421 120.00(12) . . ? C420 C422 C423 119.82(12) . . ? C421 C422 C423 107.7(6) . . ? C439 C423 C424 119.93(12) . . ? C439 C423 C422 119.99(12) . . ? C424 C423 C422 108.1(6) . . ? C443 C424 C423 120.01(12) . . ? C443 C424 C425 119.93(12) . . ? C423 C424 C425 108.2(6) . . ? C427 C425 C424 119.93(13) . . ? C427 C425 C421 119.96(13) . . ? C424 C425 C421 107.7(6) . . ? C405 C426 C430 119.93(12) . . ? C405 C426 C427 119.99(13) . . ? C430 C426 C427 107.7(6) . . ? C425 C427 C428 120.03(12) . . ? C425 C427 C426 119.97(12) . . ? C428 C427 C426 110.2(6) . . ? C444 C428 C427 119.82(13) . . ? C444 C428 C429 119.82(13) . . ? C427 C428 C429 104.8(6) . . ? C448 C429 C428 119.91(12) . . ? C448 C429 C430 119.81(12) . . ? C428 C429 C430 110.9(6) . . ? C407 C430 C426 120.09(13) . . ? C407 C430 C429 119.97(13) . . ? C426 C430 C429 106.4(6) . . ? C436 C431 C435 119.78(18) . . ? C436 C431 C432 120.01(12) . . ? C435 C431 C432 109.2(6) . . ? C441 C432 C433 119.83(12) . . ? C441 C432 C431 119.92(12) . . ? C433 C432 C431 107.2(6) . . ? C446 C433 C432 120.02(12) . . ? C446 C433 C434 119.97(12) . . ? C432 C433 C434 108.2(6) . . ? C451 C434 C433 119.95(12) . . ? C451 C434 C435 120.03(12) . . ? C433 C434 C435 108.7(6) . . ? C456 C435 C431 120.19(19) . . ? C456 C435 C434 119.97(13) . . ? C431 C435 C434 106.8(6) . . ? C431 C436 C437 120.04(13) . . ? C431 C436 C440 120.00(12) . . ? C437 C436 C440 108.3(6) . . ? C460 C437 C436 120.22(16) . . ? C460 C437 C438 120.10(13) . . ? C436 C437 C438 106.3(6) . . ? C419 C438 C439 119.87(12) . . ? C419 C438 C437 119.82(12) . . ? C439 C438 C437 110.5(6) . . ? C423 C439 C438 120.11(13) . . ? C423 C439 C440 119.99(13) . . ? C438 C439 C440 105.5(6) . . ? C442 C440 C439 119.96(12) . . ? C442 C440 C436 120.00(12) . . ? C439 C440 C436 109.3(6) . . ? C432 C441 C445 120.09(12) . . ? C432 C441 C442 120.02(12) . . ? C445 C441 C442 108.7(6) . . ? C440 C442 C443 120.00(12) . . ? C440 C442 C441 120.01(12) . . ? C443 C442 C441 108.8(7) . . ? C424 C443 C442 120.01(13) . . ? C424 C443 C444 120.05(13) . . ? C442 C443 C444 105.9(7) . . ? C428 C444 C443 119.97(12) . . ? C428 C444 C445 120.00(12) . . ? C443 C444 C445 110.6(6) . . ? C447 C445 C441 120.02(13) . . ? C447 C445 C444 119.93(13) . . ? C441 C445 C444 106.0(6) . . ? C433 C446 C447 120.01(13) . . ? C433 C446 C450 120.14(13) . . ? C447 C446 C450 105.6(6) . . ? C445 C447 C446 119.82(12) . . ? C445 C447 C448 119.93(12) . . ? C446 C447 C448 111.3(6) . . ? C429 C448 C447 119.98(13) . . ? C429 C448 C449 120.12(13) . . ? C447 C448 C449 105.3(7) . . ? C408 C449 C448 119.98(12) . . ? C408 C449 C450 120.05(12) . . ? C448 C449 C450 109.1(6) . . ? C452 C450 C446 119.88(12) . . ? C452 C450 C449 120.07(12) . . ? C446 C450 C449 108.7(6) . . ? C434 C451 C452 120.03(12) . . ? C434 C451 C455 120.03(13) . . ? C452 C451 C455 106.8(6) . . ? C450 C452 C451 119.98(12) . . ? C450 C452 C453 119.82(12) . . ? C451 C452 C453 108.1(6) . . ? C409 C453 C454 119.94(12) . . ? C409 C453 C452 120.05(12) . . ? C454 C453 C452 109.0(6) . . ? C413 C454 C453 120.05(13) . . ? C413 C454 C455 120.01(13) . . ? C453 C454 C455 106.5(6) . . ? C457 C455 C454 119.93(12) . . ? C457 C455 C451 119.92(12) . . ? C454 C455 C451 109.6(6) . . ? C435 C456 C460 119.65(18) . . ? C435 C456 C457 120.01(12) . . ? C460 C456 C457 109.4(7) . . ? C455 C457 C458 119.89(13) . . ? C455 C457 C456 119.94(13) . . ? C458 C457 C456 105.2(7) . . ? C414 C458 C457 119.95(12) . . ? C414 C458 C459 119.79(12) . . ? C457 C458 C459 111.0(6) . . ? C418 C459 C458 119.98(13) . . ? C418 C459 C460 119.86(13) . . ? C458 C459 C460 105.7(7) . . ? C437 C460 C456 120.08(13) . . ? C437 C460 C459 119.98(12) . . ? C456 C460 C459 108.6(7) . . ? C706 C701 C702 121.4(18) . . ? C706 C701 C705 121.8(19) . . ? C702 C701 C705 104.2(16) . . ? C711 C702 C703 118.0(18) . . ? C711 C702 C701 114.2(18) . . ? C703 C702 C701 113.3(16) . . ? C716 C703 C702 123.4(18) . . ? C716 C703 C704 121.6(18) . . ? C702 C703 C704 103.3(15) . . ? C721 C704 C705 121.8(19) . . ? C721 C704 C703 111.8(17) . . ? C705 C704 C703 111.1(16) . . ? C726 C705 C704 127.9(19) . . ? C726 C705 C701 115.8(18) . . ? C704 C705 C701 107.9(16) . . ? C710 C706 C701 122(2) . . ? C710 C706 C707 105.9(16) . . ? C701 C706 C707 119(2) . . ? C730 C707 C708 123(2) . . ? C730 C707 C706 115(2) . . ? C708 C707 C706 109.2(17) . . ? C749 C708 C707 118.0(19) . . ? C749 C708 C709 126(2) . . ? C707 C708 C709 106.6(16) . . ? C753 C709 C710 126(2) . . ? C753 C709 C708 115(2) . . ? C710 C709 C708 105.9(16) . . ? C706 C710 C709 112.2(17) . . ? C706 C710 C712 117.1(18) . . ? C709 C710 C712 117.8(17) . . ? C702 C711 C712 126.1(19) . . ? C702 C711 C715 118.3(18) . . ? C712 C711 C715 106.4(16) . . ? C713 C712 C711 109.7(17) . . ? C713 C712 C710 114.4(17) . . ? C711 C712 C710 118.6(18) . . ? C754 C713 C714 116.4(17) . . ? C754 C713 C712 129.6(18) . . ? C714 C713 C712 109.9(15) . . ? C713 C714 C758 114.7(19) . . ? C713 C714 C715 104.4(16) . . ? C758 C714 C715 119.7(19) . . ? C717 C715 C711 122.9(18) . . ? C717 C715 C714 121.0(18) . . ? C711 C715 C714 107.8(15) . . ? C717 C716 C703 117.6(18) . . ? C717 C716 C720 111.6(16) . . ? C703 C716 C720 122.4(19) . . ? C715 C717 C716 119(2) . . ? C715 C717 C718 120(2) . . ? C716 C717 C718 104.1(16) . . ? C759 C718 C719 120.3(18) . . ? C759 C718 C717 118(2) . . ? C719 C718 C717 112.0(16) . . ? C738 C719 C718 130(2) . . ? C738 C719 C720 116(2) . . ? C718 C719 C720 104.6(15) . . ? C722 C720 C716 117.7(19) . . ? C722 C720 C719 118(2) . . ? C716 C720 C719 107.4(16) . . ? C704 C721 C722 128.4(19) . . ? C704 C721 C725 109.7(17) . . ? C722 C721 C725 110.9(16) . . ? C720 C722 C723 127(2) . . ? C720 C722 C721 117.9(18) . . ? C723 C722 C721 103.8(16) . . ? C739 C723 C724 128.6(18) . . ? C739 C723 C722 113.9(17) . . ? C724 C723 C722 111.8(16) . . ? C743 C724 C723 118.6(19) . . ? C743 C724 C725 118.1(19) . . ? C723 C724 C725 109.0(17) . . ? C727 C725 C724 117.6(18) . . ? C727 C725 C721 129.6(19) . . ? C724 C725 C721 103.8(15) . . ? C705 C726 C730 122(2) . . ? C705 C726 C727 114(2) . . ? C730 C726 C727 103.5(17) . . ? C725 C727 C728 122.5(17) . . ? C725 C727 C726 115.6(17) . . ? C728 C727 C726 117.2(16) . . ? C744 C728 C727 116(2) . . ? C744 C728 C729 119(2) . . ? C727 C728 C729 98.6(16) . . ? C748 C729 C728 117(2) . . ? C748 C729 C730 120(2) . . ? C728 C729 C730 112.4(16) . . ? C707 C730 C726 125(2) . . ? C707 C730 C729 116.4(19) . . ? C726 C730 C729 107.0(16) . . ? C732 C731 C736 120.0(18) . . ? C732 C731 C735 106.1(16) . . ? C736 C731 C735 118.2(17) . . ? C741 C732 C731 123.9(18) . . ? C741 C732 C733 123.3(18) . . ? C731 C732 C733 108.7(15) . . ? C746 C733 C734 120.0(19) . . ? C746 C733 C732 118.0(19) . . ? C734 C733 C732 108.5(17) . . ? C751 C734 C733 119.0(18) . . ? C751 C734 C735 120.9(19) . . ? C733 C734 C735 108.8(16) . . ? C756 C735 C734 117.6(19) . . ? C756 C735 C731 125(2) . . ? C734 C735 C731 107.4(15) . . ? C740 C736 C737 121.2(18) . . ? C740 C736 C731 112.3(16) . . ? C737 C736 C731 114.8(17) . . ? C760 C737 C738 127(2) . . ? C760 C737 C736 124(2) . . ? C738 C737 C736 97.6(15) . . ? C719 C738 C737 111.0(19) . . ? C719 C738 C739 124(2) . . ? C737 C738 C739 110.2(16) . . ? C723 C739 C740 106.5(19) . . ? C723 C739 C738 119(2) . . ? C740 C739 C738 111.0(18) . . ? C742 C740 C739 128(2) . . ? C742 C740 C736 125.7(19) . . ? C739 C740 C736 98.3(15) . . ? C732 C741 C745 112.4(19) . . ? C732 C741 C742 117(2) . . ? C745 C741 C742 111.8(17) . . ? C740 C742 C743 121.4(19) . . ? C740 C742 C741 120.1(18) . . ? C743 C742 C741 109.9(16) . . ? C724 C743 C742 116.2(19) . . ? C724 C743 C744 124(2) . . ? C742 C743 C744 102.3(17) . . ? C728 C744 C743 118.8(17) . . ? C728 C744 C745 118.3(18) . . ? C743 C744 C745 117.2(16) . . ? C747 C745 C741 130.2(19) . . ? C747 C745 C744 124.6(19) . . ? C741 C745 C744 98.2(15) . . ? C733 C746 C750 124(2) . . ? C733 C746 C747 121.5(19) . . ? C750 C746 C747 101.8(16) . . ? C745 C747 C746 113(2) . . ? C745 C747 C748 113(2) . . ? C746 C747 C748 112.7(18) . . ? C729 C748 C749 119(2) . . ? C729 C748 C747 126(2) . . ? C749 C748 C747 106.0(16) . . ? C708 C749 C748 123(2) . . ? C708 C749 C750 116(2) . . ? C748 C749 C750 103.5(17) . . ? C746 C750 C752 117.9(17) . . ? C746 C750 C749 115.1(16) . . ? C752 C750 C749 121.4(17) . . ? C734 C751 C755 122.2(19) . . ? C734 C751 C752 120.9(19) . . ? C755 C751 C752 106.3(15) . . ? C750 C752 C753 118.7(19) . . ? C750 C752 C751 117.5(18) . . ? C753 C752 C751 105.2(16) . . ? C709 C753 C752 121.6(18) . . ? C709 C753 C754 117.6(18) . . ? C752 C753 C754 113.7(16) . . ? C713 C754 C753 114.0(19) . . ? C713 C754 C755 127(2) . . ? C753 C754 C755 103.2(15) . . ? C757 C755 C754 117.3(18) . . ? C757 C755 C751 116.7(18) . . ? C754 C755 C751 111.0(17) . . ? C735 C756 C760 116(2) . . ? C735 C756 C757 125(2) . . ? C760 C756 C757 104.4(16) . . ? C758 C757 C755 112.4(18) . . ? C758 C757 C756 113.1(17) . . ? C755 C757 C756 117.9(18) . . ? C714 C758 C757 131(2) . . ? C714 C758 C759 114.3(18) . . ? C757 C758 C759 106.2(16) . . ? C718 C759 C758 126(2) . . ? C718 C759 C760 114.6(18) . . ? C758 C759 C760 105.3(15) . . ? C737 C760 C756 122(2) . . ? C737 C760 C759 117.0(18) . . ? C756 C760 C759 110.6(16) . . ? C502 C501 C506 120.0 . . ? C502 C501 H501 120.0 . . ? C506 C501 H501 120.0 . . ? C501 C502 C503 120.0 . . ? C501 C502 Cl3 136.8(6) . . ? C503 C502 Cl3 102.6(6) . . ? C504 C503 C502 120.0 . . ? C504 C503 Cl4 111.7(6) . . ? C502 C503 Cl4 128.3(6) . . ? C503 C504 C505 120.0 . . ? C503 C504 H504 120.0 . . ? C505 C504 H504 120.0 . . ? C506 C505 C504 120.0 . . ? C506 C505 H505 120.0 . . ? C504 C505 H505 120.0 . . ? C505 C506 C501 120.0 . . ? C505 C506 H506 120.0 . . ? C501 C506 H506 120.0 . . ? C806 C801 C802 105.7(15) . . ? C806 C801 H801 127.1 . . ? C802 C801 H801 127.1 . . ? C803 C802 C801 124.7(16) . . ? C803 C802 Cl5 100.2(13) . . ? C801 C802 Cl5 134.8(14) . . ? C802 C803 C804 120.8(16) . . ? C802 C803 Cl6 138.5(17) . . ? C804 C803 Cl6 100.3(14) . . ? C805 C804 C803 115.0(18) . . ? C805 C804 H804 122.5 . . ? C803 C804 H804 122.5 . . ? C804 C805 C806 121.8(19) . . ? C804 C805 H805 119.1 . . ? C806 C805 H805 119.1 . . ? C805 C806 C801 124.7(19) . . ? C805 C806 H806 117.6 . . ? C801 C806 H806 117.6 . . ? N5 C307 C306 178.2(2) . . ? C302 C301 C306 120.0 . . ? C302 C301 H301 120.0 . . ? C306 C301 H301 120.0 . . ? C301 C302 C303 120.0 . . ? C301 C302 H302 120.0 . . ? C303 C302 H302 120.0 . . ? C304 C303 C302 120.0 . . ? C304 C303 H303 120.0 . . ? C302 C303 H303 120.0 . . ? C303 C304 C305 120.0 . . ? C303 C304 H304 120.0 . . ? C305 C304 H304 120.0 . . ? C306 C305 C304 120.0 . . ? C306 C305 H305 120.0 . . ? C304 C305 H305 120.0 . . ? C305 C306 C301 120.0 . . ? C305 C306 C307 119.84(6) . . ? C301 C306 C307 119.85(6) . . ? N6 C607 C606 165(3) . . ? C606 C601 C602 118.9(7) . . ? C606 C601 H601 120.6 . . ? C602 C601 H601 120.6 . . ? C603 C602 C601 118.8(8) . . ? C603 C602 H602 120.6 . . ? C601 C602 H602 120.6 . . ? C602 C603 C604 118.9(9) . . ? C602 C603 H603 120.6 . . ? C604 C603 H603 120.6 . . ? C605 C604 C603 116.9(9) . . ? C605 C604 H604 121.6 . . ? C603 C604 H604 121.6 . . ? C606 C605 C604 118.7(8) . . ? C606 C605 H605 120.6 . . ? C604 C605 H605 120.6 . . ? C601 C606 C605 120.7(7) . . ? C601 C606 C607 119.6(4) . . ? C605 C606 C607 119.5(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.549 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.059 data_PPN2_C60_DCB2_100K _database_code_depnum_ccdc_archive 'CCDC 894603' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C60, 2(C36 H30 N P2), 2(C6 H4 Cl2)' _chemical_formula_sum 'C144 H68 Cl4 N2 P4' _chemical_formula_weight 2091.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9324(4) _cell_length_b 23.1418(8) _cell_length_c 17.7613(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.424(3) _cell_angle_gamma 90.00 _cell_volume 4838.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27536 _cell_measurement_theta_min 1.7265 _cell_measurement_theta_max 32.4696 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_T_min 0.90450 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_detector_area_resol_mean 10.4752 _diffrn_measurement_method \w-scans _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 74532 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 32.54 _reflns_number_total 16545 _reflns_number_gt 14193 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+2.6890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16545 _refine_ls_number_parameters 878 _refine_ls_number_restraints 322 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.008 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9773(7) 0.4081(4) 0.2925(4) 0.0152(7) Uani 0.449(4) 1 d PG A 1 C2 C 0.9624(8) 0.4668(4) 0.2774(4) 0.0163(7) Uani 0.449(4) 1 d PG A 1 H2 H 0.9301 0.4908 0.3116 0.020 Uiso 0.449(4) 1 calc PR A 1 C3 C 0.9949(8) 0.4904(5) 0.2123(4) 0.0190(10) Uani 0.449(4) 1 d PG A 1 H3 H 0.9848 0.5305 0.2020 0.023 Uiso 0.449(4) 1 calc PR A 1 C4 C 1.0422(6) 0.4553(7) 0.1623(4) 0.0202(12) Uani 0.449(4) 1 d PG A 1 H4 H 1.0643 0.4714 0.1178 0.024 Uiso 0.449(4) 1 calc PR A 1 C5 C 1.0570(4) 0.3966(7) 0.1773(3) 0.0224(10) Uani 0.449(4) 1 d PG A 1 H5 H 1.0893 0.3726 0.1431 0.027 Uiso 0.449(4) 1 calc PR A 1 C6 C 1.0245(6) 0.3730(5) 0.2424(3) 0.0210(8) Uani 0.449(4) 1 d PG A 1 H6 H 1.0346 0.3329 0.2527 0.025 Uiso 0.449(4) 1 calc PR A 1 C1B C 0.9806(15) 0.4003(6) 0.2896(7) 0.0152(7) Uani 0.159(16) 1 d PG A 2 C2B C 0.9750(13) 0.4587(6) 0.2712(7) 0.0163(7) Uani 0.159(16) 1 d PG A 2 H2B H 0.9458 0.4855 0.3037 0.020 Uiso 0.159(16) 1 calc PR A 2 C3B C 1.0121(13) 0.4780(6) 0.2054(6) 0.0190(10) Uani 0.159(16) 1 d PG A 2 H3B H 1.0083 0.5179 0.1928 0.023 Uiso 0.159(16) 1 calc PR A 2 C4B C 1.0549(12) 0.4388(8) 0.1580(5) 0.0202(12) Uani 0.159(16) 1 d PG A 2 H4B H 1.0803 0.4520 0.1130 0.024 Uiso 0.159(16) 1 calc PR A 2 C5B C 1.0606(10) 0.3804(8) 0.1764(6) 0.0224(10) Uani 0.159(16) 1 d PG A 2 H5B H 1.0898 0.3537 0.1439 0.027 Uiso 0.159(16) 1 calc PR A 2 C6B C 1.0234(14) 0.3611(6) 0.2422(8) 0.0210(8) Uani 0.159(16) 1 d PG A 2 H6B H 1.0273 0.3212 0.2548 0.025 Uiso 0.159(16) 1 calc PR A 2 C1C C 0.9719(12) 0.4153(4) 0.2973(6) 0.0152(7) Uani 0.391(17) 1 d PG A 3 C2C C 0.9500(10) 0.4739(4) 0.2864(6) 0.0163(7) Uani 0.391(17) 1 d PG A 3 H2C H 0.9134 0.4948 0.3215 0.020 Uiso 0.391(17) 1 calc PR A 3 C3C C 0.9817(7) 0.5020(3) 0.2240(6) 0.0190(10) Uani 0.391(17) 1 d PG A 3 H3C H 0.9667 0.5421 0.2164 0.023 Uiso 0.391(17) 1 calc PR A 3 C4C C 1.0353(6) 0.4715(4) 0.1725(5) 0.0202(12) Uani 0.391(17) 1 d PG A 3 H4C H 1.0569 0.4907 0.1299 0.024 Uiso 0.391(17) 1 calc PR A 3 C5C C 1.0572(7) 0.4129(4) 0.1835(5) 0.0224(10) Uani 0.391(17) 1 d PG A 3 H5C H 1.0938 0.3920 0.1484 0.027 Uiso 0.391(17) 1 calc PR A 3 C6C C 1.0255(10) 0.3847(3) 0.2459(5) 0.0210(8) Uani 0.391(17) 1 d PG A 3 H6C H 1.0404 0.3446 0.2534 0.025 Uiso 0.391(17) 1 calc PR A 3 C7 C 0.83699(10) 0.31867(5) 0.34053(7) 0.0158(2) Uani 1 1 d . A . C8 C 0.78581(12) 0.31511(6) 0.26413(7) 0.0229(3) Uani 1 1 d . . . H8 H 0.8049 0.3421 0.2280 0.027 Uiso 1 1 calc R . . C9 C 0.70654(14) 0.27173(6) 0.24129(9) 0.0291(3) Uani 1 1 d . . . H9 H 0.6710 0.2694 0.1895 0.035 Uiso 1 1 calc R . . C10 C 0.67935(12) 0.23209(6) 0.29370(9) 0.0274(3) Uani 1 1 d . . . H10 H 0.6266 0.2020 0.2776 0.033 Uiso 1 1 calc R . . C11 C 0.72894(12) 0.23614(6) 0.36972(9) 0.0247(3) Uani 1 1 d . . . H11 H 0.7095 0.2091 0.4057 0.030 Uiso 1 1 calc R . . C12 C 0.80668(11) 0.27953(6) 0.39353(7) 0.0192(2) Uani 1 1 d . . . H12 H 0.8393 0.2826 0.4459 0.023 Uiso 1 1 calc R . . C13 C 0.84700(11) 0.42722(5) 0.41724(7) 0.0179(2) Uani 1 1 d . A . C14 C 0.88495(12) 0.45141(6) 0.48827(8) 0.0237(3) Uani 1 1 d . . . H14 H 0.9572 0.4410 0.5158 0.028 Uiso 1 1 calc R . . C15 C 0.81718(14) 0.49089(7) 0.51909(9) 0.0308(3) Uani 1 1 d . . . H15 H 0.8433 0.5075 0.5677 0.037 Uiso 1 1 calc R . . C16 C 0.71192(14) 0.50614(7) 0.47922(10) 0.0327(3) Uani 1 1 d . . . H16 H 0.6660 0.5332 0.5004 0.039 Uiso 1 1 calc R . . C17 C 0.67355(15) 0.48187(8) 0.40839(11) 0.0418(4) Uani 1 1 d . . . H17 H 0.6012 0.4923 0.3811 0.050 Uiso 1 1 calc R . . C18 C 0.74041(14) 0.44239(8) 0.37723(9) 0.0343(4) Uani 1 1 d . . . H18 H 0.7137 0.4257 0.3287 0.041 Uiso 1 1 calc R . . C19 C 1.07704(10) 0.23740(5) 0.42950(6) 0.01386(19) Uani 1 1 d . A . C20 C 1.06649(11) 0.21762(5) 0.35428(7) 0.0184(2) Uani 1 1 d . . . H20 H 1.0975 0.2395 0.3173 0.022 Uiso 1 1 calc R . . C21 C 1.01043(12) 0.16586(6) 0.33367(8) 0.0241(3) Uani 1 1 d . . . H21 H 1.0022 0.1527 0.2824 0.029 Uiso 1 1 calc R . . C22 C 0.96653(12) 0.13350(6) 0.38774(8) 0.0235(3) Uani 1 1 d . . . H22 H 0.9278 0.0984 0.3733 0.028 Uiso 1 1 calc R . . C23 C 0.97896(11) 0.15222(6) 0.46287(8) 0.0210(2) Uani 1 1 d . . . H23 H 0.9506 0.1294 0.5000 0.025 Uiso 1 1 calc R . . C24 C 1.03293(11) 0.20449(5) 0.48381(7) 0.0174(2) Uani 1 1 d . . . H24 H 1.0398 0.2178 0.5350 0.021 Uiso 1 1 calc R . . C25 C 1.18716(10) 0.30896(5) 0.55321(6) 0.01395(19) Uani 1 1 d . A . C26 C 1.25337(11) 0.26234(5) 0.58544(7) 0.0191(2) Uani 1 1 d . . . H26 H 1.2678 0.2306 0.5544 0.023 Uiso 1 1 calc R . . C27 C 1.29768(13) 0.26265(6) 0.66271(7) 0.0243(3) Uani 1 1 d . . . H27 H 1.3416 0.2308 0.6848 0.029 Uiso 1 1 calc R . . C28 C 1.27801(13) 0.30937(6) 0.70792(7) 0.0246(3) Uani 1 1 d . . . H28 H 1.3082 0.3093 0.7608 0.030 Uiso 1 1 calc R . . C29 C 1.21441(12) 0.35610(6) 0.67603(7) 0.0237(3) Uani 1 1 d . . . H29 H 1.2021 0.3882 0.7070 0.028 Uiso 1 1 calc R . . C30 C 1.16850(11) 0.35606(5) 0.59870(7) 0.0181(2) Uani 1 1 d . . . H30 H 1.1246 0.3880 0.5770 0.022 Uiso 1 1 calc R . . C31 C 1.24629(10) 0.32138(5) 0.40217(6) 0.0143(2) Uani 1 1 d . A . C32 C 1.32381(10) 0.27748(5) 0.39410(7) 0.0178(2) Uani 1 1 d . . . H32 H 1.3129 0.2398 0.4128 0.021 Uiso 1 1 calc R . . C33 C 1.41684(11) 0.28896(6) 0.35867(8) 0.0220(2) Uani 1 1 d . . . H33 H 1.4698 0.2592 0.3536 0.026 Uiso 1 1 calc R . . C34 C 1.43267(12) 0.34399(6) 0.33059(8) 0.0238(3) Uani 1 1 d . . . H34 H 1.4963 0.3517 0.3063 0.029 Uiso 1 1 calc R . . C35 C 1.35564(13) 0.38763(6) 0.33811(8) 0.0246(3) Uani 1 1 d . . . H35 H 1.3664 0.4251 0.3187 0.030 Uiso 1 1 calc R . . C36 C 1.26256(11) 0.37671(5) 0.37406(7) 0.0193(2) Uani 1 1 d . . . H36 H 1.2102 0.4067 0.3795 0.023 Uiso 1 1 calc R . . N1 N 1.03585(9) 0.35803(4) 0.43900(6) 0.01520(18) Uani 1 1 d . A . P1 P 0.93216(3) 0.376185(13) 0.375605(17) 0.01390(6) Uani 1 1 d . . . P2 P 1.12968(2) 0.308873(12) 0.453118(16) 0.01191(6) Uani 1 1 d . . . C41 C 0.3296(5) 0.3728(3) 0.9787(2) 0.0215(6) Uani 0.6483(14) 1 d PD B 1 C42 C 0.4389(5) 0.3494(4) 1.0121(4) 0.0241(8) Uani 0.6483(14) 1 d PD B 1 C43 C 0.5285(7) 0.3494(6) 0.9700(4) 0.0257(7) Uani 0.6483(14) 1 d PD B 1 C44 C 0.5127(5) 0.3711(3) 0.8936(3) 0.0230(7) Uani 0.6483(14) 1 d PD B 1 C45 C 0.4065(4) 0.3941(3) 0.8602(5) 0.0207(6) Uani 0.6483(14) 1 d PD B 1 C46 C 0.3122(4) 0.3951(2) 0.9031(3) 0.0188(7) Uani 0.6483(14) 1 d PD B 1 C47 C 0.2838(3) 0.40408(12) 1.03751(16) 0.0235(4) Uani 0.6483(14) 1 d PD B 1 C48 C 0.3649(3) 0.40019(13) 1.10772(15) 0.0271(5) Uani 0.6483(14) 1 d PD B 1 C49 C 0.4605(4) 0.3666(3) 1.0914(3) 0.0254(6) Uani 0.6483(14) 1 d PD B 1 C50 C 0.5714(3) 0.38275(15) 1.12698(17) 0.0296(6) Uani 0.6483(14) 1 d PD . 1 C51 C 0.6635(2) 0.38214(9) 1.08375(14) 0.0288(5) Uani 0.6483(14) 1 d PD . 1 C52 C 0.6444(3) 0.36614(15) 1.00725(19) 0.0272(5) Uani 0.6483(14) 1 d PD B 1 C53 C 0.6974(4) 0.3986(2) 0.9522(3) 0.0303(8) Uani 0.6483(14) 1 d PD B 1 C54 C 0.6169(6) 0.4011(4) 0.8813(4) 0.0295(6) Uani 0.6483(14) 1 d PD B 1 C55 C 0.6102(2) 0.45094(14) 0.83774(16) 0.0298(5) Uani 0.6483(14) 1 d PD . 1 C56 C 0.5009(2) 0.47423(12) 0.80275(12) 0.0288(5) Uani 0.6483(14) 1 d PD B 1 C57 C 0.4014(3) 0.44544(19) 0.8138(3) 0.0246(4) Uani 0.6483(14) 1 d PD B 1 C58 C 0.3043(2) 0.47816(11) 0.83000(16) 0.0212(5) Uani 0.6483(14) 1 d PD B 1 C59 C 0.2497(8) 0.4463(3) 0.8844(4) 0.0201(5) Uani 0.6483(14) 1 d PD B 1 C60 C 0.2035(4) 0.47601(17) 0.9406(2) 0.0240(6) Uani 0.6483(14) 1 d PD B 1 C61 C 0.22186(19) 0.45436(11) 1.01833(14) 0.0232(4) Uani 0.6483(14) 1 d PD B 1 C62 C 0.2396(2) 0.50315(13) 1.07031(18) 0.0294(5) Uani 0.6483(14) 1 d PD . 1 C63 C 0.3157(3) 0.50012(13) 1.1382(2) 0.0303(6) Uani 0.6483(14) 1 d PD . 1 C64 C 0.3808(2) 0.44760(12) 1.15728(13) 0.0308(5) Uani 0.6483(14) 1 d PD . 1 C65 C 0.76818(18) 0.44524(12) 0.97564(17) 0.0294(5) Uani 0.6483(14) 1 d PD . 1 C66 C 0.5058(3) 0.53655(15) 0.80557(17) 0.0306(6) Uani 0.6483(14) 1 d PD . 1 C67 C 0.4130(3) 0.56830(13) 0.82106(15) 0.0284(5) Uani 0.6483(14) 1 d PD . 1 C68 C 0.3108(2) 0.53876(10) 0.83399(13) 0.0246(4) Uani 0.6483(14) 1 d PD B 1 C69 C 0.2620(2) 0.56965(10) 0.89118(18) 0.0251(5) Uani 0.6483(14) 1 d PD . 1 C70 C 0.21070(19) 0.53878(11) 0.94394(17) 0.0262(5) Uani 0.6483(14) 1 d PD . 1 C71 C 0.5188(15) 0.3673(9) 0.9077(9) 0.0230(7) Uani 0.2286(9) 1 d PD B 2 C72 C 0.4204(14) 0.3902(9) 0.8619(13) 0.0207(6) Uani 0.2286(9) 1 d PD B 2 C73 C 0.3249(16) 0.3968(8) 0.8936(10) 0.0188(7) Uani 0.2286(9) 1 d PD B 2 C74 C 0.3202(15) 0.3802(7) 0.9687(8) 0.0215(6) Uani 0.2286(9) 1 d PD B 2 C75 C 0.4140(12) 0.3554(8) 1.0145(9) 0.0241(8) Uani 0.2286(9) 1 d PD B 2 C76 C 0.5202(14) 0.3474(12) 0.9825(9) 0.0257(7) Uani 0.2286(9) 1 d PD B 2 C77 C 0.6132(17) 0.3992(11) 0.8879(14) 0.0295(6) Uani 0.2286(9) 1 d PD B 2 C78 C 0.5727(8) 0.4423(4) 0.8310(5) 0.0298(5) Uani 0.2286(9) 1 d PD B 2 C79 C 0.4541(7) 0.4386(3) 0.8155(4) 0.0246(4) Uani 0.2286(9) 1 d PD B 2 C80 C 0.3877(6) 0.4886(3) 0.8040(3) 0.0246(4) Uani 0.2286(9) 1 d PD . 2 C81 C 0.2874(7) 0.4957(3) 0.8362(5) 0.0212(5) Uani 0.2286(9) 1 d PD . 2 C82 C 0.254(2) 0.4513(8) 0.8804(12) 0.0201(5) Uani 0.2286(9) 1 d PD B 2 C83 C 0.2120(15) 0.4649(5) 0.9509(9) 0.0240(6) Uani 0.2286(9) 1 d PD B 2 C84 C 0.2480(5) 0.4201(3) 1.0056(4) 0.0235(4) Uani 0.2286(9) 1 d PD B 2 C85 C 0.2807(5) 0.4337(3) 1.0822(4) 0.0235(4) Uani 0.2286(9) 1 d PD . 2 C86 C 0.3774(9) 0.4109(4) 1.1280(5) 0.0271(5) Uani 0.2286(9) 1 d PD B 2 C87 C 0.4433(12) 0.3713(9) 1.0940(10) 0.0254(6) Uani 0.2286(9) 1 d PD B 2 C88 C 0.5640(11) 0.3730(5) 1.1073(5) 0.0296(6) Uani 0.2286(9) 1 d PD B 2 C89 C 0.6114(5) 0.3597(3) 1.0392(4) 0.0272(5) Uani 0.2286(9) 1 d PD B 2 C90 C 0.7061(5) 0.3887(2) 1.0210(5) 0.0272(5) Uani 0.2286(9) 1 d PD B 2 C91 C 0.7080(15) 0.4083(7) 0.9439(9) 0.0303(8) Uani 0.2286(9) 1 d PD B 2 C92 C 0.7627(6) 0.4661(4) 0.9452(5) 0.0294(5) Uani 0.2286(9) 1 d PD . 2 C93 C 0.7225(8) 0.5065(4) 0.8918(5) 0.0303(6) Uani 0.2286(9) 1 d PD . 2 C94 C 0.6280(7) 0.4953(3) 0.8340(4) 0.0303(6) Uani 0.2286(9) 1 d PD . 2 C95 C 0.2041(6) 0.5216(3) 0.9721(5) 0.0262(5) Uani 0.2286(9) 1 d PD . 2 C96 C 0.4381(9) 0.4530(3) 1.1789(4) 0.0308(5) Uani 0.2286(9) 1 d PD . 2 C97 C 0.5551(9) 0.4546(4) 1.1934(4) 0.0306(6) Uani 0.2286(9) 1 d PD . 2 C98 C 0.6216(7) 0.4153(3) 1.1561(4) 0.0284(5) Uani 0.2286(9) 1 d PD B 2 C99 C 0.7196(6) 0.4455(3) 1.1389(5) 0.0251(5) Uani 0.2286(9) 1 d PD . 2 C100 C 0.7610(6) 0.4331(3) 1.0715(5) 0.0251(5) Uani 0.2286(9) 1 d PD . 2 C101 C 0.4905(13) 0.3689(10) 0.8952(12) 0.0230(7) Uani 0.1231(5) 1 d PD B 3 C102 C 0.3807(11) 0.3928(7) 0.8708(9) 0.0207(6) Uani 0.1231(5) 1 d PD B 3 C103 C 0.3014(17) 0.3938(8) 0.9167(9) 0.0188(7) Uani 0.1231(5) 1 d PD B 3 C104 C 0.3257(17) 0.3763(10) 0.9927(9) 0.0215(6) Uani 0.1231(5) 1 d PD B 3 C105 C 0.4337(16) 0.3542(14) 1.0232(11) 0.0241(8) Uani 0.1231(5) 1 d PD B 3 C106 C 0.5192(17) 0.3480(16) 0.9719(10) 0.0257(7) Uani 0.1231(5) 1 d PD B 3 C107 C 0.5731(10) 0.4024(6) 0.8647(8) 0.0295(6) Uani 0.1231(5) 1 d PD B 3 C108 C 0.5177(12) 0.4471(5) 0.8171(7) 0.0288(5) Uani 0.1231(5) 1 d PD B 3 C109 C 0.3988(16) 0.4408(9) 0.8198(17) 0.0246(4) Uani 0.1231(5) 1 d PD B 3 C110 C 0.3305(11) 0.4912(6) 0.8199(8) 0.0212(5) Uani 0.1231(5) 1 d PD . 3 C111 C 0.2456(9) 0.4922(4) 0.8666(6) 0.0212(5) Uani 0.1231(5) 1 d PD . 3 C112 C 0.2289(9) 0.4484(5) 0.9146(6) 0.0201(5) Uani 0.1231(5) 1 d PD B 3 C113 C 0.2123(12) 0.4602(5) 0.9904(8) 0.0232(4) Uani 0.1231(5) 1 d PD B 3 C114 C 0.2650(14) 0.4157(7) 1.0381(9) 0.0235(4) Uani 0.1231(5) 1 d PD B 3 C115 C 0.3282(11) 0.4259(6) 1.1111(7) 0.0271(5) Uani 0.1231(5) 1 d PD . 3 C116 C 0.4367(10) 0.4042(5) 1.1414(6) 0.0271(5) Uani 0.1231(5) 1 d PD B 3 C117 C 0.4933(10) 0.3672(7) 1.0984(8) 0.0254(6) Uani 0.1231(5) 1 d PD B 3 C118 C 0.6099(11) 0.3730(5) 1.0931(7) 0.0288(5) Uani 0.1231(5) 1 d PD B 3 C119 C 0.6238(13) 0.3599(9) 1.0155(9) 0.0272(5) Uani 0.1231(5) 1 d PD B 3 C120 C 0.7037(11) 0.3928(6) 0.9848(8) 0.0303(8) Uani 0.1231(5) 1 d PD B 3 C121 C 0.6799(10) 0.4136(5) 0.9068(8) 0.0303(8) Uani 0.1231(5) 1 d PD B 3 C122 C 0.7283(10) 0.4718(5) 0.9028(8) 0.0294(5) Uani 0.1231(5) 1 d PD . 3 C123 C 0.6691(14) 0.5155(7) 0.8590(11) 0.0303(6) Uani 0.1231(5) 1 d PD . 3 C124 C 0.5601(12) 0.5028(5) 0.8125(6) 0.0306(6) Uani 0.1231(5) 1 d PD . 3 C125 C 0.2125(10) 0.5163(5) 1.0189(9) 0.0294(5) Uani 0.1231(5) 1 d PD . 3 C126 C 0.5077(13) 0.4485(9) 1.1849(11) 0.0306(6) Uani 0.1231(5) 1 d PD . 3 C127 C 0.6239(11) 0.4521(6) 1.1841(6) 0.0284(5) Uani 0.1231(5) 1 d PD . 3 C128 C 0.6784(9) 0.4154(4) 1.1357(6) 0.0251(5) Uani 0.1231(5) 1 d PD B 3 C129 C 0.7596(11) 0.4482(6) 1.1022(7) 0.0251(5) Uani 0.1231(5) 1 d PD . 3 C130 C 0.7732(9) 0.4384(5) 1.0271(8) 0.0294(5) Uani 0.1231(5) 1 d PD . 3 C1S C 0.26114(13) 0.66270(7) 0.39479(8) 0.0277(3) Uani 1 1 d . . . C2S C 0.29878(13) 0.61642(7) 0.35630(8) 0.0274(3) Uani 1 1 d . . . C3S C 0.41433(14) 0.60603(8) 0.36078(9) 0.0328(3) Uani 1 1 d . . . H3S H 0.4400 0.5741 0.3346 0.039 Uiso 1 1 calc R . . C4S C 0.49202(14) 0.64263(9) 0.40376(10) 0.0393(4) Uani 1 1 d . . . H4S H 0.5712 0.6358 0.4069 0.047 Uiso 1 1 calc R . . C5S C 0.45436(16) 0.68902(9) 0.44203(10) 0.0401(4) Uani 1 1 d . . . H5S H 0.5079 0.7140 0.4712 0.048 Uiso 1 1 calc R . . C6S C 0.33938(15) 0.69916(8) 0.43807(9) 0.0339(3) Uani 1 1 d . . . H6S H 0.3138 0.7309 0.4647 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.11775(4) 0.67703(2) 0.38890(3) 0.04073(10) Uani 1 1 d . . . Cl2 Cl 0.20355(4) 0.57106(2) 0.30084(2) 0.03876(10) 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 0.0151(11) 0.0164(18) 0.0142(10) 0.0019(13) 0.0020(6) 0.0027(15) C2 0.013(2) 0.0164(18) 0.0195(17) 0.0013(13) 0.0026(9) 0.0010(14) C3 0.0124(19) 0.017(2) 0.027(2) 0.0068(18) 0.0020(13) -0.0016(15) C4 0.0133(12) 0.026(3) 0.0221(15) 0.006(2) 0.0054(9) -0.0001(19) C5 0.0204(7) 0.029(4) 0.0193(11) 0.000(2) 0.0070(7) 0.007(2) C6 0.0260(7) 0.018(2) 0.0194(8) 0.0035(19) 0.0057(7) 0.008(2) C1B 0.0151(11) 0.0164(18) 0.0142(10) 0.0019(13) 0.0020(6) 0.0027(15) C2B 0.013(2) 0.0164(18) 0.0195(17) 0.0013(13) 0.0026(9) 0.0010(14) C3B 0.0124(19) 0.017(2) 0.027(2) 0.0068(18) 0.0020(13) -0.0016(15) C4B 0.0133(12) 0.026(3) 0.0221(15) 0.006(2) 0.0054(9) -0.0001(19) C5B 0.0204(7) 0.029(4) 0.0193(11) 0.000(2) 0.0070(7) 0.007(2) C6B 0.0260(7) 0.018(2) 0.0194(8) 0.0035(19) 0.0057(7) 0.008(2) C1C 0.0151(11) 0.0164(18) 0.0142(10) 0.0019(13) 0.0020(6) 0.0027(15) C2C 0.013(2) 0.0164(18) 0.0195(17) 0.0013(13) 0.0026(9) 0.0010(14) C3C 0.0124(19) 0.017(2) 0.027(2) 0.0068(18) 0.0020(13) -0.0016(15) C4C 0.0133(12) 0.026(3) 0.0221(15) 0.006(2) 0.0054(9) -0.0001(19) C5C 0.0204(7) 0.029(4) 0.0193(11) 0.000(2) 0.0070(7) 0.007(2) C6C 0.0260(7) 0.018(2) 0.0194(8) 0.0035(19) 0.0057(7) 0.008(2) C7 0.0154(5) 0.0143(5) 0.0170(5) -0.0005(4) 0.0004(4) 0.0016(4) C8 0.0296(7) 0.0179(6) 0.0184(5) 0.0009(4) -0.0040(5) 0.0011(5) C9 0.0331(7) 0.0225(6) 0.0266(7) -0.0042(5) -0.0099(6) 0.0005(5) C10 0.0233(6) 0.0176(6) 0.0388(8) -0.0044(5) -0.0029(6) -0.0023(5) C11 0.0207(6) 0.0199(6) 0.0334(7) 0.0031(5) 0.0042(5) -0.0016(5) C12 0.0170(5) 0.0203(6) 0.0204(5) 0.0020(4) 0.0032(4) 0.0002(4) C13 0.0184(5) 0.0147(5) 0.0200(5) -0.0002(4) 0.0014(4) 0.0031(4) C14 0.0245(6) 0.0209(6) 0.0234(6) -0.0044(5) -0.0027(5) 0.0063(5) C15 0.0355(8) 0.0267(7) 0.0287(7) -0.0093(5) 0.0007(6) 0.0097(6) C16 0.0310(8) 0.0283(7) 0.0383(8) -0.0095(6) 0.0040(6) 0.0118(6) C17 0.0291(8) 0.0469(10) 0.0447(9) -0.0156(8) -0.0079(7) 0.0216(7) C18 0.0278(7) 0.0400(8) 0.0309(7) -0.0128(6) -0.0080(6) 0.0163(6) C19 0.0132(5) 0.0125(5) 0.0157(5) -0.0010(4) 0.0019(4) 0.0003(4) C20 0.0194(5) 0.0189(5) 0.0172(5) -0.0037(4) 0.0043(4) -0.0020(4) C21 0.0250(6) 0.0230(6) 0.0249(6) -0.0105(5) 0.0062(5) -0.0048(5) C22 0.0202(6) 0.0165(5) 0.0344(7) -0.0077(5) 0.0059(5) -0.0047(4) C23 0.0196(6) 0.0164(5) 0.0274(6) 0.0022(4) 0.0044(5) -0.0029(4) C24 0.0180(5) 0.0167(5) 0.0174(5) 0.0008(4) 0.0028(4) -0.0022(4) C25 0.0145(5) 0.0146(5) 0.0125(4) -0.0006(4) 0.0011(4) -0.0014(4) C26 0.0231(6) 0.0164(5) 0.0160(5) -0.0014(4) -0.0022(4) 0.0027(4) C27 0.0317(7) 0.0201(6) 0.0177(5) 0.0013(4) -0.0058(5) 0.0025(5) C28 0.0328(7) 0.0253(6) 0.0135(5) -0.0017(5) -0.0029(5) -0.0028(5) C29 0.0303(7) 0.0228(6) 0.0170(5) -0.0063(5) 0.0011(5) 0.0007(5) C30 0.0210(6) 0.0165(5) 0.0161(5) -0.0022(4) 0.0012(4) 0.0009(4) C31 0.0149(5) 0.0151(5) 0.0126(4) 0.0000(4) 0.0016(4) -0.0015(4) C32 0.0171(5) 0.0175(5) 0.0188(5) 0.0020(4) 0.0030(4) 0.0010(4) C33 0.0176(6) 0.0258(6) 0.0236(6) -0.0003(5) 0.0059(5) 0.0020(5) C34 0.0217(6) 0.0297(7) 0.0216(6) -0.0008(5) 0.0088(5) -0.0059(5) C35 0.0296(7) 0.0213(6) 0.0245(6) 0.0035(5) 0.0093(5) -0.0056(5) C36 0.0233(6) 0.0151(5) 0.0204(5) 0.0006(4) 0.0064(5) -0.0009(4) N1 0.0157(4) 0.0144(4) 0.0147(4) 0.0001(3) -0.0001(3) 0.0030(3) P1 0.01522(13) 0.01316(13) 0.01298(12) 0.00147(10) 0.00125(10) 0.00135(10) P2 0.01329(13) 0.01122(12) 0.01092(12) -0.00015(9) 0.00112(9) 0.00002(9) C41 0.0258(11) 0.0124(14) 0.0256(16) 0.0009(11) 0.0019(11) -0.0097(8) C42 0.034(2) 0.0078(17) 0.0285(13) 0.0009(11) -0.0006(14) -0.0051(13) C43 0.0301(13) 0.0094(9) 0.0340(17) -0.0057(15) -0.0050(11) 0.0022(11) C44 0.0231(11) 0.0178(11) 0.0270(18) -0.0144(13) 0.0014(14) 0.0005(9) C45 0.0227(17) 0.0188(11) 0.0197(8) -0.0101(8) 0.0011(12) -0.0023(11) C46 0.0155(17) 0.0167(7) 0.0236(19) -0.0051(11) 0.0013(10) -0.0073(10) C47 0.0201(12) 0.0230(12) 0.0287(9) 0.0016(8) 0.0079(8) -0.0109(8) C48 0.0339(12) 0.0260(14) 0.0229(13) 0.0065(10) 0.0085(10) -0.0147(9) C49 0.0321(19) 0.0163(13) 0.0246(8) 0.0095(7) -0.0053(12) -0.0085(15) C50 0.0325(11) 0.0203(15) 0.0299(17) 0.0164(11) -0.0136(12) -0.0066(9) C51 0.0257(11) 0.0149(9) 0.0398(12) 0.0038(8) -0.0131(10) 0.0049(8) C52 0.0191(12) 0.0124(10) 0.0468(14) -0.0068(9) -0.0043(8) 0.0066(8) C53 0.0191(12) 0.0259(19) 0.0467(17) -0.0148(14) 0.0080(13) 0.0068(11) C54 0.0232(10) 0.0304(10) 0.0380(16) -0.0200(9) 0.0139(11) 0.0012(8) C55 0.0244(14) 0.0446(14) 0.0234(10) -0.0169(9) 0.0131(12) -0.0064(12) C56 0.0324(11) 0.0437(15) 0.0110(8) -0.0069(9) 0.0058(8) -0.0079(11) C57 0.0311(10) 0.0281(9) 0.0128(9) -0.0071(7) -0.0017(8) -0.0055(9) C58 0.0214(11) 0.0213(15) 0.0171(8) -0.0024(9) -0.0082(7) -0.0060(9) C59 0.0161(9) 0.0194(12) 0.0218(11) -0.0003(8) -0.0058(7) -0.0057(10) C60 0.0095(11) 0.0291(18) 0.0308(15) -0.0029(11) -0.0040(11) -0.0007(12) C61 0.0146(8) 0.0304(11) 0.0260(11) -0.0032(10) 0.0076(9) -0.0084(7) C62 0.0169(10) 0.0361(14) 0.0391(14) -0.0138(10) 0.0163(10) -0.0053(9) C63 0.0296(15) 0.0426(15) 0.0235(12) -0.0128(13) 0.0190(10) -0.0114(12) C64 0.0345(14) 0.0421(13) 0.0185(10) 0.0047(9) 0.0126(9) -0.0161(11) C65 0.0127(7) 0.0315(13) 0.0433(15) -0.0160(11) 0.0027(10) 0.0077(8) C66 0.0410(15) 0.0422(19) 0.0093(9) 0.0034(9) 0.0067(10) -0.0133(13) C67 0.0324(15) 0.0353(15) 0.0143(11) 0.0135(10) -0.0062(8) -0.0141(10) C68 0.0266(11) 0.0210(10) 0.0205(9) 0.0073(8) -0.0131(8) -0.0043(8) C69 0.0205(10) 0.0154(10) 0.0333(14) 0.0037(9) -0.0134(10) 0.0027(7) C70 0.0133(8) 0.0233(13) 0.0388(16) -0.0019(9) -0.0051(9) 0.0061(8) C71 0.0231(11) 0.0178(11) 0.0270(18) -0.0144(13) 0.0014(14) 0.0005(9) C72 0.0227(17) 0.0188(11) 0.0197(8) -0.0101(8) 0.0011(12) -0.0023(11) C73 0.0155(17) 0.0167(7) 0.0236(19) -0.0051(11) 0.0013(10) -0.0073(10) C74 0.0258(11) 0.0124(14) 0.0256(16) 0.0009(11) 0.0019(11) -0.0097(8) C75 0.034(2) 0.0078(17) 0.0285(13) 0.0009(11) -0.0006(14) -0.0051(13) C76 0.0301(13) 0.0094(9) 0.0340(17) -0.0057(15) -0.0050(11) 0.0022(11) C77 0.0232(10) 0.0304(10) 0.0380(16) -0.0200(9) 0.0139(11) 0.0012(8) C78 0.0244(14) 0.0446(14) 0.0234(10) -0.0169(9) 0.0131(12) -0.0064(12) C79 0.0311(10) 0.0281(9) 0.0128(9) -0.0071(7) -0.0017(8) -0.0055(9) C80 0.0311(10) 0.0281(9) 0.0128(9) -0.0071(7) -0.0017(8) -0.0055(9) C81 0.0214(11) 0.0213(15) 0.0171(8) -0.0024(9) -0.0082(7) -0.0060(9) C82 0.0161(9) 0.0194(12) 0.0218(11) -0.0003(8) -0.0058(7) -0.0057(10) C83 0.0095(11) 0.0291(18) 0.0308(15) -0.0029(11) -0.0040(11) -0.0007(12) C84 0.0201(12) 0.0230(12) 0.0287(9) 0.0016(8) 0.0079(8) -0.0109(8) C85 0.0201(12) 0.0230(12) 0.0287(9) 0.0016(8) 0.0079(8) -0.0109(8) C86 0.0339(12) 0.0260(14) 0.0229(13) 0.0065(10) 0.0085(10) -0.0147(9) C87 0.0321(19) 0.0163(13) 0.0246(8) 0.0095(7) -0.0053(12) -0.0085(15) C88 0.0325(11) 0.0203(15) 0.0299(17) 0.0164(11) -0.0136(12) -0.0066(9) C89 0.0191(12) 0.0124(10) 0.0468(14) -0.0068(9) -0.0043(8) 0.0066(8) C90 0.0191(12) 0.0124(10) 0.0468(14) -0.0068(9) -0.0043(8) 0.0066(8) C91 0.0191(12) 0.0259(19) 0.0467(17) -0.0148(14) 0.0080(13) 0.0068(11) C92 0.0127(7) 0.0315(13) 0.0433(15) -0.0160(11) 0.0027(10) 0.0077(8) C93 0.0296(15) 0.0426(15) 0.0235(12) -0.0128(13) 0.0190(10) -0.0114(12) C94 0.0296(15) 0.0426(15) 0.0235(12) -0.0128(13) 0.0190(10) -0.0114(12) C95 0.0133(8) 0.0233(13) 0.0388(16) -0.0019(9) -0.0051(9) 0.0061(8) C96 0.0345(14) 0.0421(13) 0.0185(10) 0.0047(9) 0.0126(9) -0.0161(11) C97 0.0410(15) 0.0422(19) 0.0093(9) 0.0034(9) 0.0067(10) -0.0133(13) C98 0.0324(15) 0.0353(15) 0.0143(11) 0.0135(10) -0.0062(8) -0.0141(10) C99 0.0205(10) 0.0154(10) 0.0333(14) 0.0037(9) -0.0134(10) 0.0027(7) C100 0.0205(10) 0.0154(10) 0.0333(14) 0.0037(9) -0.0134(10) 0.0027(7) C101 0.0231(11) 0.0178(11) 0.0270(18) -0.0144(13) 0.0014(14) 0.0005(9) C102 0.0227(17) 0.0188(11) 0.0197(8) -0.0101(8) 0.0011(12) -0.0023(11) C103 0.0155(17) 0.0167(7) 0.0236(19) -0.0051(11) 0.0013(10) -0.0073(10) C104 0.0258(11) 0.0124(14) 0.0256(16) 0.0009(11) 0.0019(11) -0.0097(8) C105 0.034(2) 0.0078(17) 0.0285(13) 0.0009(11) -0.0006(14) -0.0051(13) C106 0.0301(13) 0.0094(9) 0.0340(17) -0.0057(15) -0.0050(11) 0.0022(11) C107 0.0232(10) 0.0304(10) 0.0380(16) -0.0200(9) 0.0139(11) 0.0012(8) C108 0.0324(11) 0.0437(15) 0.0110(8) -0.0069(9) 0.0058(8) -0.0079(11) C109 0.0311(10) 0.0281(9) 0.0128(9) -0.0071(7) -0.0017(8) -0.0055(9) C110 0.0214(11) 0.0213(15) 0.0171(8) -0.0024(9) -0.0082(7) -0.0060(9) C111 0.0214(11) 0.0213(15) 0.0171(8) -0.0024(9) -0.0082(7) -0.0060(9) C112 0.0161(9) 0.0194(12) 0.0218(11) -0.0003(8) -0.0058(7) -0.0057(10) C113 0.0146(8) 0.0304(11) 0.0260(11) -0.0032(10) 0.0076(9) -0.0084(7) C114 0.0201(12) 0.0230(12) 0.0287(9) 0.0016(8) 0.0079(8) -0.0109(8) C115 0.0339(12) 0.0260(14) 0.0229(13) 0.0065(10) 0.0085(10) -0.0147(9) C116 0.0339(12) 0.0260(14) 0.0229(13) 0.0065(10) 0.0085(10) -0.0147(9) C117 0.0321(19) 0.0163(13) 0.0246(8) 0.0095(7) -0.0053(12) -0.0085(15) C118 0.0257(11) 0.0149(9) 0.0398(12) 0.0038(8) -0.0131(10) 0.0049(8) C119 0.0191(12) 0.0124(10) 0.0468(14) -0.0068(9) -0.0043(8) 0.0066(8) C120 0.0191(12) 0.0259(19) 0.0467(17) -0.0148(14) 0.0080(13) 0.0068(11) C121 0.0191(12) 0.0259(19) 0.0467(17) -0.0148(14) 0.0080(13) 0.0068(11) C122 0.0169(10) 0.0361(14) 0.0391(14) -0.0138(10) 0.0163(10) -0.0053(9) C123 0.0296(15) 0.0426(15) 0.0235(12) -0.0128(13) 0.0190(10) -0.0114(12) C124 0.0410(15) 0.0422(19) 0.0093(9) 0.0034(9) 0.0067(10) -0.0133(13) C125 0.0169(10) 0.0361(14) 0.0391(14) -0.0138(10) 0.0163(10) -0.0053(9) C126 0.0410(15) 0.0422(19) 0.0093(9) 0.0034(9) 0.0067(10) -0.0133(13) C127 0.0324(15) 0.0353(15) 0.0143(11) 0.0135(10) -0.0062(8) -0.0141(10) C128 0.0205(10) 0.0154(10) 0.0333(14) 0.0037(9) -0.0134(10) 0.0027(7) C129 0.0205(10) 0.0154(10) 0.0333(14) 0.0037(9) -0.0134(10) 0.0027(7) C130 0.0127(7) 0.0315(13) 0.0433(15) -0.0160(11) 0.0027(10) 0.0077(8) C1S 0.0250(7) 0.0376(8) 0.0218(6) -0.0025(5) 0.0077(5) -0.0070(6) C2S 0.0268(7) 0.0362(8) 0.0193(6) -0.0050(5) 0.0044(5) -0.0115(6) C3S 0.0282(7) 0.0453(9) 0.0257(7) -0.0021(6) 0.0073(6) -0.0030(6) C4S 0.0243(7) 0.0608(12) 0.0319(8) 0.0007(8) 0.0020(6) -0.0084(7) C5S 0.0353(9) 0.0563(11) 0.0273(7) -0.0059(7) 0.0013(6) -0.0218(8) C6S 0.0404(9) 0.0398(9) 0.0230(6) -0.0071(6) 0.0096(6) -0.0135(7) Cl1 0.02876(19) 0.0562(3) 0.0394(2) -0.00712(18) 0.01209(16) -0.00075(17) Cl2 0.0359(2) 0.0474(2) 0.03196(18) -0.01454(16) 0.00251(15) -0.01457(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.3900 . ? C1 C6 1.3900 . ? C1 P1 1.809(3) . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B P1 1.807(9) . ? C2B C3B 1.3900 . ? C2B H2B 0.9500 . ? C3B C4B 1.3900 . ? C3B H3B 0.9500 . ? C4B C5B 1.3900 . ? C4B H4B 0.9500 . ? C5B C6B 1.3900 . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C1C P1 1.786(6) . ? C2C C3C 1.3900 . ? C2C H2C 0.9500 . ? C3C C4C 1.3900 . ? C3C H3C 0.9500 . ? C4C C5C 1.3900 . ? C4C H4C 0.9500 . ? C5C C6C 1.3900 . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? C7 C12 1.3962(17) . ? C7 C8 1.3963(17) . ? C7 P1 1.7938(12) . ? C8 C9 1.393(2) . ? C8 H8 0.9500 . ? C9 C10 1.383(2) . ? C9 H9 0.9500 . ? C10 C11 1.386(2) . ? C10 H10 0.9500 . ? C11 C12 1.3853(18) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3868(18) . ? C13 C18 1.3964(18) . ? C13 P1 1.7945(13) . ? C14 C15 1.3903(19) . ? C14 H14 0.9500 . ? C15 C16 1.383(2) . ? C15 H15 0.9500 . ? C16 C17 1.385(2) . ? C16 H16 0.9500 . ? C17 C18 1.386(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.3978(16) . ? C19 C20 1.3983(16) . ? C19 P2 1.7944(12) . ? C20 C21 1.3915(18) . ? C20 H20 0.9500 . ? C21 C22 1.386(2) . ? C21 H21 0.9500 . ? C22 C23 1.3875(19) . ? C22 H22 0.9500 . ? C23 C24 1.3919(17) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.3961(16) . ? C25 C26 1.4029(16) . ? C25 P2 1.7977(11) . ? C26 C27 1.3876(17) . ? C26 H26 0.9500 . ? C27 C28 1.3895(19) . ? C27 H27 0.9500 . ? C28 C29 1.387(2) . ? C28 H28 0.9500 . ? C29 C30 1.3930(17) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.3970(17) . ? C31 C36 1.3992(16) . ? C31 P2 1.8031(12) . ? C32 C33 1.3884(18) . ? C32 H32 0.9500 . ? C33 C34 1.392(2) . ? C33 H33 0.9500 . ? C34 C35 1.387(2) . ? C34 H34 0.9500 . ? C35 C36 1.3918(18) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N1 P2 1.5869(10) . ? N1 P1 1.5872(10) . ? C41 C46 1.422(5) . ? C41 C42 1.447(6) . ? C41 C47 1.448(6) . ? C42 C43 1.403(7) . ? C42 C49 1.446(7) . ? C43 C44 1.430(7) . ? C43 C52 1.483(8) . ? C44 C45 1.412(6) . ? C44 C54 1.472(7) . ? C45 C57 1.441(7) . ? C45 C46 1.459(6) . ? C46 C59 1.410(7) . ? C47 C61 1.390(3) . ? C47 C48 1.451(4) . ? C48 C64 1.400(4) . ? C48 C49 1.448(5) . ? C49 C50 1.419(5) . ? C50 C51 1.440(5) . ? C50 C67 1.454(4) 3_667 ? C51 C52 1.391(4) . ? C51 C69 1.450(3) 3_667 ? C52 C53 1.457(5) . ? C53 C65 1.392(5) . ? C53 C54 1.455(6) . ? C54 C55 1.384(7) . ? C55 C56 1.453(4) . ? C55 C63 1.457(4) 3_667 ? C56 C57 1.403(4) . ? C56 C66 1.444(4) . ? C57 C58 1.452(4) . ? C58 C68 1.406(3) . ? C58 C59 1.452(5) . ? C59 C60 1.397(6) . ? C60 C61 1.452(5) . ? C60 C70 1.456(5) . ? C61 C62 1.452(3) . ? C62 C63 1.387(4) . ? C62 C65 1.441(4) 3_667 ? C63 C64 1.452(4) . ? C63 C55 1.457(4) 3_667 ? C64 C66 1.452(4) 3_667 ? C65 C62 1.441(4) 3_667 ? C65 C70 1.457(4) 3_667 ? C66 C67 1.393(4) . ? C66 C64 1.452(4) 3_667 ? C67 C68 1.448(3) . ? C67 C50 1.454(4) 3_667 ? C68 C69 1.441(4) . ? C69 C70 1.397(4) . ? C69 C51 1.450(3) 3_667 ? C70 C65 1.457(4) 3_667 ? C71 C76 1.404(16) . ? C71 C72 1.417(16) . ? C71 C77 1.438(18) . ? C72 C73 1.361(15) . ? C72 C79 1.485(16) . ? C73 C74 1.398(15) . ? C73 C82 1.519(17) . ? C74 C75 1.395(15) . ? C74 C84 1.486(15) . ? C75 C87 1.446(17) . ? C75 C76 1.482(16) . ? C76 C89 1.386(16) . ? C77 C91 1.395(16) . ? C77 C78 1.445(15) . ? C78 C94 1.390(9) . ? C78 C79 1.399(10) . ? C79 C80 1.398(9) . ? C80 C81 1.417(10) . ? C80 C97 1.479(11) 3_667 ? C81 C82 1.393(15) . ? C81 C99 1.438(11) 3_667 ? C82 C83 1.454(16) . ? C83 C95 1.374(13) . ? C83 C84 1.436(12) . ? C84 C85 1.389(9) . ? C85 C86 1.401(11) . ? C85 C93 1.463(10) 3_667 ? C86 C87 1.406(14) . ? C86 C96 1.440(11) . ? C87 C88 1.420(15) . ? C88 C98 1.411(10) . ? C88 C89 1.449(12) . ? C89 C90 1.398(9) . ? C90 C91 1.447(14) . ? C90 C100 1.447(8) . ? C91 C92 1.487(13) . ? C92 C93 1.362(11) . ? C92 C95 1.485(12) 3_667 ? C93 C94 1.419(11) . ? C93 C85 1.463(10) 3_667 ? C94 C96 1.431(12) 3_667 ? C95 C100 1.405(11) 3_667 ? C95 C92 1.485(12) 3_667 ? C96 C97 1.378(11) . ? C96 C94 1.431(12) 3_667 ? C97 C98 1.438(11) . ? C97 C80 1.479(10) 3_667 ? C98 C99 1.437(10) . ? C99 C100 1.398(11) . ? C99 C81 1.438(11) 3_667 ? C100 C95 1.405(11) 3_667 ? C101 C102 1.422(15) . ? C101 C107 1.427(16) . ? C101 C106 1.434(17) . ? C102 C103 1.347(14) . ? C102 C109 1.472(17) . ? C103 C104 1.392(15) . ? C103 C112 1.530(16) . ? C104 C105 1.409(17) . ? C104 C114 1.483(16) . ? C105 C117 1.438(17) . ? C105 C106 1.483(18) . ? C106 C119 1.384(18) . ? C107 C121 1.392(13) . ? C107 C108 1.429(14) . ? C108 C124 1.392(13) . ? C108 C109 1.435(15) . ? C109 C110 1.422(16) . ? C110 C111 1.411(13) . ? C110 C127 1.427(18) 3_667 ? C111 C112 1.359(12) . ? C111 C129 1.492(16) 3_667 ? C112 C113 1.419(13) . ? C113 C125 1.393(13) . ? C113 C114 1.414(14) . ? C114 C115 1.408(14) . ? C115 C116 1.412(13) . ? C115 C123 1.45(2) 3_667 ? C116 C117 1.393(14) . ? C116 C126 1.466(14) . ? C117 C118 1.416(14) . ? C118 C128 1.414(12) . ? C118 C119 1.447(15) . ? C119 C120 1.400(13) . ? C120 C121 1.449(14) . ? C120 C130 1.470(13) . ? C121 C122 1.472(13) . ? C122 C123 1.396(14) . ? C122 C125 1.478(19) 3_667 ? C123 C124 1.452(15) . ? C123 C115 1.45(2) 3_667 ? C124 C126 1.39(2) 3_667 ? C125 C130 1.36(2) 3_667 ? C125 C122 1.478(19) 3_667 ? C126 C127 1.391(15) . ? C126 C124 1.39(2) 3_667 ? C127 C110 1.427(18) 3_667 ? C127 C128 1.437(13) . ? C128 C129 1.435(13) . ? C129 C130 1.389(14) . ? C129 C111 1.492(16) 3_667 ? C130 C125 1.36(2) 3_667 ? C1S C2S 1.384(2) . ? C1S C6S 1.393(2) . ? C1S Cl1 1.7291(16) . ? C2S C3S 1.389(2) . ? C2S Cl2 1.7311(14) . ? C3S C4S 1.388(2) . ? C3S H3S 0.9500 . ? C4S C5S 1.384(3) . ? C4S H4S 0.9500 . ? C5S C6S 1.382(3) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? 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 C2 C1 C6 120.0 . . ? C2 C1 P1 120.7(3) . . ? C6 C1 P1 119.3(3) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 119.3(6) . . ? C6B C1B P1 120.7(6) . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2B 120.0 . . ? C3B C2B H2B 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B H4B 120.0 . . ? C5B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B H6B 120.0 . . ? C1B C6B H6B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C P1 122.4(4) . . ? C6C C1C P1 117.6(4) . . ? C1C C2C C3C 120.0 . . ? C1C C2C H2C 120.0 . . ? C3C C2C H2C 120.0 . . ? C4C C3C C2C 120.0 . . ? C4C C3C H3C 120.0 . . ? C2C C3C H3C 120.0 . . ? C3C C4C C5C 120.0 . . ? C3C C4C H4C 120.0 . . ? C5C C4C H4C 120.0 . . ? C4C C5C C6C 120.0 . . ? C4C C5C H5C 120.0 . . ? C6C C5C H5C 120.0 . . ? C5C C6C C1C 120.0 . . ? C5C C6C H6C 120.0 . . ? C1C C6C H6C 120.0 . . ? C12 C7 C8 119.78(12) . . ? C12 C7 P1 117.80(9) . . ? C8 C7 P1 122.18(10) . . ? C9 C8 C7 119.57(13) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.32(13) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.08(13) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.28(13) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 119.92(12) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 119.74(12) . . ? C14 C13 P1 121.20(10) . . ? C18 C13 P1 119.06(10) . . ? C13 C14 C15 119.94(13) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.28(14) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.93(14) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.23(15) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 119.88(14) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C24 C19 C20 119.72(11) . . ? C24 C19 P2 119.86(9) . . ? C20 C19 P2 119.90(9) . . ? C21 C20 C19 119.82(12) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.18(12) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.29(12) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 120.02(12) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 119.94(11) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C30 C25 C26 119.79(11) . . ? C30 C25 P2 120.13(9) . . ? C26 C25 P2 120.06(9) . . ? C27 C26 C25 119.84(11) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 120.16(12) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.23(12) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.17(12) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 119.79(12) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C32 C31 C36 119.73(11) . . ? C32 C31 P2 120.87(9) . . ? C36 C31 P2 119.31(9) . . ? C33 C32 C31 119.96(12) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.19(12) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 120.06(12) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.21(12) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 119.84(12) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? P2 N1 P1 138.57(7) . . ? N1 P1 C1C 114.2(5) . . ? N1 P1 C7 115.19(5) . . ? C1C P1 C7 109.8(4) . . ? N1 P1 C13 108.07(6) . . ? C1C P1 C13 103.2(3) . . ? C7 P1 C13 105.21(6) . . ? N1 P1 C1B 111.2(6) . . ? C1C P1 C1B 12.5(6) . . ? C7 P1 C1B 102.0(6) . . ? C13 P1 C1B 115.2(4) . . ? N1 P1 C1 112.7(3) . . ? C1C P1 C1 6.4(4) . . ? C7 P1 C1 106.0(3) . . ? C13 P1 C1 109.4(3) . . ? C1B P1 C1 6.1(3) . . ? N1 P2 C19 114.39(5) . . ? N1 P2 C25 107.49(5) . . ? C19 P2 C25 107.13(5) . . ? N1 P2 C31 112.83(6) . . ? C19 P2 C31 107.46(5) . . ? C25 P2 C31 107.17(5) . . ? C46 C41 C42 120.3(6) . . ? C46 C41 C47 119.1(4) . . ? C42 C41 C47 108.3(4) . . ? C43 C42 C49 119.3(6) . . ? C43 C42 C41 119.8(7) . . ? C49 C42 C41 107.5(4) . . ? C42 C43 C44 120.8(8) . . ? C42 C43 C52 119.9(6) . . ? C44 C43 C52 107.5(6) . . ? C45 C44 C43 120.1(7) . . ? C45 C44 C54 118.8(6) . . ? C43 C44 C54 108.8(5) . . ? C44 C45 C57 120.1(5) . . ? C44 C45 C46 120.1(6) . . ? C57 C45 C46 108.8(4) . . ? C59 C46 C41 121.1(4) . . ? C59 C46 C45 108.3(4) . . ? C41 C46 C45 118.8(5) . . ? C61 C47 C41 119.3(3) . . ? C61 C47 C48 121.0(3) . . ? C41 C47 C48 108.1(3) . . ? C64 C48 C49 121.0(3) . . ? C64 C48 C47 119.7(3) . . ? C49 C48 C47 107.3(3) . . ? C50 C49 C42 120.7(5) . . ? C50 C49 C48 118.5(5) . . ? C42 C49 C48 108.8(4) . . ? C49 C50 C51 119.8(3) . . ? C49 C50 C67 120.1(4) . 3_667 ? C51 C50 C67 108.4(3) . 3_667 ? C52 C51 C50 120.4(2) . . ? C52 C51 C69 119.9(3) . 3_667 ? C50 C51 C69 108.2(2) . 3_667 ? C51 C52 C53 119.9(3) . . ? C51 C52 C43 119.8(4) . . ? C53 C52 C43 108.1(4) . . ? C65 C53 C54 120.7(4) . . ? C65 C53 C52 120.6(4) . . ? C54 C53 C52 107.7(4) . . ? C55 C54 C53 119.1(6) . . ? C55 C54 C44 120.2(5) . . ? C53 C54 C44 107.9(5) . . ? C54 C55 C56 121.0(4) . . ? C54 C55 C63 120.5(4) . 3_667 ? C56 C55 C63 107.2(3) . 3_667 ? C57 C56 C66 120.0(3) . . ? C57 C56 C55 119.0(3) . . ? C66 C56 C55 109.1(3) . . ? C56 C57 C45 120.9(4) . . ? C56 C57 C58 120.1(4) . . ? C45 C57 C58 106.1(3) . . ? C68 C58 C57 119.4(3) . . ? C68 C58 C59 120.0(4) . . ? C57 C58 C59 109.1(3) . . ? C60 C59 C46 120.1(5) . . ? C60 C59 C58 119.8(5) . . ? C46 C59 C58 107.8(4) . . ? C59 C60 C61 119.6(3) . . ? C59 C60 C70 119.5(4) . . ? C61 C60 C70 107.8(3) . . ? C47 C61 C60 120.9(3) . . ? C47 C61 C62 118.6(3) . . ? C60 C61 C62 108.7(3) . . ? C63 C62 C65 120.4(2) . 3_667 ? C63 C62 C61 121.3(3) . . ? C65 C62 C61 107.2(2) 3_667 . ? C62 C63 C64 119.6(3) . . ? C62 C63 C55 119.7(3) . 3_667 ? C64 C63 C55 107.8(3) . 3_667 ? C48 C64 C66 120.3(3) . 3_667 ? C48 C64 C63 119.8(3) . . ? C66 C64 C63 108.5(3) 3_667 . ? C53 C65 C62 119.6(3) . 3_667 ? C53 C65 C70 119.3(3) . 3_667 ? C62 C65 C70 109.2(2) 3_667 3_667 ? C67 C66 C56 120.3(3) . . ? C67 C66 C64 119.3(2) . 3_667 ? C56 C66 C64 107.3(3) . 3_667 ? C66 C67 C68 119.9(3) . . ? C66 C67 C50 120.8(3) . 3_667 ? C68 C67 C50 106.9(3) . 3_667 ? C58 C68 C69 120.3(2) . . ? C58 C68 C67 120.3(3) . . ? C69 C68 C67 109.0(2) . . ? C70 C69 C68 119.4(2) . . ? C70 C69 C51 120.1(3) . 3_667 ? C68 C69 C51 107.5(2) . 3_667 ? C69 C70 C60 120.8(3) . . ? C69 C70 C65 120.2(2) . 3_667 ? C60 C70 C65 107.1(3) . 3_667 ? C76 C71 C72 123.1(17) . . ? C76 C71 C77 120.8(15) . . ? C72 C71 C77 106.0(13) . . ? C73 C72 C71 118.4(18) . . ? C73 C72 C79 117.8(14) . . ? C71 C72 C79 109.1(13) . . ? C72 C73 C74 122.1(16) . . ? C72 C73 C82 121.0(14) . . ? C74 C73 C82 105.5(12) . . ? C75 C74 C73 121.0(15) . . ? C75 C74 C84 117.8(12) . . ? C73 C74 C84 111.5(10) . . ? C74 C75 C87 120.5(13) . . ? C74 C75 C76 118.9(15) . . ? C87 C75 C76 108.7(12) . . ? C89 C76 C71 120.5(15) . . ? C89 C76 C75 108.3(12) . . ? C71 C76 C75 116.3(17) . . ? C91 C77 C71 118.6(15) . . ? C91 C77 C78 122.2(15) . . ? C71 C77 C78 109.9(13) . . ? C94 C78 C79 121.3(9) . . ? C94 C78 C77 118.7(11) . . ? C79 C78 C77 107.9(10) . . ? C80 C79 C78 120.7(7) . . ? C80 C79 C72 120.4(9) . . ? C78 C79 C72 107.1(9) . . ? C79 C80 C81 122.2(6) . . ? C79 C80 C97 118.8(7) . 3_667 ? C81 C80 C97 107.5(7) . 3_667 ? C82 C81 C80 118.9(10) . . ? C82 C81 C99 119.2(11) . 3_667 ? C80 C81 C99 109.3(7) . 3_667 ? C81 C82 C83 119.9(15) . . ? C81 C82 C73 119.6(15) . . ? C83 C82 C73 107.9(12) . . ? C95 C83 C84 122.0(12) . . ? C95 C83 C82 119.3(13) . . ? C84 C83 C82 108.7(10) . . ? C85 C84 C83 120.3(8) . . ? C85 C84 C74 118.8(8) . . ? C83 C84 C74 106.3(9) . . ? C84 C85 C86 123.9(6) . . ? C84 C85 C93 120.4(7) . 3_667 ? C86 C85 C93 103.5(7) . 3_667 ? C85 C86 C87 117.4(9) . . ? C85 C86 C96 113.1(8) . . ? C87 C86 C96 116.7(11) . . ? C86 C87 C88 122.3(14) . . ? C86 C87 C75 121.5(13) . . ? C88 C87 C75 104.2(11) . . ? C98 C88 C87 120.0(11) . . ? C98 C88 C89 116.3(9) . . ? C87 C88 C89 112.3(9) . . ? C76 C89 C90 119.9(10) . . ? C76 C89 C88 106.4(9) . . ? C90 C89 C88 122.1(7) . . ? C89 C90 C91 120.6(8) . . ? C89 C90 C100 120.0(7) . . ? C91 C90 C100 106.8(8) . . ? C77 C91 C90 119.4(13) . . ? C77 C91 C92 116.7(13) . . ? C90 C91 C92 110.0(11) . . ? C93 C92 C95 124.4(8) . 3_667 ? C93 C92 C91 120.2(9) . . ? C95 C92 C91 103.5(9) 3_667 . ? C92 C93 C94 121.8(7) . . ? C92 C93 C85 117.0(8) . 3_667 ? C94 C93 C85 110.0(8) . 3_667 ? C78 C94 C93 120.3(8) . . ? C78 C94 C96 119.1(8) . 3_667 ? C93 C94 C96 108.3(7) . 3_667 ? C83 C95 C100 121.5(10) . 3_667 ? C83 C95 C92 115.8(9) . 3_667 ? C100 C95 C92 110.3(7) 3_667 3_667 ? C97 C96 C94 121.5(8) . 3_667 ? C97 C96 C86 121.7(8) . . ? C94 C96 C86 104.9(9) 3_667 . ? C96 C97 C98 121.0(7) . . ? C96 C97 C80 118.6(9) . 3_667 ? C98 C97 C80 106.8(8) . 3_667 ? C88 C98 C99 122.5(9) . . ? C88 C98 C97 118.1(8) . . ? C99 C98 C97 108.8(7) . . ? C100 C99 C98 119.8(7) . . ? C100 C99 C81 120.3(7) . 3_667 ? C98 C99 C81 107.7(8) . 3_667 ? C99 C100 C95 119.8(6) . 3_667 ? C99 C100 C90 119.2(8) . . ? C95 C100 C90 109.5(7) 3_667 . ? C102 C101 C107 109.5(13) . . ? C102 C101 C106 119.0(17) . . ? C107 C101 C106 118.1(15) . . ? C103 C102 C101 121.7(14) . . ? C103 C102 C109 123.3(14) . . ? C101 C102 C109 105.1(12) . . ? C102 C103 C104 121.8(16) . . ? C102 C103 C112 116.7(13) . . ? C104 C103 C112 106.9(12) . . ? C103 C104 C105 120.7(16) . . ? C103 C104 C114 107.8(13) . . ? C105 C104 C114 120.7(15) . . ? C104 C105 C117 124.3(16) . . ? C104 C105 C106 118.4(18) . . ? C117 C105 C106 107.8(15) . . ? C119 C106 C101 121.2(19) . . ? C119 C106 C105 106.6(16) . . ? C101 C106 C105 118(2) . . ? C121 C107 C101 121.7(12) . . ? C121 C107 C108 118.5(11) . . ? C101 C107 C108 109.6(11) . . ? C124 C108 C107 124.6(12) . . ? C124 C108 C109 117.9(14) . . ? C107 C108 C109 105.7(11) . . ? C110 C109 C108 119.1(16) . . ? C110 C109 C102 118.4(15) . . ? C108 C109 C102 110.0(13) . . ? C111 C110 C109 118.8(12) . . ? C111 C110 C127 109.3(11) . 3_667 ? C109 C110 C127 122.1(13) . 3_667 ? C112 C111 C110 123.3(10) . . ? C112 C111 C129 115.9(10) . 3_667 ? C110 C111 C129 108.1(10) . 3_667 ? C111 C112 C113 120.7(10) . . ? C111 C112 C103 119.4(11) . . ? C113 C112 C103 107.6(9) . . ? C125 C113 C114 119.1(13) . . ? C125 C113 C112 122.1(12) . . ? C114 C113 C112 108.1(10) . . ? C115 C114 C113 123.2(14) . . ? C115 C114 C104 111.6(12) . . ? C113 C114 C104 109.3(12) . . ? C114 C115 C116 127.7(12) . . ? C114 C115 C123 118.0(13) . 3_667 ? C116 C115 C123 103.2(10) . 3_667 ? C117 C116 C115 120.4(10) . . ? C117 C116 C126 115.3(11) . . ? C115 C116 C126 111.5(11) . . ? C116 C117 C118 123.3(12) . . ? C116 C117 C105 115.3(12) . . ? C118 C117 C105 107.5(12) . . ? C128 C118 C117 121.2(11) . . ? C128 C118 C119 120.7(12) . . ? C117 C118 C119 108.1(10) . . ? C106 C119 C120 120.0(16) . . ? C106 C119 C118 109.9(13) . . ? C120 C119 C118 116.6(13) . . ? C119 C120 C121 120.9(12) . . ? C119 C120 C130 123.7(12) . . ? C121 C120 C130 104.9(11) . . ? C107 C121 C120 118.0(11) . . ? C107 C121 C122 118.5(11) . . ? C120 C121 C122 109.5(11) . . ? C123 C122 C121 121.6(12) . . ? C123 C122 C125 120.6(12) . 3_667 ? C121 C122 C125 104.8(11) . 3_667 ? C122 C123 C124 119.6(13) . . ? C122 C123 C115 119.6(13) . 3_667 ? C124 C123 C115 111.2(13) . 3_667 ? C108 C124 C126 121.9(13) . 3_667 ? C108 C124 C123 117.0(12) . . ? C126 C124 C123 106.8(12) 3_667 . ? C130 C125 C113 119.6(13) 3_667 . ? C130 C125 C122 109.6(10) 3_667 3_667 ? C113 C125 C122 119.2(13) . 3_667 ? C127 C126 C124 122.4(15) . 3_667 ? C127 C126 C116 121.9(13) . . ? C124 C126 C116 107.1(12) 3_667 . ? C126 C127 C110 116.4(13) . 3_667 ? C126 C127 C128 121.3(11) . . ? C110 C127 C128 107.5(11) 3_667 . ? C118 C128 C129 121.0(11) . . ? C118 C128 C127 116.9(10) . . ? C129 C128 C127 109.7(10) . . ? C130 C129 C128 120.3(10) . . ? C130 C129 C111 121.8(11) . 3_667 ? C128 C129 C111 105.3(10) . 3_667 ? C125 C130 C129 119.8(11) 3_667 . ? C125 C130 C120 111.2(12) 3_667 . ? C129 C130 C120 117.7(11) . . ? C2S C1S C6S 119.93(15) . . ? C2S C1S Cl1 121.08(11) . . ? C6S C1S Cl1 118.98(13) . . ? C1S C2S C3S 120.32(14) . . ? C1S C2S Cl2 120.95(12) . . ? C3S C2S Cl2 118.73(12) . . ? C4S C3S C2S 119.55(16) . . ? C4S C3S H3S 120.2 . . ? C2S C3S H3S 120.2 . . ? C5S C4S C3S 120.12(16) . . ? C5S C4S H4S 119.9 . . ? C3S C4S H4S 119.9 . . ? C6S C5S C4S 120.39(15) . . ? C6S C5S H5S 119.8 . . ? C4S C5S H5S 119.8 . . ? C5S C6S C1S 119.69(16) . . ? C5S C6S H6S 120.2 . . ? C1S C6S H6S 120.2 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.499 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.060 data_C60_TMP2_DCB2_90K _database_code_depnum_ccdc_archive 'CCDC 894604' _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) SHELXL-97 ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60, 2(C7 H17 N2), 2(C6 H4 Cl2)' _chemical_formula_sum 'C86 H42 Cl4 N4' _chemical_formula_weight 1273.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_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 29.656(3) _cell_length_b 13.5007(9) _cell_length_c 14.8007(15) _cell_angle_alpha 90.00 _cell_angle_beta 113.549(12) _cell_angle_gamma 90.00 _cell_volume 5432.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 10305 _cell_measurement_theta_min 2.9915 _cell_measurement_theta_max 27.8154 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 0.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8761 _exptl_absorpt_correction_T_max 0.9722 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4752 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21952 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6429 _reflns_number_gt 5011 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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 'calc w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+11.1440P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6429 _refine_ls_number_parameters 745 _refine_ls_number_restraints 898 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.04684(7) 0.24904(12) 0.19640(15) 0.0263(4) Uani 1 1 d U . . N2 N 0.12513(8) 0.24821(12) 0.39428(14) 0.0266(4) Uani 1 1 d U . . C1 C 0.07620(9) 0.16021(15) 0.23644(16) 0.0265(4) Uani 1 1 d U . . H1A H 0.1040 0.1591 0.2177 0.032 Uiso 1 1 calc R . . H1B H 0.0564 0.1018 0.2090 0.032 Uiso 1 1 calc R . . C2 C 0.07658(8) 0.33734(15) 0.23706(17) 0.0278(4) Uani 1 1 d U . . H2A H 0.0570 0.3961 0.2099 0.033 Uiso 1 1 calc R . . H2B H 0.1044 0.3381 0.2184 0.033 Uiso 1 1 calc R . . C3 C 0.09441(9) 0.15807(15) 0.34697(17) 0.0309(5) Uani 1 1 d U . . H3A H 0.1140 0.0988 0.3718 0.037 Uiso 1 1 calc R . . H3B H 0.0665 0.1550 0.3653 0.037 Uiso 1 1 calc R . . C4 C 0.09475(9) 0.33902(16) 0.34741(18) 0.0317(5) Uani 1 1 d U . . H4A H 0.0668 0.3425 0.3657 0.038 Uiso 1 1 calc R . . H4B H 0.1146 0.3979 0.3726 0.038 Uiso 1 1 calc R . . C5 C 0.02728(9) 0.24978(16) 0.08988(19) 0.0309(5) Uani 1 1 d U . . H5A H 0.0082 0.1910 0.0648 0.046 Uiso 1 1 calc R . . H5B H 0.0539 0.2518 0.0686 0.046 Uiso 1 1 calc R . . H5C H 0.0068 0.3070 0.0655 0.046 Uiso 1 1 calc R . . C6 C 0.17253(9) 0.24815(15) 0.38215(18) 0.0286(5) Uani 1 1 d U . . H6A H 0.1908 0.1896 0.4118 0.043 Uiso 1 1 calc R . . H6B H 0.1913 0.3057 0.4136 0.043 Uiso 1 1 calc R . . H6C H 0.1661 0.2492 0.3132 0.043 Uiso 1 1 calc R . . C7 C 0.13644(12) 0.24823(19) 0.50218(19) 0.0414(6) Uani 1 1 d U . . H7A H 0.1063 0.2484 0.5118 0.062 Uiso 1 1 calc R . . H7B H 0.1552 0.3062 0.5320 0.062 Uiso 1 1 calc R . . H7C H 0.1551 0.1901 0.5320 0.062 Uiso 1 1 calc R . . C301 C 0.19873(9) 0.98191(15) 0.51827(17) 0.0189(4) Uani 0.878(2) 1 d PDU A 1 C302 C 0.22894(9) 1.00870(17) 0.46559(18) 0.0201(4) Uani 0.878(2) 1 d PDU A 1 C303 C 0.27923(9) 1.00635(18) 0.53208(18) 0.0193(4) Uani 0.878(2) 1 d PDU A 1 C304 C 0.28085(9) 0.97816(19) 0.62830(18) 0.0205(5) Uani 0.878(2) 1 d PDU A 1 C305 C 0.23046(8) 0.96320(16) 0.61960(17) 0.0194(4) Uani 0.878(2) 1 d PDU A 1 C306 C 0.15640(8) 0.92441(16) 0.47257(17) 0.0179(4) Uani 0.878(2) 1 d PDU A 1 C307 C 0.14247(9) 0.89130(18) 0.37097(18) 0.0214(5) Uani 0.878(2) 1 d PDU A 1 C308 C 0.17194(9) 0.91626(18) 0.32070(17) 0.0224(5) Uani 0.878(2) 1 d PDU A 1 C309 C 0.21504(10) 0.97513(18) 0.36713(18) 0.0235(5) Uani 0.878(2) 1 d PDU A 1 C310 C 0.25351(10) 0.93715(17) 0.33750(18) 0.0242(5) Uani 0.878(2) 1 d PDU A 1 C311 C 0.30187(10) 0.93478(17) 0.40276(19) 0.0255(5) Uani 0.878(2) 1 d PDU . 1 C312 C 0.31612(10) 0.9698(2) 0.5030(2) 0.0237(5) Uani 0.878(2) 1 d PDU A 1 C313 C 0.35399(9) 0.90659(18) 0.5665(2) 0.0235(5) Uani 0.878(2) 1 d PDU . 1 C314 C 0.35594(10) 0.87926(19) 0.65958(19) 0.0230(5) Uani 0.878(2) 1 d PDU A 1 C315 C 0.31807(9) 0.9170(2) 0.69041(18) 0.0198(5) Uani 0.878(2) 1 d PDU A 1 C316 C 0.30616(9) 0.8401(2) 0.74506(19) 0.0193(5) Uani 0.878(2) 1 d PDU A 1 C317 C 0.25821(9) 0.82442(19) 0.73618(16) 0.0207(5) Uani 0.878(2) 1 d PDU A 1 C318 C 0.21956(8) 0.88857(17) 0.67177(16) 0.0216(4) Uani 0.878(2) 1 d PDU A 1 C319 C 0.17555(9) 0.82846(18) 0.62410(18) 0.0214(5) Uani 0.878(2) 1 d PDU A 1 C320 C 0.14492(8) 0.84666(17) 0.52661(18) 0.0195(4) Uani 0.878(2) 1 d PDU A 1 C321 C 0.12427(8) 0.76465(18) 0.45897(19) 0.0222(5) Uani 0.878(2) 1 d PDU A 1 C322 C 0.12231(8) 0.79183(18) 0.36319(17) 0.0235(5) Uani 0.878(2) 1 d PDU . 1 C323 C 0.18255(10) 0.8419(2) 0.26034(18) 0.0240(5) Uani 0.878(2) 1 d PDU . 1 C324 C 0.23242(10) 0.85470(18) 0.26929(19) 0.0235(5) Uani 0.878(2) 1 d PDU . 1 C325 C 0.36757(8) 0.78044(19) 0.69488(17) 0.0245(5) Uani 0.878(2) 1 d PDU . 1 C326 C 0.33683(11) 0.7540(2) 0.7464(2) 0.0234(6) Uani 0.878(2) 1 d PDU . 1 C327 C 0.23859(10) 0.7264(2) 0.72870(17) 0.0246(5) Uani 0.878(2) 1 d PDU . 1 C328 C 0.18720(10) 0.72899(19) 0.65888(19) 0.0240(5) Uani 0.878(2) 1 d PDU A 1 C329 C 0.16751(10) 0.65029(19) 0.5949(2) 0.0250(5) Uani 0.878(2) 1 d PDU . 1 C330 C 0.13603(9) 0.66804(18) 0.4943(2) 0.0234(5) Uani 0.878(2) 1 d PDU . 1 C401 C 0.1853(3) 0.9672(4) 0.4990(5) 0.0222(18) Uani 0.122(2) 1 d PDU A 2 C402 C 0.1992(3) 0.9339(5) 0.5997(5) 0.026(2) Uani 0.122(2) 1 d PDU A 2 C403 C 0.1696(3) 0.8512(6) 0.6000(5) 0.025(2) Uani 0.122(2) 1 d PDU A 2 C404 C 0.1366(2) 0.8316(5) 0.4981(5) 0.0222(18) Uani 0.122(2) 1 d PDU A 2 C405 C 0.1463(2) 0.9047(5) 0.4351(5) 0.0207(17) Uani 0.122(2) 1 d PDU A 2 C406 C 0.2210(3) 1.0018(5) 0.4673(5) 0.0208(16) Uani 0.122(2) 1 d PDU A 2 C407 C 0.2727(3) 1.0044(8) 0.5360(5) 0.0220(17) Uani 0.122(2) 1 d PDU A 2 C408 C 0.2860(3) 0.9706(8) 0.6325(6) 0.0226(19) Uani 0.122(2) 1 d PDU A 2 C409 C 0.2496(3) 0.9361(6) 0.6652(5) 0.024(2) Uani 0.122(2) 1 d PDU A 2 C410 C 0.2699(3) 0.8511(7) 0.7309(6) 0.023(2) Uani 0.122(2) 1 d PDU A 2 C411 C 0.2410(4) 0.7713(8) 0.7295(9) 0.026(3) Uani 0.122(2) 1 d PDU . 2 C412 C 0.1893(3) 0.7699(6) 0.6640(5) 0.026(2) Uani 0.122(2) 1 d PDU A 2 C413 C 0.1764(5) 0.6710(6) 0.6298(7) 0.023(2) Uani 0.122(2) 1 d PDU . 2 C414 C 0.1458(4) 0.6514(5) 0.5310(6) 0.0199(19) Uani 0.122(2) 1 d PDU A 2 C415 C 0.1249(3) 0.7350(5) 0.4645(5) 0.0223(18) Uani 0.122(2) 1 d PDU A 2 C416 C 0.1225(3) 0.7087(6) 0.3682(5) 0.025(2) Uani 0.122(2) 1 d PDU A 2 C417 C 0.1319(3) 0.7775(6) 0.3080(5) 0.027(2) Uani 0.122(2) 1 d PDU A 2 C418 C 0.1441(3) 0.8781(6) 0.3431(5) 0.0220(17) Uani 0.122(2) 1 d PDU A 2 C419 C 0.1814(3) 0.9139(6) 0.3102(5) 0.0216(17) Uani 0.122(2) 1 d PDU A 2 C420 C 0.2188(3) 0.9748(6) 0.3714(5) 0.0227(18) Uani 0.122(2) 1 d PDU A 2 C421 C 0.2689(3) 0.9606(7) 0.3802(6) 0.022(2) Uani 0.122(2) 1 d PDU A 2 C422 C 0.3022(3) 0.9790(13) 0.4810(7) 0.0224(19) Uani 0.122(2) 1 d PDU . 2 C423 C 0.3296(3) 0.9084(15) 0.6777(11) 0.022(2) Uani 0.122(2) 1 d PDU . 2 C424 C 0.3205(4) 0.8366(12) 0.7407(14) 0.021(2) Uani 0.122(2) 1 d PDU . 2 C425 C 0.1576(6) 0.5753(6) 0.4775(8) 0.016(2) Uani 0.122(2) 1 d PDU . 2 C426 C 0.1434(6) 0.6085(7) 0.3769(8) 0.018(3) Uani 0.122(2) 1 d PDU . 2 C427 C 0.1606(6) 0.7516(9) 0.2532(11) 0.028(4) Uani 0.122(2) 1 d PDU . 2 C428 C 0.1921(4) 0.8358(8) 0.2565(7) 0.0198(18) Uani 0.122(2) 1 d PDU A 2 C429 C 0.2402(4) 0.8201(11) 0.2666(13) 0.020(2) Uani 0.122(2) 1 d PDU . 2 C430 C 0.2785(3) 0.8851(9) 0.3259(9) 0.021(2) Uani 0.122(2) 1 d PDU . 2 Cl1 Cl -0.08650(3) 0.44883(8) -0.08173(8) 0.0260(2) Uani 0.50 1 d PDU B -1 Cl2 Cl 0.00087(4) 0.40940(9) -0.14595(8) 0.0337(3) Uani 0.50 1 d PDU B -1 C1S C -0.02853(5) 0.49520(16) -0.01292(13) 0.0168(7) Uani 0.50 1 d PGDU B -1 C2S C 0.01001(5) 0.47829(17) -0.04181(14) 0.0203(7) Uani 0.50 1 d PGDU B -1 C3S C 0.05635(5) 0.51715(19) 0.01317(15) 0.0229(8) Uani 0.50 1 d PGDU B -1 H3S H 0.0821 0.5058 -0.0062 0.027 Uiso 0.50 1 calc PR B -1 C4S C 0.06414(5) 0.57293(18) 0.09704(15) 0.0246(8) Uani 0.50 1 d PGDU B -1 H4S H 0.0951 0.5989 0.1338 0.029 Uiso 0.50 1 calc PR B -1 C5S C 0.02559(7) 0.58985(18) 0.12593(14) 0.0244(8) Uani 0.50 1 d PGDU B -1 H5S H 0.0308 0.6272 0.1820 0.029 Uiso 0.50 1 calc PR B -1 C6S C -0.02074(6) 0.55098(18) 0.07095(14) 0.0210(8) Uani 0.50 1 d PGDU B -1 H6S H -0.0465 0.5623 0.0903 0.025 Uiso 0.50 1 calc PR B -1 Cl3 Cl -0.08107(4) 1.05786(8) -0.08836(8) 0.0292(3) Uani 0.50 1 d PDU C -1 Cl4 Cl 0.01610(5) 1.07318(10) -0.12616(9) 0.0398(3) Uani 0.50 1 d PDU C -1 C12S C -0.02745(6) 1.0014(3) -0.00954(19) 0.0185(8) Uani 0.50 1 d PGDU C -1 C11S C 0.01541(6) 1.0087(3) -0.02600(19) 0.0227(9) Uani 0.50 1 d PGDU C -1 C16S C 0.05791(5) 0.9608(2) 0.03652(17) 0.0255(8) Uani 0.50 1 d PGDU C -1 H16S H 0.0866 0.9656 0.0255 0.031 Uiso 0.50 1 calc PR C -1 C15S C 0.05756(7) 0.90556(19) 0.11550(16) 0.0277(8) Uani 0.50 1 d PGDU C -1 H15S H 0.0860 0.8735 0.1573 0.033 Uiso 0.50 1 calc PR C -1 C14S C 0.01470(8) 0.89828(18) 0.13196(15) 0.0229(8) Uani 0.50 1 d PGDU C -1 H14S H 0.0145 0.8613 0.1848 0.027 Uiso 0.50 1 calc PR C -1 C13S C -0.02781(7) 0.9462(2) 0.06945(16) 0.0206(7) Uani 0.50 1 d PGDU C -1 H13S H -0.0565 0.9414 0.0805 0.025 Uiso 0.50 1 calc PR C -1 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 N1 0.0349(10) 0.0151(8) 0.0371(9) 0.0021(7) 0.0231(8) 0.0013(6) N2 0.0466(11) 0.0142(8) 0.0286(9) -0.0001(6) 0.0249(8) 0.0001(7) C1 0.0389(12) 0.0130(8) 0.0339(10) 0.0006(8) 0.0211(9) 0.0001(8) C2 0.0352(11) 0.0130(9) 0.0416(11) 0.0045(8) 0.0219(9) 0.0031(8) C3 0.0515(14) 0.0147(9) 0.0360(11) 0.0022(8) 0.0275(10) -0.0035(9) C4 0.0462(13) 0.0152(9) 0.0426(11) -0.0025(8) 0.0272(10) 0.0043(8) C5 0.0296(11) 0.0265(11) 0.0394(11) 0.0049(9) 0.0165(9) 0.0020(9) C6 0.0386(11) 0.0193(10) 0.0314(12) 0.0015(8) 0.0176(10) 0.0024(8) C7 0.0670(18) 0.0366(13) 0.0312(11) -0.0032(10) 0.0308(12) -0.0046(12) C301 0.0234(10) 0.0092(9) 0.0232(10) -0.0044(7) 0.0085(8) 0.0055(8) C302 0.0286(10) 0.0059(9) 0.0244(10) 0.0013(8) 0.0092(8) 0.0014(8) C303 0.0269(10) 0.0070(9) 0.0234(10) -0.0018(8) 0.0095(8) -0.0047(8) C304 0.0277(10) 0.0120(10) 0.0200(10) -0.0073(8) 0.0076(8) -0.0019(8) C305 0.0224(10) 0.0156(10) 0.0184(10) -0.0084(8) 0.0063(8) 0.0052(8) C306 0.0147(9) 0.0184(10) 0.0200(10) -0.0022(8) 0.0062(8) 0.0091(7) C307 0.0193(10) 0.0232(10) 0.0166(10) 0.0017(8) 0.0018(8) 0.0124(8) C308 0.0285(11) 0.0188(10) 0.0147(10) 0.0041(8) 0.0032(8) 0.0100(8) C309 0.0339(11) 0.0128(10) 0.0196(10) 0.0077(8) 0.0063(9) 0.0058(8) C310 0.0463(12) 0.0133(10) 0.0192(11) 0.0079(8) 0.0196(9) 0.0011(9) C311 0.0375(11) 0.0166(11) 0.0319(11) 0.0021(9) 0.0239(9) -0.0071(9) C312 0.0286(12) 0.0137(11) 0.0338(11) -0.0033(9) 0.0177(9) -0.0092(10) C313 0.0191(11) 0.0195(11) 0.0353(13) -0.0066(10) 0.0146(11) -0.0089(8) C314 0.0161(10) 0.0272(11) 0.0216(12) -0.0128(9) 0.0034(10) -0.0075(9) C315 0.0209(10) 0.0193(10) 0.0156(10) -0.0098(8) 0.0034(8) -0.0026(8) C316 0.0257(11) 0.0202(10) 0.0072(9) -0.0059(7) 0.0014(9) 0.0006(9) C317 0.0306(10) 0.0254(12) 0.0097(9) -0.0028(8) 0.0118(8) 0.0029(9) C318 0.0262(10) 0.0259(10) 0.0150(10) -0.0082(7) 0.0107(8) 0.0063(8) C319 0.0247(10) 0.0258(10) 0.0230(10) -0.0022(8) 0.0192(8) 0.0040(8) C320 0.0158(10) 0.0201(10) 0.0261(10) -0.0035(8) 0.0121(8) 0.0046(8) C321 0.0110(9) 0.0261(11) 0.0307(11) -0.0046(8) 0.0097(8) 0.0006(8) C322 0.0105(9) 0.0300(11) 0.0235(10) -0.0046(9) 0.0000(8) 0.0054(8) C323 0.0348(11) 0.0225(11) 0.0077(9) 0.0037(8) 0.0011(9) 0.0132(9) C324 0.0409(12) 0.0185(12) 0.0122(10) 0.0077(9) 0.0116(9) 0.0035(10) C325 0.0157(10) 0.0302(11) 0.0185(11) -0.0082(9) -0.0027(8) 0.0005(9) C326 0.0216(12) 0.0320(12) 0.0074(12) -0.0009(9) -0.0037(9) 0.0059(9) C327 0.0404(12) 0.0274(12) 0.0132(10) 0.0013(9) 0.0182(9) -0.0004(10) C328 0.0335(11) 0.0254(11) 0.0252(11) 0.0010(8) 0.0244(9) 0.0008(9) C329 0.0296(13) 0.0258(11) 0.0310(12) 0.0006(9) 0.0241(10) -0.0049(9) C330 0.0162(11) 0.0224(10) 0.0367(12) -0.0057(9) 0.0161(10) -0.0081(9) C401 0.026(3) 0.015(4) 0.024(3) -0.001(2) 0.009(2) 0.005(3) C402 0.030(3) 0.024(4) 0.025(3) -0.001(3) 0.011(3) 0.002(3) C403 0.028(3) 0.026(3) 0.025(3) -0.001(2) 0.016(3) 0.003(3) C404 0.019(4) 0.025(2) 0.026(3) 0.001(2) 0.013(2) 0.004(3) C405 0.016(3) 0.021(3) 0.025(2) 0.002(2) 0.008(2) 0.006(3) C406 0.027(2) 0.008(4) 0.025(2) 0.001(3) 0.0065(19) 0.001(3) C407 0.027(2) 0.011(4) 0.025(2) -0.001(3) 0.007(2) -0.002(3) C408 0.029(3) 0.013(4) 0.021(3) -0.006(3) 0.006(2) -0.003(3) C409 0.032(3) 0.020(4) 0.021(4) -0.004(4) 0.010(2) 0.003(3) C410 0.032(3) 0.023(4) 0.015(4) -0.004(3) 0.010(3) 0.001(2) C411 0.032(3) 0.024(5) 0.025(6) 0.000(4) 0.013(3) 0.001(3) C412 0.032(3) 0.025(3) 0.024(3) -0.001(2) 0.015(3) 0.000(3) C413 0.030(4) 0.026(3) 0.022(3) -0.002(3) 0.019(3) -0.003(3) C414 0.019(4) 0.024(3) 0.024(3) 0.000(2) 0.016(3) -0.005(3) C415 0.015(4) 0.026(2) 0.028(3) 0.000(2) 0.011(3) -0.001(3) C416 0.019(6) 0.030(3) 0.019(3) 0.001(3) 0.001(4) -0.002(3) C417 0.024(5) 0.029(3) 0.023(4) 0.001(3) 0.006(4) 0.001(4) C418 0.017(3) 0.027(3) 0.019(3) 0.005(3) 0.003(3) 0.007(3) C419 0.022(3) 0.024(3) 0.017(3) 0.004(3) 0.006(2) 0.006(2) C420 0.029(2) 0.015(4) 0.021(3) 0.007(3) 0.007(2) 0.002(3) C421 0.028(3) 0.016(5) 0.022(3) 0.008(4) 0.010(3) -0.006(4) C422 0.026(3) 0.013(4) 0.028(3) 0.001(3) 0.011(2) -0.009(4) C423 0.026(3) 0.018(4) 0.017(4) -0.004(3) 0.004(3) -0.004(3) C424 0.026(3) 0.021(4) 0.010(4) -0.004(3) 0.002(3) -0.002(3) C425 0.014(6) 0.017(4) 0.018(4) -0.001(3) 0.008(5) -0.011(4) C426 0.016(6) 0.026(4) 0.019(4) -0.001(4) 0.012(5) -0.010(4) C427 0.027(6) 0.031(5) 0.023(8) -0.004(5) 0.008(6) -0.002(5) C428 0.025(3) 0.021(3) 0.009(4) 0.006(3) 0.003(3) 0.008(3) C429 0.028(3) 0.016(4) 0.016(4) 0.007(3) 0.009(3) 0.005(3) C430 0.028(4) 0.024(5) 0.013(4) 0.011(3) 0.010(4) -0.002(3) Cl1 0.0199(5) 0.0275(5) 0.0259(5) -0.0014(4) 0.0040(4) -0.0062(4) Cl2 0.0403(6) 0.0348(6) 0.0289(6) -0.0078(4) 0.0167(5) 0.0081(5) C1S 0.0143(15) 0.0144(18) 0.0190(18) 0.0020(13) 0.0038(13) 0.0003(14) C2S 0.0237(16) 0.016(2) 0.022(2) -0.0001(14) 0.0101(15) 0.0033(15) C3S 0.0181(16) 0.024(2) 0.0259(19) 0.0077(14) 0.0084(15) 0.0039(15) C4S 0.0168(17) 0.025(2) 0.027(2) 0.0041(14) 0.0029(16) -0.0016(16) C5S 0.0284(18) 0.023(2) 0.0179(19) -0.0028(14) 0.0049(15) 0.0005(16) C6S 0.0207(16) 0.018(2) 0.023(2) 0.0007(14) 0.0074(14) 0.0035(14) Cl3 0.0240(5) 0.0280(5) 0.0254(5) 0.0022(4) -0.0009(4) 0.0083(4) Cl4 0.0516(8) 0.0431(7) 0.0292(6) 0.0026(5) 0.0210(6) -0.0168(6) C12S 0.0166(16) 0.017(2) 0.017(2) 0.0024(16) 0.0013(16) 0.0009(15) C11S 0.0232(17) 0.024(2) 0.020(3) -0.0014(17) 0.0077(18) -0.0046(17) C16S 0.0164(17) 0.033(2) 0.023(2) -0.0093(14) 0.0042(16) -0.0022(15) C15S 0.0223(17) 0.032(2) 0.0196(19) -0.0041(14) -0.0014(15) 0.0046(17) C14S 0.0259(19) 0.0195(19) 0.0163(18) 0.0022(14) 0.0012(15) 0.0094(16) C13S 0.0203(17) 0.022(2) 0.0182(19) 0.0006(14) 0.0065(15) 0.0013(14) _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 N1 C5 1.446(3) . ? N1 C1 1.461(3) . ? N1 C2 1.462(3) . ? N2 C6 1.487(3) . ? N2 C7 1.495(3) . ? N2 C3 1.514(3) . ? N2 C4 1.515(3) . ? C1 C3 1.504(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.502(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C301 C306 1.399(3) . ? C301 C305 1.439(3) . ? C301 C302 1.449(3) . ? C302 C309 1.421(3) . ? C302 C303 1.421(3) . ? C303 C312 1.415(4) . ? C303 C304 1.456(3) . ? C304 C315 1.391(3) . ? C304 C305 1.462(3) . ? C305 C318 1.384(3) . ? C306 C320 1.440(3) . ? C306 C307 1.461(3) . ? C307 C308 1.397(4) . ? C307 C322 1.456(3) . ? C308 C309 1.427(3) . ? C308 C323 1.459(3) . ? C309 C310 1.469(4) . ? C310 C311 1.372(4) . ? C310 C324 1.464(4) . ? C311 C312 1.450(4) . ? C311 C329 1.456(4) 7_566 ? C312 C313 1.425(4) . ? C313 C314 1.405(4) . ? C313 C330 1.458(3) 7_566 ? C314 C325 1.424(4) . ? C314 C315 1.462(3) . ? C315 C316 1.444(3) . ? C316 C317 1.391(4) . ? C316 C326 1.472(4) . ? C317 C327 1.433(4) . ? C317 C318 1.449(3) . ? C318 C319 1.457(3) . ? C319 C320 1.386(3) . ? C319 C328 1.430(3) . ? C320 C321 1.454(3) . ? C321 C330 1.397(3) . ? C321 C322 1.443(4) . ? C322 C325 1.409(3) 7_566 ? C323 C326 1.404(4) 7_566 ? C323 C324 1.442(4) . ? C324 C327 1.385(4) 7_566 ? C325 C322 1.409(3) 7_566 ? C325 C326 1.448(4) . ? C326 C323 1.404(4) 7_566 ? C327 C324 1.385(4) 7_566 ? C327 C328 1.461(4) . ? C328 C329 1.387(4) . ? C329 C330 1.427(4) . ? C329 C311 1.456(4) 7_566 ? C330 C313 1.458(3) 7_566 ? C401 C406 1.399(4) . ? C401 C405 1.439(4) . ? C401 C402 1.449(4) . ? C402 C409 1.421(4) . ? C402 C403 1.421(4) . ? C403 C412 1.415(4) . ? C403 C404 1.456(4) . ? C404 C415 1.391(4) . ? C404 C405 1.462(4) . ? C405 C418 1.384(4) . ? C406 C420 1.441(4) . ? C406 C407 1.461(4) . ? C407 C408 1.396(4) . ? C407 C422 1.455(4) . ? C408 C409 1.427(4) . ? C408 C423 1.459(4) . ? C409 C410 1.469(4) . ? C410 C411 1.372(4) . ? C410 C424 1.464(4) . ? C411 C429 1.346(18) 7_566 ? C411 C412 1.450(4) . ? C412 C413 1.424(4) . ? C413 C414 1.405(4) . ? C413 C430 1.446(16) 7_566 ? C414 C425 1.424(4) . ? C414 C415 1.462(4) . ? C415 C416 1.444(4) . ? C416 C417 1.391(4) . ? C416 C426 1.472(4) . ? C417 C427 1.433(4) . ? C417 C418 1.449(4) . ? C418 C419 1.457(4) . ? C419 C420 1.386(4) . ? C419 C428 1.430(4) . ? C420 C421 1.454(4) . ? C421 C430 1.397(4) . ? C421 C422 1.443(4) . ? C422 C425 1.324(16) 7_566 ? C423 C426 1.366(16) 7_566 ? C423 C424 1.442(4) . ? C424 C427 1.30(2) 7_566 ? C425 C422 1.324(16) 7_566 ? C425 C426 1.448(4) . ? C426 C423 1.366(16) 7_566 ? C427 C424 1.30(2) 7_566 ? C427 C428 1.461(4) . ? C428 C429 1.388(4) . ? C429 C411 1.346(17) 7_566 ? C429 C430 1.427(4) . ? C430 C413 1.445(16) 7_566 ? Cl1 C1S 1.7279(13) . ? Cl2 C2S 1.7263(13) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C3S H3S 0.9300 . ? C4S C5S 1.3900 . ? C4S H4S 0.9300 . ? C5S C6S 1.3900 . ? C5S H5S 0.9300 . ? C6S H6S 0.9300 . ? Cl3 C12S 1.7284(14) . ? Cl4 C11S 1.7262(14) . ? C12S C11S 1.3900 . ? C12S C13S 1.3900 . ? C11S C16S 1.3900 . ? C16S C15S 1.3900 . ? C16S H16S 0.9300 . ? C15S C14S 1.3900 . ? C15S H15S 0.9300 . ? C14S C13S 1.3900 . ? C14S H14S 0.9300 . ? C13S H13S 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N1 C1 111.25(17) . . ? C5 N1 C2 110.88(17) . . ? C1 N1 C2 109.79(18) . . ? C6 N2 C7 108.0(2) . . ? C6 N2 C3 111.54(17) . . ? C7 N2 C3 109.32(17) . . ? C6 N2 C4 111.29(17) . . ? C7 N2 C4 109.11(18) . . ? C3 N2 C4 107.50(19) . . ? N1 C1 C3 110.72(18) . . ? N1 C1 H1A 109.5 . . ? C3 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1 C2 C4 110.82(18) . . ? N1 C2 H2A 109.5 . . ? C4 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C1 C3 N2 112.07(17) . . ? C1 C3 H3A 109.2 . . ? N2 C3 H3A 109.2 . . ? C1 C3 H3B 109.2 . . ? N2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C2 C4 N2 112.02(17) . . ? C2 C4 H4A 109.2 . . ? N2 C4 H4A 109.2 . . ? C2 C4 H4B 109.2 . . ? N2 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 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 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C306 C301 C305 119.6(2) . . ? C306 C301 C302 120.4(2) . . ? C305 C301 C302 108.5(2) . . ? C309 C302 C303 119.8(2) . . ? C309 C302 C301 118.9(2) . . ? C303 C302 C301 109.0(2) . . ? C312 C303 C302 121.5(2) . . ? C312 C303 C304 118.6(2) . . ? C302 C303 C304 107.4(2) . . ? C315 C304 C303 120.6(2) . . ? C315 C304 C305 119.3(2) . . ? C303 C304 C305 108.5(2) . . ? C318 C305 C301 120.5(2) . . ? C318 C305 C304 120.7(2) . . ? C301 C305 C304 106.7(2) . . ? C301 C306 C320 120.1(2) . . ? C301 C306 C307 119.8(2) . . ? C320 C306 C307 108.4(2) . . ? C308 C307 C322 120.3(2) . . ? C308 C307 C306 119.7(2) . . ? C322 C307 C306 107.6(2) . . ? C307 C308 C309 120.6(2) . . ? C307 C308 C323 119.6(2) . . ? C309 C308 C323 107.9(2) . . ? C302 C309 C308 120.6(2) . . ? C302 C309 C310 118.4(2) . . ? C308 C309 C310 108.4(2) . . ? C311 C310 C324 120.4(2) . . ? C311 C310 C309 121.1(2) . . ? C324 C310 C309 107.6(2) . . ? C310 C311 C312 120.5(2) . . ? C310 C311 C329 120.1(2) . 7_566 ? C312 C311 C329 108.0(2) . 7_566 ? C303 C312 C313 120.6(2) . . ? C303 C312 C311 118.7(2) . . ? C313 C312 C311 108.1(2) . . ? C314 C313 C312 121.1(2) . . ? C314 C313 C330 119.0(2) . 7_566 ? C312 C313 C330 107.9(2) . 7_566 ? C313 C314 C325 121.0(2) . . ? C313 C314 C315 118.6(2) . . ? C325 C314 C315 108.4(2) . . ? C304 C315 C316 119.3(2) . . ? C304 C315 C314 120.4(2) . . ? C316 C315 C314 108.4(2) . . ? C317 C316 C315 121.8(2) . . ? C317 C316 C326 118.9(2) . . ? C315 C316 C326 106.7(2) . . ? C316 C317 C327 121.1(2) . . ? C316 C317 C318 118.8(2) . . ? C327 C317 C318 108.1(2) . . ? C305 C318 C317 120.2(2) . . ? C305 C318 C319 119.9(2) . . ? C317 C318 C319 107.8(2) . . ? C320 C319 C328 120.3(2) . . ? C320 C319 C318 119.6(2) . . ? C328 C319 C318 107.9(2) . . ? C319 C320 C306 120.4(2) . . ? C319 C320 C321 120.2(2) . . ? C306 C320 C321 107.5(2) . . ? C330 C321 C322 120.7(2) . . ? C330 C321 C320 118.7(2) . . ? C322 C321 C320 108.9(2) . . ? C325 C322 C321 119.2(2) 7_566 . ? C325 C322 C307 120.4(2) 7_566 . ? C321 C322 C307 107.6(2) . . ? C326 C323 C324 119.5(2) 7_566 . ? C326 C323 C308 119.7(2) 7_566 . ? C324 C323 C308 109.0(2) . . ? C327 C324 C323 120.8(2) 7_566 . ? C327 C324 C310 119.7(2) 7_566 . ? C323 C324 C310 107.1(2) . . ? C322 C325 C314 120.3(2) 7_566 . ? C322 C325 C326 118.9(2) 7_566 . ? C314 C325 C326 108.3(2) . . ? C323 C326 C325 121.1(2) 7_566 . ? C323 C326 C316 119.6(3) 7_566 . ? C325 C326 C316 108.3(2) . . ? C324 C327 C317 120.0(2) 7_566 . ? C324 C327 C328 119.9(2) 7_566 . ? C317 C327 C328 108.0(2) . . ? C329 C328 C319 119.9(2) . . ? C329 C328 C327 120.0(2) . . ? C319 C328 C327 108.1(2) . . ? C328 C329 C330 120.4(2) . . ? C328 C329 C311 119.9(2) . 7_566 ? C330 C329 C311 107.4(2) . 7_566 ? C321 C330 C329 120.6(2) . . ? C321 C330 C313 119.8(2) . 7_566 ? C329 C330 C313 108.6(2) . 7_566 ? C406 C401 C405 119.5(3) . . ? C406 C401 C402 120.4(3) . . ? C405 C401 C402 108.5(2) . . ? C409 C402 C403 119.8(3) . . ? C409 C402 C401 118.9(3) . . ? C403 C402 C401 109.0(3) . . ? C412 C403 C402 121.4(3) . . ? C412 C403 C404 118.6(3) . . ? C402 C403 C404 107.4(3) . . ? C415 C404 C403 120.6(3) . . ? C415 C404 C405 119.3(3) . . ? C403 C404 C405 108.5(2) . . ? C418 C405 C401 120.6(3) . . ? C418 C405 C404 120.6(3) . . ? C401 C405 C404 106.7(3) . . ? C401 C406 C420 120.1(3) . . ? C401 C406 C407 119.8(3) . . ? C420 C406 C407 108.4(2) . . ? C408 C407 C422 120.4(4) . . ? C408 C407 C406 119.7(3) . . ? C422 C407 C406 107.6(3) . . ? C407 C408 C409 120.6(3) . . ? C407 C408 C423 119.7(4) . . ? C409 C408 C423 107.9(3) . . ? C402 C409 C408 120.6(3) . . ? C402 C409 C410 118.5(3) . . ? C408 C409 C410 108.3(3) . . ? C411 C410 C424 120.4(4) . . ? C411 C410 C409 121.0(3) . . ? C424 C410 C409 107.6(3) . . ? C429 C411 C410 118.2(10) 7_566 . ? C429 C411 C412 109.1(8) 7_566 . ? C410 C411 C412 120.5(3) . . ? C403 C412 C413 120.6(3) . . ? C403 C412 C411 118.8(3) . . ? C413 C412 C411 108.1(3) . . ? C414 C413 C412 121.1(3) . . ? C414 C413 C430 118.1(8) . 7_566 ? C412 C413 C430 105.2(7) . 7_566 ? C413 C414 C425 120.9(4) . . ? C413 C414 C415 118.6(3) . . ? C425 C414 C415 108.4(3) . . ? C404 C415 C416 119.3(3) . . ? C404 C415 C414 120.3(3) . . ? C416 C415 C414 108.4(3) . . ? C417 C416 C415 121.7(3) . . ? C417 C416 C426 118.9(4) . . ? C415 C416 C426 106.7(3) . . ? C416 C417 C427 121.1(4) . . ? C416 C417 C418 118.8(3) . . ? C427 C417 C418 108.2(3) . . ? C405 C418 C417 120.2(3) . . ? C405 C418 C419 119.9(3) . . ? C417 C418 C419 107.8(3) . . ? C420 C419 C428 120.3(3) . . ? C420 C419 C418 119.5(3) . . ? C428 C419 C418 108.0(3) . . ? C419 C420 C406 120.3(3) . . ? C419 C420 C421 120.2(3) . . ? C406 C420 C421 107.5(3) . . ? C430 C421 C422 120.6(4) . . ? C430 C421 C420 118.7(3) . . ? C422 C421 C420 108.8(3) . . ? C425 C422 C421 120.1(9) 7_566 . ? C425 C422 C407 120.2(8) 7_566 . ? C421 C422 C407 107.7(3) . . ? C426 C423 C424 125.0(15) 7_566 . ? C426 C423 C408 116.5(8) 7_566 . ? C424 C423 C408 109.0(3) . . ? C427 C424 C423 118.3(15) 7_566 . ? C427 C424 C410 121.6(10) 7_566 . ? C423 C424 C410 107.1(3) . . ? C422 C425 C414 121.2(8) 7_566 . ? C422 C425 C426 119.2(11) 7_566 . ? C414 C425 C426 108.3(3) . . ? C423 C426 C425 123.9(12) 7_566 . ? C423 C426 C416 115.4(9) 7_566 . ? C425 C426 C416 108.3(3) . . ? C424 C427 C417 121.2(9) 7_566 . ? C424 C427 C428 117.2(10) 7_566 . ? C417 C427 C428 108.0(3) . . ? C429 C428 C419 119.9(3) . . ? C429 C428 C427 120.0(4) . . ? C419 C428 C427 108.1(3) . . ? C411 C429 C428 122.5(9) 7_566 . ? C411 C429 C430 108.8(10) 7_566 . ? C428 C429 C430 120.3(3) . . ? C421 C430 C429 120.5(3) . . ? C421 C430 C413 119.0(8) . 7_566 ? C429 C430 C413 108.8(9) . 7_566 ? C2S C1S C6S 120.0 . . ? C2S C1S Cl1 120.40(6) . . ? C6S C1S Cl1 119.60(6) . . ? C1S C2S C3S 120.0 . . ? C1S C2S Cl2 120.53(6) . . ? C3S C2S Cl2 119.47(6) . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3S 120.0 . . ? C2S C3S H3S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? C11S C12S C13S 120.0 . . ? C11S C12S Cl3 120.64(7) . . ? C13S C12S Cl3 119.34(7) . . ? C16S C11S C12S 120.0 . . ? C16S C11S Cl4 119.19(7) . . ? C12S C11S Cl4 120.77(7) . . ? C11S C16S C15S 120.0 . . ? C11S C16S H16S 120.0 . . ? C15S C16S H16S 120.0 . . ? C16S C15S C14S 120.0 . . ? C16S C15S H15S 120.0 . . ? C14S C15S H15S 120.0 . . ? C13S C14S C15S 120.0 . . ? C13S C14S H14S 120.0 . . ? C15S C14S H14S 120.0 . . ? C14S C13S C12S 120.0 . . ? C14S C13S H13S 120.0 . . ? C12S C13S H13S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.583 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.062