# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name L.Latos-Grazynski _publ_author_name L.Latos-Grazynski _publ_contact_author_email lechoslaw.latos-grazynski@chem.uni.wroc.pl data_test-sr _database_code_depnum_ccdc_archive 'CCDC 893465' #TrackingRef '- 2xp.cif' _audit_update_record ; 2012-03-19 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,10,15,20-tetratolyl-2-aza-3,21-bis(diphenylphosphoryl)-21-carbaporphiryn 3.25 dichloromethane solvate ; _chemical_name_common ; 5,10,15,20-tetratolyl-2-aza-3,21-bis(diphenylphosphoryl)-21- carbaporphiryn 3.25 dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C72 H56 N4 O2 P2, 3.25(C H2 Cl2)' _chemical_formula_sum 'C75.25 H62.50 Cl6.50 N4 O2 P2' _chemical_formula_weight 1347.16 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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.2071(6) _cell_length_b 31.4686(13) _cell_length_c 15.2236(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.554(4) _cell_angle_gamma 90.00 _cell_volume 7222.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2794 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47788 _diffrn_reflns_av_R_equivalents 0.1429 _diffrn_reflns_av_sigmaI/netI 0.2724 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 30.09 _reflns_number_total 14729 _reflns_number_gt 5305 _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 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 483 77 ' ' 2 0.500 0.500 1.000 483 76 ' ' 3 0.000 0.500 0.500 222 35 ' ' 4 0.500 0.000 0.000 222 35 ' ' _platon_squeeze_details ; The assymetric part of unit cell contains 3.25 dichloromethane molecules from wchich 1.25 have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 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^)+(0.0740P)^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_number_reflns 14729 _refine_ls_number_parameters 781 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2110 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.2344 _refine_ls_wR_factor_gt 0.2146 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 P1 P 0.96075(9) 0.08691(5) 0.09790(9) 0.0322(4) Uani 1 1 d . . . P2 P 1.16075(9) 0.17972(5) 0.38502(10) 0.0379(4) Uani 1 1 d . . . O1 O 0.9371(2) 0.04109(11) 0.1071(2) 0.0358(9) Uani 1 1 d . . . O2 O 1.2103(2) 0.21674(12) 0.3571(2) 0.0474(11) Uani 1 1 d . . . N2 N 0.9984(3) 0.17324(13) 0.2952(3) 0.0321(10) Uani 1 1 d . . . N22 N 1.0801(3) 0.02798(13) 0.2478(3) 0.0321(11) Uani 1 1 d . . . H22 H 1.0383 0.0383 0.2743 0.038 Uiso 1 1 calc R . . N23 N 0.8933(3) -0.00669(14) 0.2442(3) 0.0344(11) Uani 1 1 d . . . H23N H 0.9103 0.0165 0.2217 0.041 Uiso 1 1 calc R . . N24 N 0.8162(3) 0.08044(14) 0.2414(3) 0.0344(11) Uani 1 1 d . . . C1 C 0.9455(3) 0.14808(17) 0.2346(3) 0.0338(13) Uani 1 1 d . . . C3 C 1.0791(4) 0.15736(17) 0.3000(3) 0.0347(13) Uani 1 1 d . . . C4 C 1.0828(3) 0.12104(15) 0.2405(3) 0.0270(12) Uani 1 1 d . . . C5 C 1.1589(3) 0.09481(17) 0.2317(3) 0.0312(13) Uani 1 1 d . . . C6 C 1.1489(3) 0.05139(17) 0.2195(3) 0.0327(13) Uani 1 1 d . . . C7 C 1.2044(3) 0.02171(17) 0.1805(3) 0.0351(13) Uani 1 1 d . . . H7 H 1.2559 0.0282 0.1564 0.042 Uiso 1 1 calc R . . C8 C 1.1684(3) -0.01718(18) 0.1853(3) 0.0341(13) Uani 1 1 d . . . H8 H 1.1909 -0.0423 0.1650 0.041 Uiso 1 1 calc R . . C9 C 1.0890(3) -0.01334(17) 0.2272(3) 0.0331(13) Uani 1 1 d . . . C10 C 1.0318(3) -0.04669(17) 0.2466(3) 0.0326(13) Uani 1 1 d . . . C11 C 0.9462(3) -0.04232(17) 0.2642(3) 0.0340(13) Uani 1 1 d . . . C12 C 0.8926(4) -0.07202(18) 0.3045(3) 0.0369(14) Uani 1 1 d . . . H12 H 0.9113 -0.0986 0.3264 0.044 Uiso 1 1 calc R . . C13 C 0.8111(4) -0.05562(17) 0.3061(4) 0.0389(14) Uani 1 1 d . . . H13 H 0.7645 -0.0688 0.3292 0.047 Uiso 1 1 calc R . . C14 C 0.8085(4) -0.01429(17) 0.2661(3) 0.0402(14) Uani 1 1 d . . . C15 C 0.7344(3) 0.01316(17) 0.2519(4) 0.0358(13) Uani 1 1 d . . . C16 C 0.7405(4) 0.05682(18) 0.2299(3) 0.0387(14) Uani 1 1 d . . . C17 C 0.6668(4) 0.08308(18) 0.1933(3) 0.0378(14) Uani 1 1 d . . . H17 H 0.6084 0.0743 0.1780 0.045 Uiso 1 1 calc R . . C18 C 0.6985(3) 0.12277(19) 0.1855(3) 0.0364(14) Uani 1 1 d . . . H18 H 0.6662 0.1466 0.1645 0.044 Uiso 1 1 calc R . . C19 C 0.7911(3) 0.12099(17) 0.2155(3) 0.0329(13) Uani 1 1 d . . . C20 C 0.8501(3) 0.15552(17) 0.2238(3) 0.0314(13) Uani 1 1 d . . . C21 C 0.9948(3) 0.11677(15) 0.1974(3) 0.0273(12) Uani 1 1 d . . . C22 C 0.8677(3) 0.11439(18) 0.0359(3) 0.0345(13) Uani 1 1 d . . . C23 C 0.8691(4) 0.1575(2) 0.0166(3) 0.0453(15) Uani 1 1 d . . . H23 H 0.9196 0.1732 0.0360 0.054 Uiso 1 1 calc R . . C24 C 0.7966(4) 0.1775(2) -0.0310(4) 0.0566(18) Uani 1 1 d . . . H24 H 0.7988 0.2063 -0.0439 0.068 Uiso 1 1 calc R . . C25 C 0.7220(5) 0.1542(3) -0.0589(4) 0.072(2) Uani 1 1 d . . . H25 H 0.6725 0.1676 -0.0893 0.087 Uiso 1 1 calc R . . C26 C 0.7195(4) 0.1095(3) -0.0414(4) 0.0616(19) Uani 1 1 d . . . H26 H 0.6695 0.0935 -0.0615 0.074 Uiso 1 1 calc R . . C27 C 0.7930(4) 0.0906(2) 0.0059(4) 0.0485(16) Uani 1 1 d . . . H27 H 0.7923 0.0616 0.0178 0.058 Uiso 1 1 calc R . . C28 C 1.0513(3) 0.09205(17) 0.0345(3) 0.0316(13) Uani 1 1 d . . . C29 C 1.0952(4) 0.13093(18) 0.0248(4) 0.0416(15) Uani 1 1 d . . . H29 H 1.0752 0.1555 0.0498 0.050 Uiso 1 1 calc R . . C30 C 1.1684(4) 0.1329(2) -0.0220(4) 0.0436(15) Uani 1 1 d . . . H30 H 1.1966 0.1588 -0.0276 0.052 Uiso 1 1 calc R . . C31 C 1.1985(4) 0.0976(2) -0.0593(4) 0.0420(15) Uani 1 1 d . . . H31 H 1.2474 0.0992 -0.0900 0.050 Uiso 1 1 calc R . . C32 C 1.1564(3) 0.05922(19) -0.0517(3) 0.0398(14) Uani 1 1 d . . . H32 H 1.1769 0.0350 -0.0777 0.048 Uiso 1 1 calc R . . C33 C 1.0838(3) 0.05648(17) -0.0056(3) 0.0345(13) Uani 1 1 d . . . H33 H 1.0561 0.0304 -0.0014 0.041 Uiso 1 1 calc R . . C34 C 1.2313(4) 0.1378(2) 0.4327(4) 0.0470(16) Uani 1 1 d . . . C35 C 1.3211(4) 0.1486(3) 0.4634(4) 0.077(2) Uani 1 1 d . . . H35 H 1.3417 0.1758 0.4542 0.092 Uiso 1 1 calc R . . C36 C 1.3784(6) 0.1185(4) 0.5074(5) 0.108(4) Uani 1 1 d . . . H36 H 1.4362 0.1258 0.5297 0.130 Uiso 1 1 calc R . . C37 C 1.3473(8) 0.0771(4) 0.5172(6) 0.108(4) Uani 1 1 d . . . H37 H 1.3860 0.0568 0.5447 0.129 Uiso 1 1 calc R . . C38 C 1.2602(7) 0.0654(3) 0.4872(5) 0.088(3) Uani 1 1 d . . . H38 H 1.2406 0.0377 0.4934 0.106 Uiso 1 1 calc R . . C39 C 1.2027(4) 0.0969(3) 0.4470(4) 0.063(2) Uani 1 1 d . . . H39 H 1.1435 0.0901 0.4295 0.076 Uiso 1 1 calc R . . C40 C 1.0982(3) 0.19412(17) 0.4725(3) 0.0322(13) Uani 1 1 d . . . C41 C 1.1177(3) 0.23249(19) 0.5139(4) 0.0416(14) Uani 1 1 d . . . H41 H 1.1586 0.2506 0.4932 0.050 Uiso 1 1 calc R . . C42 C 1.0763(4) 0.2444(2) 0.5869(4) 0.0491(16) Uani 1 1 d . . . H42 H 1.0892 0.2707 0.6137 0.059 Uiso 1 1 calc R . . C43 C 1.0173(4) 0.2179(2) 0.6193(4) 0.0488(16) Uani 1 1 d . . . H43 H 0.9911 0.2256 0.6688 0.059 Uiso 1 1 calc R . . C44 C 0.9964(4) 0.1786(2) 0.5770(4) 0.0482(16) Uani 1 1 d . . . H44 H 0.9546 0.1608 0.5974 0.058 Uiso 1 1 calc R . . C45 C 1.0372(3) 0.16658(18) 0.5062(4) 0.0403(14) Uani 1 1 d . . . H45 H 1.0249 0.1402 0.4800 0.048 Uiso 1 1 calc R . . C51 C 1.2467(3) 0.11404(16) 0.2327(3) 0.0304(12) Uani 1 1 d . . . C52 C 1.3226(3) 0.09205(17) 0.2707(4) 0.0386(14) Uani 1 1 d . . . H52 H 1.3169 0.0649 0.2934 0.046 Uiso 1 1 calc R . . C53 C 1.4073(4) 0.1107(2) 0.2747(4) 0.0494(16) Uani 1 1 d . . . H53 H 1.4570 0.0957 0.2997 0.059 Uiso 1 1 calc R . . C54 C 1.4173(3) 0.15189(19) 0.2412(4) 0.0450(15) Uani 1 1 d . . . C55 C 1.3412(4) 0.17213(19) 0.2029(4) 0.0486(16) Uani 1 1 d . . . H55 H 1.3465 0.1990 0.1787 0.058 Uiso 1 1 calc R . . C56 C 1.2586(3) 0.15466(17) 0.1989(3) 0.0355(13) Uani 1 1 d . . . H56 H 1.2095 0.1700 0.1733 0.043 Uiso 1 1 calc R . . C57 C 1.5059(4) 0.1730(2) 0.2486(7) 0.103(3) Uani 1 1 d . . . H57A H 1.5493 0.1554 0.2826 0.155 Uiso 1 1 calc R . . H57B H 1.5030 0.2000 0.2776 0.155 Uiso 1 1 calc R . . H57C H 1.5223 0.1772 0.1905 0.155 Uiso 1 1 calc R . . C101 C 1.0693(3) -0.09051(17) 0.2479(3) 0.0366(14) Uani 1 1 d . . . C102 C 1.1515(3) -0.10046(18) 0.2929(4) 0.0400(14) Uani 1 1 d . . . H102 H 1.1848 -0.0795 0.3251 0.048 Uiso 1 1 calc R . . C103 C 1.1853(4) -0.14148(19) 0.2905(4) 0.0435(15) Uani 1 1 d . . . H103 H 1.2411 -0.1475 0.3207 0.052 Uiso 1 1 calc R . . C104 C 1.1377(4) -0.17330(18) 0.2442(4) 0.0397(14) Uani 1 1 d . . . C105 C 1.0575(4) -0.16325(18) 0.1978(4) 0.0453(15) Uani 1 1 d . . . H105 H 1.0260 -0.1842 0.1641 0.054 Uiso 1 1 calc R . . C106 C 1.0211(4) -0.12278(16) 0.1992(4) 0.0370(14) Uani 1 1 d . . . H106 H 0.9655 -0.1171 0.1682 0.044 Uiso 1 1 calc R . . C107 C 1.1757(4) -0.21704(18) 0.2428(4) 0.0570(18) Uani 1 1 d . . . H10A H 1.1316 -0.2361 0.2143 0.085 Uiso 1 1 calc R . . H10B H 1.1939 -0.2264 0.3025 0.085 Uiso 1 1 calc R . . H10C H 1.2260 -0.2167 0.2108 0.085 Uiso 1 1 calc R . . C151 C 0.6471(3) -0.00432(17) 0.2620(4) 0.0357(13) Uani 1 1 d . . . C152 C 0.6168(4) -0.0418(2) 0.2216(4) 0.0544(17) Uani 1 1 d . . . H152 H 0.6521 -0.0563 0.1859 0.065 Uiso 1 1 calc R . . C153 C 0.5332(4) -0.0586(2) 0.2336(5) 0.0621(19) Uani 1 1 d . . . H153 H 0.5139 -0.0838 0.2057 0.074 Uiso 1 1 calc R . . C154 C 0.4800(4) -0.0379(2) 0.2862(6) 0.070(2) Uani 1 1 d . . . C155 C 0.5107(4) -0.0005(2) 0.3258(5) 0.0601(19) Uani 1 1 d . . . H155 H 0.4753 0.0141 0.3612 0.072 Uiso 1 1 calc R . . C156 C 0.5924(4) 0.01616(19) 0.3145(4) 0.0482(16) Uani 1 1 d . . . H156 H 0.6111 0.0415 0.3426 0.058 Uiso 1 1 calc R . . C157 C 0.3911(4) -0.0563(2) 0.3030(6) 0.099(3) Uani 1 1 d . . . H15A H 0.4006 -0.0777 0.3482 0.149 Uiso 1 1 calc R . . H15B H 0.3618 -0.0687 0.2494 0.149 Uiso 1 1 calc R . . H15C H 0.3548 -0.0340 0.3222 0.149 Uiso 1 1 calc R . . C201 C 0.8168(3) 0.19947(18) 0.2251(3) 0.0348(14) Uani 1 1 d . . . C202 C 0.8578(4) 0.23177(18) 0.1816(4) 0.0415(14) Uani 1 1 d . . . H202 H 0.9062 0.2253 0.1525 0.050 Uiso 1 1 calc R . . C203 C 0.8270(4) 0.27362(18) 0.1816(4) 0.0471(15) Uani 1 1 d . . . H203 H 0.8543 0.2946 0.1518 0.057 Uiso 1 1 calc R . . C204 C 0.7559(4) 0.28393(19) 0.2259(4) 0.0445(15) Uani 1 1 d . . . C205 C 0.7161(4) 0.2522(2) 0.2687(4) 0.0457(16) Uani 1 1 d . . . H205 H 0.6682 0.2588 0.2984 0.055 Uiso 1 1 calc R . . C206 C 0.7460(3) 0.21048(18) 0.2685(3) 0.0361(14) Uani 1 1 d . . . H206 H 0.7179 0.1897 0.2981 0.043 Uiso 1 1 calc R . . C207 C 0.7236(4) 0.32954(18) 0.2257(4) 0.0611(19) Uani 1 1 d . . . H20A H 0.7737 0.3484 0.2321 0.092 Uiso 1 1 calc R . . H20B H 0.6898 0.3337 0.2740 0.092 Uiso 1 1 calc R . . H20C H 0.6870 0.3354 0.1707 0.092 Uiso 1 1 calc R . . C3S C 1.0767(5) 0.2692(2) 0.2252(5) 0.074(2) Uani 1 1 d . . . H3S1 H 1.0268 0.2563 0.2490 0.089 Uiso 1 1 calc R . . H3S2 H 1.1302 0.2628 0.2651 0.089 Uiso 1 1 calc R . . Cl6 Cl 1.06160(14) 0.32511(6) 0.21709(15) 0.0944(7) Uani 1 1 d . . . Cl5 Cl 1.08527(14) 0.24776(7) 0.11783(17) 0.1010(7) Uani 1 1 d . . . Cl3 Cl 0.80493(15) 0.25091(10) 0.49463(14) 0.1284(11) Uani 1 1 d . . . Cl4 Cl 0.9233(2) 0.31275(9) 0.4344(2) 0.1816(16) Uani 1 1 d . . . C2S C 0.8930(4) 0.2606(2) 0.4317(5) 0.077(2) Uani 1 1 d . . . H2S1 H 0.9437 0.2434 0.4549 0.092 Uiso 1 1 calc R . . H2S2 H 0.8748 0.2521 0.3708 0.092 Uiso 1 1 calc R . . 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 P1 0.0388(8) 0.0285(9) 0.0291(8) -0.0029(7) 0.0038(6) -0.0004(6) P2 0.0406(8) 0.0420(10) 0.0306(8) -0.0020(7) 0.0026(6) -0.0017(7) O1 0.046(2) 0.027(2) 0.034(2) -0.0080(17) 0.0029(16) -0.0041(16) O2 0.056(2) 0.052(3) 0.036(2) -0.009(2) 0.0140(18) -0.022(2) N2 0.041(3) 0.023(3) 0.032(3) 0.000(2) 0.002(2) -0.006(2) N22 0.044(3) 0.019(3) 0.033(3) 0.001(2) 0.003(2) 0.009(2) N23 0.044(3) 0.029(3) 0.031(3) 0.003(2) 0.010(2) -0.011(2) N24 0.044(3) 0.026(3) 0.035(3) -0.006(2) 0.012(2) 0.008(2) C1 0.047(3) 0.031(3) 0.022(3) 0.001(3) 0.003(2) -0.006(3) C3 0.048(4) 0.030(3) 0.026(3) 0.005(3) 0.005(2) -0.006(3) C4 0.036(3) 0.021(3) 0.024(3) 0.002(2) 0.002(2) 0.002(2) C5 0.038(3) 0.031(4) 0.024(3) 0.001(3) 0.002(2) -0.004(3) C6 0.034(3) 0.032(4) 0.033(3) 0.003(3) 0.003(2) -0.002(3) C7 0.039(3) 0.032(4) 0.035(3) -0.005(3) 0.007(2) 0.004(3) C8 0.045(3) 0.028(3) 0.030(3) 0.003(3) 0.006(2) 0.008(3) C9 0.039(3) 0.025(3) 0.034(3) 0.000(3) -0.005(2) 0.001(3) C10 0.037(3) 0.031(3) 0.029(3) -0.005(3) 0.003(2) 0.002(3) C11 0.044(3) 0.027(3) 0.031(3) 0.001(3) 0.001(2) 0.007(3) C12 0.048(4) 0.030(3) 0.031(3) -0.001(3) 0.002(3) -0.012(3) C13 0.051(4) 0.028(4) 0.039(3) -0.001(3) 0.012(3) -0.007(3) C14 0.065(4) 0.027(4) 0.028(3) -0.009(3) 0.000(3) 0.003(3) C15 0.038(3) 0.023(3) 0.046(4) -0.005(3) 0.005(3) -0.001(3) C16 0.041(3) 0.041(4) 0.033(3) 0.001(3) 0.000(2) -0.004(3) C17 0.042(3) 0.038(4) 0.032(3) -0.001(3) -0.002(2) -0.001(3) C18 0.027(3) 0.048(4) 0.034(3) 0.001(3) 0.003(2) 0.007(3) C19 0.047(3) 0.029(4) 0.024(3) -0.009(3) 0.011(2) -0.001(3) C20 0.046(3) 0.033(4) 0.013(3) 0.001(2) -0.004(2) 0.012(3) C21 0.041(3) 0.014(3) 0.026(3) 0.001(2) -0.001(2) 0.004(2) C22 0.037(3) 0.042(4) 0.024(3) -0.008(3) 0.003(2) 0.004(3) C23 0.050(4) 0.055(5) 0.029(3) 0.001(3) 0.000(3) 0.011(3) C24 0.066(4) 0.070(5) 0.033(4) 0.010(3) 0.003(3) 0.033(4) C25 0.070(5) 0.104(7) 0.038(4) -0.001(4) -0.011(3) 0.044(5) C26 0.061(4) 0.078(6) 0.042(4) -0.022(4) -0.006(3) 0.013(4) C27 0.052(4) 0.060(4) 0.031(3) -0.009(3) -0.001(3) 0.016(3) C28 0.040(3) 0.029(3) 0.026(3) 0.003(3) 0.007(2) 0.004(3) C29 0.054(4) 0.033(4) 0.034(3) -0.005(3) -0.006(3) -0.003(3) C30 0.043(3) 0.050(4) 0.037(4) -0.003(3) 0.002(3) -0.012(3) C31 0.041(3) 0.054(4) 0.030(3) -0.002(3) 0.001(3) 0.000(3) C32 0.043(3) 0.051(4) 0.025(3) -0.006(3) 0.004(3) 0.007(3) C33 0.045(3) 0.028(3) 0.030(3) -0.006(3) 0.002(3) -0.001(3) C34 0.054(4) 0.063(5) 0.025(3) 0.002(3) 0.008(3) 0.021(3) C35 0.058(4) 0.121(7) 0.047(4) -0.026(4) -0.011(3) 0.029(4) C36 0.093(6) 0.177(11) 0.048(5) -0.032(7) -0.013(4) 0.077(8) C37 0.134(10) 0.139(10) 0.049(5) 0.013(6) 0.009(6) 0.066(8) C38 0.124(7) 0.090(6) 0.059(5) 0.041(5) 0.039(5) 0.057(6) C39 0.064(4) 0.094(6) 0.034(4) 0.022(4) 0.016(3) 0.035(4) C40 0.032(3) 0.037(4) 0.026(3) 0.001(3) -0.002(2) 0.000(3) C41 0.042(3) 0.044(4) 0.035(3) -0.003(3) -0.006(3) -0.005(3) C42 0.065(4) 0.049(4) 0.032(3) -0.016(3) 0.002(3) 0.001(3) C43 0.066(4) 0.046(4) 0.036(4) -0.005(3) 0.012(3) 0.005(3) C44 0.059(4) 0.050(4) 0.038(4) 0.001(3) 0.016(3) 0.008(3) C45 0.049(3) 0.038(4) 0.035(3) 0.003(3) 0.009(3) 0.001(3) C51 0.032(3) 0.029(3) 0.029(3) -0.001(3) 0.001(2) -0.002(2) C52 0.041(3) 0.028(3) 0.047(4) -0.005(3) 0.007(3) -0.007(3) C53 0.037(4) 0.054(5) 0.057(4) -0.006(4) 0.006(3) 0.004(3) C54 0.028(3) 0.037(4) 0.071(4) 0.001(3) 0.013(3) -0.004(3) C55 0.063(4) 0.029(4) 0.058(4) -0.002(3) 0.025(3) -0.002(3) C56 0.042(3) 0.023(3) 0.040(3) -0.005(3) 0.003(3) 0.003(3) C57 0.043(4) 0.071(6) 0.203(10) 0.021(6) 0.040(5) -0.006(4) C101 0.049(3) 0.027(3) 0.035(3) 0.009(3) 0.009(3) 0.003(3) C102 0.047(3) 0.031(4) 0.039(3) 0.005(3) -0.007(3) 0.000(3) C103 0.049(4) 0.037(4) 0.046(4) 0.013(3) 0.013(3) 0.006(3) C104 0.049(4) 0.032(4) 0.039(3) 0.011(3) 0.011(3) 0.011(3) C105 0.073(4) 0.031(4) 0.034(3) 0.000(3) 0.016(3) 0.003(3) C106 0.049(3) 0.024(3) 0.036(3) -0.003(3) 0.002(3) 0.003(3) C107 0.073(4) 0.038(4) 0.059(4) 0.006(3) 0.004(3) 0.025(3) C151 0.035(3) 0.027(3) 0.044(4) -0.002(3) 0.003(3) 0.004(3) C152 0.046(4) 0.046(4) 0.069(5) -0.007(4) 0.001(3) 0.000(3) C153 0.043(4) 0.051(5) 0.088(5) 0.004(4) -0.005(4) -0.008(3) C154 0.042(4) 0.057(5) 0.107(6) 0.029(5) -0.007(4) -0.007(4) C155 0.045(4) 0.057(5) 0.079(5) 0.027(4) 0.011(3) 0.010(3) C156 0.042(4) 0.040(4) 0.061(4) 0.008(3) 0.000(3) 0.004(3) C157 0.040(4) 0.081(6) 0.177(9) 0.044(6) 0.014(5) -0.008(4) C201 0.037(3) 0.041(4) 0.023(3) -0.003(3) -0.007(2) 0.005(3) C202 0.056(4) 0.030(4) 0.038(3) -0.007(3) 0.001(3) 0.006(3) C203 0.058(4) 0.033(4) 0.047(4) -0.002(3) -0.004(3) 0.003(3) C204 0.033(3) 0.037(4) 0.060(4) -0.010(3) -0.006(3) 0.000(3) C205 0.036(3) 0.049(4) 0.049(4) -0.015(3) -0.005(3) 0.008(3) C206 0.037(3) 0.039(4) 0.031(3) -0.010(3) 0.000(2) 0.006(3) C207 0.072(4) 0.033(4) 0.072(5) -0.010(3) -0.012(4) 0.019(3) C3S 0.074(5) 0.051(5) 0.095(6) -0.014(4) 0.000(4) 0.001(4) Cl6 0.0991(15) 0.0586(13) 0.1177(18) -0.0043(13) -0.0152(13) -0.0020(11) Cl5 0.0965(15) 0.0704(15) 0.140(2) -0.0090(14) 0.0309(14) -0.0010(11) Cl3 0.1047(17) 0.223(3) 0.0547(13) -0.0097(17) 0.0014(12) 0.0625(18) Cl4 0.233(4) 0.078(2) 0.200(3) -0.004(2) -0.095(3) 0.009(2) C2S 0.079(5) 0.080(6) 0.066(5) -0.018(4) -0.009(4) 0.019(4) _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 P1 O1 1.497(4) . ? P1 C28 1.790(5) . ? P1 C21 1.800(5) . ? P1 C22 1.813(5) . ? P2 O2 1.479(4) . ? P2 C40 1.794(5) . ? P2 C34 1.794(6) . ? P2 C3 1.814(5) . ? N2 C3 1.318(6) . ? N2 C1 1.389(6) . ? N22 C9 1.349(6) . ? N22 C6 1.393(6) . ? N23 C11 1.390(6) . ? N23 C14 1.395(6) . ? N24 C16 1.363(6) . ? N24 C19 1.375(6) . ? C1 C21 1.401(7) . ? C1 C20 1.459(7) . ? C3 C4 1.464(7) . ? C4 C21 1.417(6) . ? C4 C5 1.441(7) . ? C5 C6 1.384(7) . ? C5 C51 1.465(7) . ? C6 C7 1.439(7) . ? C7 C8 1.347(7) . ? C8 C9 1.442(7) . ? C9 C10 1.419(7) . ? C10 C11 1.370(7) . ? C10 C101 1.491(7) . ? C11 C12 1.431(7) . ? C12 C13 1.345(7) . ? C13 C14 1.435(7) . ? C14 C15 1.413(7) . ? C15 C16 1.420(7) . ? C15 C151 1.464(7) . ? C16 C17 1.444(7) . ? C17 C18 1.350(7) . ? C18 C19 1.422(7) . ? C19 C20 1.404(7) . ? C20 C201 1.474(7) . ? C22 C27 1.388(7) . ? C22 C23 1.388(8) . ? C23 C24 1.388(7) . ? C24 C25 1.370(9) . ? C25 C26 1.435(10) . ? C26 C27 1.381(8) . ? C28 C33 1.396(7) . ? C28 C29 1.410(7) . ? C29 C30 1.400(7) . ? C30 C31 1.356(7) . ? C31 C32 1.378(8) . ? C32 C33 1.387(7) . ? C34 C39 1.383(9) . ? C34 C35 1.425(8) . ? C35 C36 1.396(11) . ? C36 C37 1.398(13) . ? C37 C38 1.394(12) . ? C38 C39 1.408(9) . ? C40 C41 1.376(7) . ? C40 C45 1.413(7) . ? C41 C42 1.398(7) . ? C42 C43 1.366(8) . ? C43 C44 1.411(8) . ? C44 C45 1.366(7) . ? C51 C56 1.399(7) . ? C51 C52 1.402(7) . ? C52 C53 1.410(7) . ? C53 C54 1.408(8) . ? C54 C55 1.381(8) . ? C54 C57 1.493(8) . ? C55 C56 1.366(7) . ? C101 C102 1.381(7) . ? C101 C106 1.405(7) . ? C102 C103 1.391(7) . ? C103 C104 1.374(8) . ? C104 C105 1.364(7) . ? C104 C107 1.494(7) . ? C105 C106 1.389(7) . ? C151 C152 1.382(7) . ? C151 C156 1.386(7) . ? C152 C153 1.410(8) . ? C153 C154 1.374(9) . ? C154 C155 1.377(9) . ? C154 C157 1.523(9) . ? C155 C156 1.379(8) . ? C201 C206 1.379(7) . ? C201 C202 1.403(7) . ? C202 C203 1.398(7) . ? C203 C204 1.386(8) . ? C204 C205 1.375(8) . ? C204 C207 1.517(8) . ? C205 C206 1.390(7) . ? C3S Cl6 1.777(7) . ? C3S Cl5 1.789(7) . ? Cl3 C2S 1.772(7) . ? Cl4 C2S 1.705(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 C28 110.4(2) . . ? O1 P1 C21 118.0(2) . . ? C28 P1 C21 104.5(2) . . ? O1 P1 C22 109.1(2) . . ? C28 P1 C22 106.2(2) . . ? C21 P1 C22 107.9(2) . . ? O2 P2 C40 110.7(2) . . ? O2 P2 C34 113.3(3) . . ? C40 P2 C34 103.5(2) . . ? O2 P2 C3 115.3(2) . . ? C40 P2 C3 104.3(2) . . ? C34 P2 C3 108.7(3) . . ? C3 N2 C1 105.9(4) . . ? C9 N22 C6 109.6(4) . . ? C11 N23 C14 109.6(4) . . ? C16 N24 C19 105.7(4) . . ? N2 C1 C21 112.1(4) . . ? N2 C1 C20 117.6(5) . . ? C21 C1 C20 130.2(5) . . ? N2 C3 C4 111.9(4) . . ? N2 C3 P2 116.0(4) . . ? C4 C3 P2 131.7(4) . . ? C21 C4 C5 128.5(4) . . ? C21 C4 C3 104.4(4) . . ? C5 C4 C3 127.0(4) . . ? C6 C5 C4 120.2(4) . . ? C6 C5 C51 119.5(5) . . ? C4 C5 C51 120.3(5) . . ? C5 C6 N22 123.6(5) . . ? C5 C6 C7 129.5(5) . . ? N22 C6 C7 106.8(4) . . ? C8 C7 C6 107.6(5) . . ? C7 C8 C9 108.5(5) . . ? N22 C9 C10 125.6(5) . . ? N22 C9 C8 107.4(4) . . ? C10 C9 C8 127.0(5) . . ? C11 C10 C9 126.2(5) . . ? C11 C10 C101 117.5(5) . . ? C9 C10 C101 116.3(4) . . ? C10 C11 N23 125.2(5) . . ? C10 C11 C12 128.9(5) . . ? N23 C11 C12 106.0(4) . . ? C13 C12 C11 109.6(5) . . ? C12 C13 C14 108.4(5) . . ? N23 C14 C15 127.0(5) . . ? N23 C14 C13 106.4(5) . . ? C15 C14 C13 126.6(5) . . ? C14 C15 C16 123.5(5) . . ? C14 C15 C151 118.0(5) . . ? C16 C15 C151 118.4(5) . . ? N24 C16 C15 125.3(5) . . ? N24 C16 C17 109.7(5) . . ? C15 C16 C17 125.0(5) . . ? C18 C17 C16 107.2(5) . . ? C17 C18 C19 106.6(5) . . ? N24 C19 C20 122.8(5) . . ? N24 C19 C18 110.8(5) . . ? C20 C19 C18 126.3(5) . . ? C19 C20 C1 120.0(5) . . ? C19 C20 C201 120.8(5) . . ? C1 C20 C201 119.2(5) . . ? C1 C21 C4 105.6(4) . . ? C1 C21 P1 126.6(4) . . ? C4 C21 P1 126.1(4) . . ? C27 C22 C23 119.4(5) . . ? C27 C22 P1 117.6(5) . . ? C23 C22 P1 122.9(4) . . ? C22 C23 C24 121.4(6) . . ? C25 C24 C23 119.2(7) . . ? C24 C25 C26 120.5(6) . . ? C27 C26 C25 118.7(6) . . ? C26 C27 C22 120.7(6) . . ? C33 C28 C29 116.8(5) . . ? C33 C28 P1 120.3(4) . . ? C29 C28 P1 122.9(4) . . ? C30 C29 C28 120.7(5) . . ? C31 C30 C29 120.7(5) . . ? C30 C31 C32 119.9(5) . . ? C31 C32 C33 120.4(5) . . ? C32 C33 C28 121.5(5) . . ? C39 C34 C35 118.6(6) . . ? C39 C34 P2 124.3(5) . . ? C35 C34 P2 117.0(6) . . ? C36 C35 C34 120.3(9) . . ? C35 C36 C37 119.0(10) . . ? C38 C37 C36 122.1(9) . . ? C37 C38 C39 117.7(9) . . ? C34 C39 C38 122.2(7) . . ? C41 C40 C45 118.9(5) . . ? C41 C40 P2 117.3(4) . . ? C45 C40 P2 123.5(4) . . ? C40 C41 C42 120.5(5) . . ? C43 C42 C41 120.5(6) . . ? C42 C43 C44 119.4(5) . . ? C45 C44 C43 120.3(6) . . ? C44 C45 C40 120.3(6) . . ? C56 C51 C52 117.6(5) . . ? C56 C51 C5 122.3(5) . . ? C52 C51 C5 120.0(5) . . ? C51 C52 C53 120.6(5) . . ? C54 C53 C52 120.6(5) . . ? C55 C54 C53 116.9(5) . . ? C55 C54 C57 121.6(6) . . ? C53 C54 C57 121.5(6) . . ? C56 C55 C54 123.2(5) . . ? C55 C56 C51 120.9(5) . . ? C102 C101 C106 118.2(5) . . ? C102 C101 C10 122.4(5) . . ? C106 C101 C10 119.3(5) . . ? C101 C102 C103 120.7(5) . . ? C104 C103 C102 121.2(5) . . ? C105 C104 C103 118.1(5) . . ? C105 C104 C107 121.8(5) . . ? C103 C104 C107 120.0(5) . . ? C104 C105 C106 122.4(5) . . ? C105 C106 C101 119.3(5) . . ? C152 C151 C156 117.6(5) . . ? C152 C151 C15 121.9(5) . . ? C156 C151 C15 120.4(5) . . ? C151 C152 C153 121.0(6) . . ? C154 C153 C152 120.6(6) . . ? C153 C154 C155 117.9(6) . . ? C153 C154 C157 121.5(7) . . ? C155 C154 C157 120.5(8) . . ? C154 C155 C156 122.0(6) . . ? C155 C156 C151 120.9(6) . . ? C206 C201 C202 117.9(5) . . ? C206 C201 C20 122.2(5) . . ? C202 C201 C20 119.9(5) . . ? C203 C202 C201 120.8(5) . . ? C204 C203 C202 120.2(6) . . ? C205 C204 C203 118.7(5) . . ? C205 C204 C207 121.7(5) . . ? C203 C204 C207 119.5(6) . . ? C204 C205 C206 121.3(5) . . ? C201 C206 C205 121.0(5) . . ? Cl6 C3S Cl5 109.5(4) . . ? Cl4 C2S Cl3 111.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 C21 -2.7(6) . . . . ? C3 N2 C1 C20 173.0(4) . . . . ? C1 N2 C3 C4 1.1(5) . . . . ? C1 N2 C3 P2 -172.5(3) . . . . ? O2 P2 C3 N2 -90.2(4) . . . . ? C40 P2 C3 N2 31.4(4) . . . . ? C34 P2 C3 N2 141.3(4) . . . . ? O2 P2 C3 C4 97.6(5) . . . . ? C40 P2 C3 C4 -140.7(5) . . . . ? C34 P2 C3 C4 -30.8(5) . . . . ? N2 C3 C4 C21 0.8(5) . . . . ? P2 C3 C4 C21 173.1(4) . . . . ? N2 C3 C4 C5 -176.9(5) . . . . ? P2 C3 C4 C5 -4.5(8) . . . . ? C21 C4 C5 C6 -35.9(8) . . . . ? C3 C4 C5 C6 141.2(5) . . . . ? C21 C4 C5 C51 142.3(5) . . . . ? C3 C4 C5 C51 -40.6(7) . . . . ? C4 C5 C6 N22 -25.6(7) . . . . ? C51 C5 C6 N22 156.2(5) . . . . ? C4 C5 C6 C7 156.6(5) . . . . ? C51 C5 C6 C7 -21.6(8) . . . . ? C9 N22 C6 C5 -179.4(5) . . . . ? C9 N22 C6 C7 -1.2(5) . . . . ? C5 C6 C7 C8 178.7(5) . . . . ? N22 C6 C7 C8 0.6(6) . . . . ? C6 C7 C8 C9 0.1(6) . . . . ? C6 N22 C9 C10 179.2(5) . . . . ? C6 N22 C9 C8 1.2(5) . . . . ? C7 C8 C9 N22 -0.8(6) . . . . ? C7 C8 C9 C10 -178.8(5) . . . . ? N22 C9 C10 C11 20.9(8) . . . . ? C8 C9 C10 C11 -161.4(5) . . . . ? N22 C9 C10 C101 -159.0(5) . . . . ? C8 C9 C10 C101 18.6(7) . . . . ? C9 C10 C11 N23 17.4(8) . . . . ? C101 C10 C11 N23 -162.6(5) . . . . ? C9 C10 C11 C12 -163.2(5) . . . . ? C101 C10 C11 C12 16.8(8) . . . . ? C14 N23 C11 C10 176.2(5) . . . . ? C14 N23 C11 C12 -3.3(5) . . . . ? C10 C11 C12 C13 -177.6(5) . . . . ? N23 C11 C12 C13 1.9(6) . . . . ? C11 C12 C13 C14 0.2(6) . . . . ? C11 N23 C14 C15 -176.6(5) . . . . ? C11 N23 C14 C13 3.4(5) . . . . ? C12 C13 C14 N23 -2.2(6) . . . . ? C12 C13 C14 C15 177.8(5) . . . . ? N23 C14 C15 C16 -14.1(9) . . . . ? C13 C14 C15 C16 165.9(5) . . . . ? N23 C14 C15 C151 167.0(5) . . . . ? C13 C14 C15 C151 -13.0(8) . . . . ? C19 N24 C16 C15 -177.2(5) . . . . ? C19 N24 C16 C17 1.8(6) . . . . ? C14 C15 C16 N24 -17.6(9) . . . . ? C151 C15 C16 N24 161.3(5) . . . . ? C14 C15 C16 C17 163.4(5) . . . . ? C151 C15 C16 C17 -17.7(8) . . . . ? N24 C16 C17 C18 -1.8(6) . . . . ? C15 C16 C17 C18 177.3(5) . . . . ? C16 C17 C18 C19 0.9(6) . . . . ? C16 N24 C19 C20 175.1(5) . . . . ? C16 N24 C19 C18 -1.3(5) . . . . ? C17 C18 C19 N24 0.2(6) . . . . ? C17 C18 C19 C20 -176.1(5) . . . . ? N24 C19 C20 C1 19.0(7) . . . . ? C18 C19 C20 C1 -165.1(5) . . . . ? N24 C19 C20 C201 -158.7(5) . . . . ? C18 C19 C20 C201 17.1(8) . . . . ? N2 C1 C20 C19 -138.7(5) . . . . ? C21 C1 C20 C19 36.1(8) . . . . ? N2 C1 C20 C201 39.1(6) . . . . ? C21 C1 C20 C201 -146.1(5) . . . . ? N2 C1 C21 C4 3.2(5) . . . . ? C20 C1 C21 C4 -171.9(5) . . . . ? N2 C1 C21 P1 -162.7(4) . . . . ? C20 C1 C21 P1 22.3(8) . . . . ? C5 C4 C21 C1 175.3(5) . . . . ? C3 C4 C21 C1 -2.3(5) . . . . ? C5 C4 C21 P1 -18.8(7) . . . . ? C3 C4 C21 P1 163.7(4) . . . . ? O1 P1 C21 C1 -107.4(4) . . . . ? C28 P1 C21 C1 129.6(4) . . . . ? C22 P1 C21 C1 16.8(5) . . . . ? O1 P1 C21 C4 89.6(5) . . . . ? C28 P1 C21 C4 -33.5(5) . . . . ? C22 P1 C21 C4 -146.2(4) . . . . ? O1 P1 C22 C27 -1.2(5) . . . . ? C28 P1 C22 C27 117.8(4) . . . . ? C21 P1 C22 C27 -130.6(4) . . . . ? O1 P1 C22 C23 179.8(4) . . . . ? C28 P1 C22 C23 -61.2(5) . . . . ? C21 P1 C22 C23 50.4(5) . . . . ? C27 C22 C23 C24 1.0(8) . . . . ? P1 C22 C23 C24 180.0(4) . . . . ? C22 C23 C24 C25 0.5(8) . . . . ? C23 C24 C25 C26 -1.9(9) . . . . ? C24 C25 C26 C27 1.7(9) . . . . ? C25 C26 C27 C22 -0.1(9) . . . . ? C23 C22 C27 C26 -1.3(8) . . . . ? P1 C22 C27 C26 179.7(4) . . . . ? O1 P1 C28 C33 6.2(5) . . . . ? C21 P1 C28 C33 134.1(4) . . . . ? C22 P1 C28 C33 -112.0(4) . . . . ? O1 P1 C28 C29 -171.5(4) . . . . ? C21 P1 C28 C29 -43.7(5) . . . . ? C22 P1 C28 C29 70.3(5) . . . . ? C33 C28 C29 C30 -0.8(7) . . . . ? P1 C28 C29 C30 177.0(4) . . . . ? C28 C29 C30 C31 0.2(8) . . . . ? C29 C30 C31 C32 0.4(8) . . . . ? C30 C31 C32 C33 -0.4(8) . . . . ? C31 C32 C33 C28 -0.2(8) . . . . ? C29 C28 C33 C32 0.8(7) . . . . ? P1 C28 C33 C32 -177.0(4) . . . . ? O2 P2 C34 C39 -166.1(5) . . . . ? C40 P2 C34 C39 73.9(5) . . . . ? C3 P2 C34 C39 -36.5(6) . . . . ? O2 P2 C34 C35 18.8(5) . . . . ? C40 P2 C34 C35 -101.2(5) . . . . ? C3 P2 C34 C35 148.3(4) . . . . ? C39 C34 C35 C36 -0.3(9) . . . . ? P2 C34 C35 C36 175.1(5) . . . . ? C34 C35 C36 C37 2.8(11) . . . . ? C35 C36 C37 C38 -2.2(13) . . . . ? C36 C37 C38 C39 -0.9(12) . . . . ? C35 C34 C39 C38 -2.9(9) . . . . ? P2 C34 C39 C38 -178.0(5) . . . . ? C37 C38 C39 C34 3.5(10) . . . . ? O2 P2 C40 C41 -13.4(5) . . . . ? C34 P2 C40 C41 108.4(4) . . . . ? C3 P2 C40 C41 -138.0(4) . . . . ? O2 P2 C40 C45 173.1(4) . . . . ? C34 P2 C40 C45 -65.2(5) . . . . ? C3 P2 C40 C45 48.5(5) . . . . ? C45 C40 C41 C42 -1.4(8) . . . . ? P2 C40 C41 C42 -175.2(4) . . . . ? C40 C41 C42 C43 1.3(8) . . . . ? C41 C42 C43 C44 -1.7(9) . . . . ? C42 C43 C44 C45 2.3(8) . . . . ? C43 C44 C45 C40 -2.5(8) . . . . ? C41 C40 C45 C44 2.1(8) . . . . ? P2 C40 C45 C44 175.5(4) . . . . ? C6 C5 C51 C56 145.6(5) . . . . ? C4 C5 C51 C56 -32.6(7) . . . . ? C6 C5 C51 C52 -36.1(7) . . . . ? C4 C5 C51 C52 145.7(5) . . . . ? C56 C51 C52 C53 0.5(8) . . . . ? C5 C51 C52 C53 -178.0(5) . . . . ? C51 C52 C53 C54 0.4(8) . . . . ? C52 C53 C54 C55 -1.6(8) . . . . ? C52 C53 C54 C57 177.1(6) . . . . ? C53 C54 C55 C56 2.0(9) . . . . ? C57 C54 C55 C56 -176.7(6) . . . . ? C54 C55 C56 C51 -1.2(9) . . . . ? C52 C51 C56 C55 -0.1(8) . . . . ? C5 C51 C56 C55 178.3(5) . . . . ? C11 C10 C101 C102 -132.0(5) . . . . ? C9 C10 C101 C102 48.0(7) . . . . ? C11 C10 C101 C106 50.3(7) . . . . ? C9 C10 C101 C106 -129.7(5) . . . . ? C106 C101 C102 C103 -0.6(8) . . . . ? C10 C101 C102 C103 -178.2(5) . . . . ? C101 C102 C103 C104 -0.6(8) . . . . ? C102 C103 C104 C105 2.3(8) . . . . ? C102 C103 C104 C107 180.0(5) . . . . ? C103 C104 C105 C106 -2.9(8) . . . . ? C107 C104 C105 C106 179.5(5) . . . . ? C104 C105 C106 C101 1.8(8) . . . . ? C102 C101 C106 C105 0.0(8) . . . . ? C10 C101 C106 C105 177.7(5) . . . . ? C14 C15 C151 C152 -49.2(8) . . . . ? C16 C15 C151 C152 131.9(6) . . . . ? C14 C15 C151 C156 129.5(6) . . . . ? C16 C15 C151 C156 -49.5(7) . . . . ? C156 C151 C152 C153 0.0(8) . . . . ? C15 C151 C152 C153 178.7(5) . . . . ? C151 C152 C153 C154 -0.2(10) . . . . ? C152 C153 C154 C155 0.5(10) . . . . ? C152 C153 C154 C157 -177.6(6) . . . . ? C153 C154 C155 C156 -0.5(10) . . . . ? C157 C154 C155 C156 177.5(6) . . . . ? C154 C155 C156 C151 0.3(9) . . . . ? C152 C151 C156 C155 -0.1(8) . . . . ? C15 C151 C156 C155 -178.8(5) . . . . ? C19 C20 C201 C206 39.1(7) . . . . ? C1 C20 C201 C206 -138.7(5) . . . . ? C19 C20 C201 C202 -141.3(5) . . . . ? C1 C20 C201 C202 41.0(7) . . . . ? C206 C201 C202 C203 -0.7(7) . . . . ? C20 C201 C202 C203 179.6(5) . . . . ? C201 C202 C203 C204 0.9(8) . . . . ? C202 C203 C204 C205 -0.7(8) . . . . ? C202 C203 C204 C207 179.7(5) . . . . ? C203 C204 C205 C206 0.3(8) . . . . ? C207 C204 C205 C206 179.9(5) . . . . ? C202 C201 C206 C205 0.3(7) . . . . ? C20 C201 C206 C205 180.0(5) . . . . ? C204 C205 C206 C201 -0.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.692 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.553 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.081 # Attachment '- Ag.cif' data_ng06a-sr _database_code_depnum_ccdc_archive 'CCDC 893466' #TrackingRef '- Ag.cif' _audit_update_record ; 2012-03-16 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(III) complex of 5,10,15,20-tetratolyl-2-aza-3-diphenylphosphoryl-21-carbaporphiryn hexane and dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H44 Ag N4 O P, 1.1(C H2 Cl2), (C6 H14)' _chemical_formula_sum 'C67.10 H70.20 Ag Cl2.20 Cs0 N4 O P0 P' _chemical_formula_weight 1165.50 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' Ag Ag -0.8971 1.1015 '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' Cs Cs -0.3680 2.1192 '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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M P21/c 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 22.7262(8) _cell_length_b 9.7497(4) _cell_length_c 29.1825(15) _cell_angle_alpha 90.00 _cell_angle_beta 122.445(3) _cell_angle_gamma 90.00 _cell_volume 5456.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2433 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.94748 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67866 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.2165 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 37.01 _reflns_number_total 22650 _reflns_number_gt 7030 _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 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.044 0.250 371 95 ' ' 2 0.500 -0.012 0.750 371 97 ' ' _platon_squeeze_details ; The assymetric part of unit cell contain hexane molecule which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 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^)+(0.0180P)^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_number_reflns 22650 _refine_ls_number_parameters 717 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1919 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.026 _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 Ag1 Ag 0.447685(10) -0.23624(2) -0.001213(8) 0.03960(7) Uani 1 1 d . . . P P 0.13969(4) -0.23882(14) -0.09610(3) 0.0747(3) Uani 1 1 d . . . O2 O 0.11139(12) -0.3330(3) -0.07339(12) 0.0918(9) Uani 1 1 d . C . N23 N 0.55084(11) -0.1836(2) 0.03339(9) 0.0419(6) Uani 1 1 d . . . C101 C 0.61624(17) 0.0351(4) 0.15770(12) 0.0525(9) Uani 1 1 d . . . N24 N 0.45318(12) -0.3613(2) -0.05436(9) 0.0394(6) Uani 1 1 d . . . N22 N 0.44036(11) -0.1150(2) 0.05210(9) 0.0389(6) Uani 1 1 d . C . N2 N 0.23761(12) -0.3451(3) -0.10470(10) 0.0535(7) Uani 1 1 d . . . C14 C 0.59154(13) -0.2158(3) 0.01306(12) 0.0422(8) Uani 1 1 d . . . C15 C 0.57622(15) -0.3153(3) -0.02564(13) 0.0459(8) Uani 1 1 d . . . C151 C 0.63029(17) -0.3469(3) -0.03854(16) 0.0549(9) Uani 1 1 d . . . C8 C 0.47560(16) -0.0100(3) 0.13234(11) 0.0490(8) Uani 1 1 d . . . H8 H 0.5040 0.0309 0.1661 0.059 Uiso 1 1 calc R . . C152 C 0.69572(17) -0.3951(3) 0.00074(17) 0.0681(11) Uani 1 1 d . . . H152 H 0.7063 -0.4093 0.0359 0.082 Uiso 1 1 calc R . . C19 C 0.40137(16) -0.4473(3) -0.09341(11) 0.0447(8) Uani 1 1 d . . . C4 C 0.29910(13) -0.2200(3) -0.02571(10) 0.0412(7) Uani 1 1 d . . . C201 C 0.27754(16) -0.5232(4) -0.15795(12) 0.0534(9) Uani 1 1 d D . . C10 C 0.56410(16) -0.0392(3) 0.10725(12) 0.0453(8) Uani 1 1 d . . . C51 C 0.26132(14) -0.1116(3) 0.03288(11) 0.0390(7) Uani 1 1 d . . . C57 C 0.11076(16) -0.0320(3) 0.07682(13) 0.0558(9) Uani 1 1 d . . . H57A H 0.1096 0.0645 0.0827 0.084 Uiso 1 1 calc R . . H57B H 0.1234 -0.0811 0.1094 0.084 Uiso 1 1 calc R . . H57C H 0.0656 -0.0616 0.0478 0.084 Uiso 1 1 calc R . . C107 C 0.7689(2) 0.2402(5) 0.30636(13) 0.1203(18) Uani 1 1 d . . . H10A H 0.7534 0.3320 0.3061 0.180 Uiso 1 1 calc R . . H10B H 0.8128 0.2432 0.3090 0.180 Uiso 1 1 calc R . . H10C H 0.7742 0.1913 0.3369 0.180 Uiso 1 1 calc R . . C204 C 0.1697(2) -0.6688(4) -0.24716(15) 0.0667(10) Uani 1 1 d D . . C52 C 0.24808(15) 0.0206(3) 0.04229(12) 0.0461(8) Uani 1 1 d . C . H52 H 0.2718 0.0939 0.0390 0.055 Uiso 1 1 calc R . . C1 C 0.30879(15) -0.3556(3) -0.08466(11) 0.0483(8) Uani 1 1 d . A . C13 C 0.65384(15) -0.1340(3) 0.04074(13) 0.0520(9) Uani 1 1 d . . . H13 H 0.6892 -0.1329 0.0337 0.062 Uiso 1 1 calc R . . C21 C 0.34690(13) -0.2791(3) -0.03696(10) 0.0401(7) Uani 1 1 d . A . C12 C 0.65192(15) -0.0592(3) 0.07866(13) 0.0513(9) Uani 1 1 d . . . H12 H 0.6861 0.0014 0.1030 0.062 Uiso 1 1 calc R . . C11 C 0.58659(14) -0.0904(3) 0.07460(12) 0.0435(8) Uani 1 1 d . . . C3 C 0.23072(13) -0.2654(4) -0.07172(11) 0.0536(8) Uani 1 1 d . C . C20 C 0.33097(15) -0.4412(3) -0.11069(11) 0.0444(8) Uani 1 1 d . A . C55 C 0.17584(15) -0.1922(3) 0.05146(11) 0.0451(8) Uani 1 1 d . . . H55 H 0.1509 -0.2647 0.0537 0.054 Uiso 1 1 calc R C . C27 C 0.07709(16) -0.0265(4) -0.07562(13) 0.0679(11) Uani 1 1 d . . . H27 H 0.0531 -0.0949 -0.0699 0.081 Uiso 1 1 calc R C . C16 C 0.51314(15) -0.3878(3) -0.05439(12) 0.0423(8) Uani 1 1 d . . . C9 C 0.49706(15) -0.0556(3) 0.09710(11) 0.0408(8) Uani 1 1 d . . . C5 C 0.31560(15) -0.1442(3) 0.02064(11) 0.0400(7) Uani 1 1 d . C . C7 C 0.40683(16) -0.0366(3) 0.10813(11) 0.0452(8) Uani 1 1 d . C . H7 H 0.3795 -0.0162 0.1222 0.054 Uiso 1 1 calc R . . C324 C 0.09793(18) 0.2132(4) -0.08061(15) 0.0840(13) Uani 1 1 d . . . H324 H 0.0889 0.3048 -0.0777 0.101 Uiso 1 1 calc R C . C53 C 0.20066(16) 0.0447(3) 0.05633(12) 0.0469(8) Uani 1 1 d . . . H53 H 0.1927 0.1345 0.0623 0.056 Uiso 1 1 calc R C . C6 C 0.38355(15) -0.1007(3) 0.05780(11) 0.0386(7) Uani 1 1 d . . . C102 C 0.6051(2) 0.1669(4) 0.16694(13) 0.0737(12) Uani 1 1 d . . . H102 H 0.5647 0.2121 0.1410 0.088 Uiso 1 1 calc R . . C156 C 0.61587(19) -0.3267(3) -0.09135(17) 0.0696(11) Uani 1 1 d . . . H156 H 0.5723 -0.2948 -0.1187 0.084 Uiso 1 1 calc R . . C207 C 0.11057(18) -0.7466(4) -0.29510(13) 0.0925(12) Uani 1 1 d . A . H20A H 0.1213 -0.7588 -0.3225 0.139 Uiso 1 1 calc R . . H20B H 0.0681 -0.6954 -0.3099 0.139 Uiso 1 1 calc R . . H20C H 0.1051 -0.8346 -0.2831 0.139 Uiso 1 1 calc R . . C104 C 0.7154(2) 0.1677(5) 0.25427(14) 0.0900(15) Uani 1 1 d . . . C56 C 0.22490(14) -0.2178(3) 0.03756(10) 0.0407(7) Uani 1 1 d . C . H56 H 0.2330 -0.3074 0.0314 0.049 Uiso 1 1 calc R . . C106 C 0.67621(19) -0.0283(4) 0.19765(14) 0.0746(12) Uani 1 1 d . . . H106 H 0.6845 -0.1186 0.1924 0.090 Uiso 1 1 calc R . . C54 C 0.16402(15) -0.0603(3) 0.06191(11) 0.0445(8) Uani 1 1 d . C . C18 C 0.43179(18) -0.5329(3) -0.11516(12) 0.0519(9) Uani 1 1 d . . . H18 H 0.4090 -0.6012 -0.1412 0.062 Uiso 1 1 calc R . . C45 C 0.12632(16) -0.0605(4) -0.08799(12) 0.0608(10) Uani 1 1 d . C . C17 C 0.49963(18) -0.4969(3) -0.09114(13) 0.0517(9) Uani 1 1 d . . . H17 H 0.5318 -0.5365 -0.0975 0.062 Uiso 1 1 calc R . . C47 C 0.14713(19) 0.1783(5) -0.09419(16) 0.0882(15) Uani 1 1 d . C . H47 H 0.1695 0.2468 -0.1014 0.106 Uiso 1 1 calc R . . C103 C 0.6538(2) 0.2355(4) 0.21515(14) 0.0932(14) Uani 1 1 d . . . H103 H 0.6454 0.3250 0.2211 0.112 Uiso 1 1 calc R . . C49 C 0.06387(17) 0.1120(5) -0.07176(14) 0.0755(12) Uani 1 1 d . C . H49 H 0.0313 0.1352 -0.0630 0.091 Uiso 1 1 calc R . . C153 C 0.7460(2) -0.4225(4) -0.0116(2) 0.0902(15) Uani 1 1 d . . . H153 H 0.7896 -0.4545 0.0155 0.108 Uiso 1 1 calc R . . C154 C 0.7313(3) -0.4025(4) -0.0641(3) 0.102(2) Uani 1 1 d . . . C105 C 0.7242(2) 0.0370(5) 0.24500(15) 0.0940(15) Uani 1 1 d . . . H105 H 0.7635 -0.0105 0.2712 0.113 Uiso 1 1 calc R . . C157 C 0.7860(2) -0.4355(4) -0.0777(2) 0.139(2) Uani 1 1 d . . . H15A H 0.7674 -0.4157 -0.1153 0.208 Uiso 1 1 calc R . . H15B H 0.7982 -0.5308 -0.0708 0.208 Uiso 1 1 calc R . . H15C H 0.8268 -0.3806 -0.0555 0.208 Uiso 1 1 calc R . . C155 C 0.6670(3) -0.3547(4) -0.1026(2) 0.0870(14) Uani 1 1 d . . . H155 H 0.6569 -0.3402 -0.1377 0.104 Uiso 1 1 calc R . . Cl1 Cl -0.03352(5) -0.30156(10) -0.04473(4) 0.0855(3) Uani 1 1 d . . . Cl2 Cl -0.06534(7) -0.55935(11) -0.10244(5) 0.1030(4) Uani 1 1 d . . . C1C C 0.00042(19) -0.4414(4) -0.06111(18) 0.0875(13) Uani 1 1 d . . . H1C1 H 0.0358 -0.4866 -0.0280 0.105 Uiso 1 1 calc R . . H1C2 H 0.0223 -0.4087 -0.0799 0.105 Uiso 1 1 calc R . . C87 C 0.16128(17) 0.0460(6) -0.09658(13) 0.0796(13) Uani 1 1 d . . . H87 H 0.1951 0.0239 -0.1041 0.096 Uiso 1 1 calc R C . C202 C 0.2242(2) -0.4439(5) -0.20405(16) 0.0437(14) Uani 0.669(5) 1 d P A 1 H202 H 0.2251 -0.3486 -0.2044 0.052 Uiso 0.669(5) 1 calc PR A 1 C205 C 0.2202(4) -0.7245(8) -0.1987(3) 0.071(2) Uani 0.669(5) 1 d P A 1 H205 H 0.2185 -0.8183 -0.1938 0.085 Uiso 0.669(5) 1 calc PR A 1 C203 C 0.1718(3) -0.5186(6) -0.24753(19) 0.0553(16) Uani 0.669(5) 1 d P A 1 H203 H 0.1370 -0.4717 -0.2778 0.066 Uiso 0.669(5) 1 calc PR A 1 C206 C 0.2742(3) -0.6487(6) -0.1562(2) 0.0535(16) Uani 0.669(5) 1 d P A 1 H206 H 0.3087 -0.6949 -0.1256 0.064 Uiso 0.669(5) 1 calc PR A 1 C208 C 0.2337(5) -0.6405(9) -0.1545(4) 0.033(2) Uani 0.331(5) 1 d PD A 2 H208 H 0.2422 -0.6673 -0.1209 0.040 Uiso 0.331(5) 1 calc PR A 2 C211 C 0.2723(6) -0.5419(10) -0.2089(4) 0.064(4) Uani 0.331(5) 1 d PD A 2 H211 H 0.3077 -0.5074 -0.2126 0.076 Uiso 0.331(5) 1 calc PR A 2 C210 C 0.2171(6) -0.6086(11) -0.2524(4) 0.063(4) Uani 0.331(5) 1 d PD A 2 H210 H 0.2136 -0.6108 -0.2857 0.076 Uiso 0.331(5) 1 calc PR A 2 C209 C 0.1825(7) -0.7047(14) -0.2008(6) 0.054(4) Uani 0.331(5) 1 d PD A 2 H209 H 0.1570 -0.7752 -0.1982 0.065 Uiso 0.331(5) 1 calc PR A 2 C36 C 0.0155(3) -0.3676(9) -0.2562(2) 0.215(4) Uani 1 1 d D . . H36 H -0.0191 -0.4333 -0.2748 0.259 Uiso 1 1 calc R B 3 C31 C 0.1007(2) -0.2484(7) -0.17181(19) 0.0908(19) Uani 0.744(5) 1 d PD C 3 C32 C 0.1215(3) -0.1673(6) -0.20034(16) 0.106(2) Uani 0.744(5) 1 d PD C 3 H32 H 0.1567 -0.1028 -0.1817 0.127 Uiso 0.744(5) 1 calc PR C 3 C33 C 0.0901(4) -0.1817(8) -0.25648(17) 0.174(5) Uani 0.744(5) 1 d PD C 3 H33 H 0.1031 -0.1272 -0.2758 0.209 Uiso 0.744(5) 1 calc PR C 3 C34 C 0.0383(4) -0.2821(9) -0.2822(3) 0.218(7) Uani 0.744(5) 1 d PD C 3 H34 H 0.0174 -0.2929 -0.3194 0.262 Uiso 0.744(5) 1 calc PR C 3 C35 C 0.0486(4) -0.3469(9) -0.2001(2) 0.182(5) Uani 0.744(5) 1 d PD C 3 H35 H 0.0354 -0.4010 -0.1809 0.218 Uiso 0.744(5) 1 calc PR C 3 C32A C 0.0884(7) -0.3073(8) -0.1573(5) 0.048(4) Uiso 0.256(5) 1 d PD C 4 C33A C 0.0614(8) -0.2143(17) -0.2005(6) 0.084(6) Uiso 0.256(5) 1 d PD C 4 H33A H 0.0709 -0.1237 -0.1889 0.100 Uiso 0.256(5) 1 calc PR C 4 C35A C 0.0747(5) -0.4451(9) -0.1730(4) 0.031(3) Uiso 0.256(5) 1 d PD C 4 H35A H 0.0937 -0.5112 -0.1457 0.037 Uiso 0.256(5) 1 calc PR C 4 C31A C 0.0235(9) -0.2256(8) -0.2572(6) 0.112(7) Uiso 0.256(5) 1 d PD C 4 H31A H 0.0091 -0.1623 -0.2851 0.134 Uiso 0.256(5) 1 calc PR C 4 C34A C 0.0343(5) -0.4905(8) -0.2268(3) 0.044(3) Uiso 0.256(5) 1 d PD C 4 H34A H 0.0229 -0.5799 -0.2398 0.053 Uiso 0.256(5) 1 calc PR C 4 C2C C 0.1708(14) -0.252(3) -0.2333(10) 0.048(7) Uani 0.10 1 d P C . H2C1 H 0.2181 -0.2760 -0.2221 0.057 Uiso 0.10 1 calc PR . . H2C2 H 0.1575 -0.3104 -0.2134 0.057 Uiso 0.10 1 calc PR . . Cl3 Cl 0.1695(4) -0.0814(7) -0.2157(3) 0.049(2) Uani 0.10 1 d P . . Cl4 Cl 0.1160(5) -0.2864(10) -0.3023(3) 0.078(3) Uani 0.10 1 d P . . 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 Ag1 0.02089(10) 0.06099(16) 0.02940(10) 0.01037(13) 0.00850(8) -0.00355(14) P 0.0217(4) 0.1267(9) 0.0592(5) -0.0212(7) 0.0108(4) -0.0101(7) O2 0.0530(16) 0.100(2) 0.143(2) -0.0454(18) 0.0670(18) -0.0325(14) N23 0.0242(13) 0.0580(17) 0.0366(15) 0.0151(12) 0.0117(12) -0.0014(12) C101 0.038(2) 0.064(3) 0.0351(19) 0.0146(17) 0.0066(17) -0.0181(19) N24 0.0261(14) 0.0537(17) 0.0352(14) 0.0112(12) 0.0142(13) -0.0013(12) N22 0.0245(13) 0.0550(17) 0.0260(13) 0.0061(11) 0.0061(12) -0.0048(12) N2 0.0228(14) 0.095(2) 0.0342(15) -0.0001(14) 0.0094(13) -0.0088(14) C14 0.0159(14) 0.055(2) 0.0447(18) 0.0239(16) 0.0089(14) 0.0012(15) C15 0.0303(18) 0.049(2) 0.058(2) 0.0217(17) 0.0237(18) 0.0034(16) C151 0.043(2) 0.037(2) 0.098(3) 0.0130(19) 0.047(2) 0.0024(16) C8 0.041(2) 0.064(2) 0.0275(16) 0.0003(15) 0.0085(16) -0.0121(17) C152 0.039(2) 0.035(2) 0.128(3) 0.010(2) 0.043(2) 0.0008(17) C19 0.041(2) 0.063(2) 0.0312(17) 0.0137(15) 0.0194(17) -0.0005(18) C4 0.0224(14) 0.065(2) 0.0301(15) 0.0062(15) 0.0099(13) -0.0044(16) C201 0.039(2) 0.090(3) 0.0295(18) 0.0019(19) 0.0176(17) -0.011(2) C10 0.0301(19) 0.060(2) 0.0287(17) 0.0176(15) 0.0045(16) -0.0135(16) C51 0.0324(17) 0.048(2) 0.0343(17) 0.0072(14) 0.0163(15) -0.0020(16) C57 0.048(2) 0.056(2) 0.074(2) 0.0096(17) 0.039(2) 0.0077(17) C107 0.114(3) 0.131(4) 0.042(2) -0.005(3) -0.007(2) -0.075(4) C204 0.054(3) 0.079(3) 0.047(2) -0.002(2) 0.014(2) -0.010(2) C52 0.0339(19) 0.048(2) 0.0510(19) 0.0095(16) 0.0192(17) -0.0045(16) C1 0.0256(17) 0.087(3) 0.0255(16) 0.0017(16) 0.0094(15) -0.0109(17) C13 0.0281(18) 0.069(2) 0.055(2) 0.0325(18) 0.0195(17) 0.0039(17) C21 0.0205(13) 0.067(2) 0.0268(14) 0.0047(15) 0.0085(12) -0.0094(16) C12 0.0219(17) 0.070(2) 0.0418(19) 0.0236(17) 0.0040(15) -0.0130(16) C11 0.0209(16) 0.061(2) 0.0311(17) 0.0216(16) 0.0022(14) -0.0032(16) C3 0.0247(15) 0.095(3) 0.0334(15) -0.0006(19) 0.0106(13) -0.009(2) C20 0.0331(18) 0.071(2) 0.0238(16) 0.0057(15) 0.0115(15) -0.0045(17) C55 0.0388(18) 0.045(2) 0.054(2) 0.0082(15) 0.0270(17) 0.0001(15) C27 0.027(2) 0.100(3) 0.064(2) 0.017(2) 0.0159(19) 0.008(2) C16 0.0338(19) 0.046(2) 0.0463(19) 0.0155(16) 0.0210(17) 0.0044(16) C9 0.0278(18) 0.054(2) 0.0249(16) 0.0118(14) 0.0038(15) -0.0063(16) C5 0.0267(16) 0.053(2) 0.0354(17) 0.0115(15) 0.0136(15) -0.0019(15) C7 0.0368(19) 0.060(2) 0.0352(17) 0.0067(15) 0.0170(16) -0.0052(17) C324 0.032(2) 0.086(3) 0.090(3) 0.032(2) 0.003(2) 0.002(2) C53 0.044(2) 0.036(2) 0.058(2) 0.0051(15) 0.0253(18) 0.0016(16) C6 0.0299(17) 0.048(2) 0.0341(17) 0.0044(14) 0.0146(15) -0.0037(15) C102 0.064(3) 0.086(3) 0.038(2) 0.013(2) 0.006(2) -0.029(2) C156 0.076(3) 0.051(2) 0.116(3) 0.024(2) 0.075(3) 0.0151(19) C207 0.077(3) 0.088(3) 0.061(2) -0.017(2) 0.004(2) -0.030(3) C104 0.080(3) 0.098(3) 0.037(2) 0.012(2) -0.006(2) -0.050(3) C56 0.0361(16) 0.045(2) 0.0428(16) 0.0008(14) 0.0223(14) 0.0032(15) C106 0.053(2) 0.085(3) 0.046(2) 0.017(2) -0.001(2) -0.023(2) C54 0.0383(19) 0.046(2) 0.0469(19) 0.0052(15) 0.0213(16) 0.0084(16) C18 0.052(2) 0.067(2) 0.039(2) 0.0074(16) 0.0256(19) -0.0062(19) C45 0.0270(19) 0.093(3) 0.045(2) 0.0049(18) 0.0073(17) -0.0005(19) C17 0.048(2) 0.057(2) 0.062(2) 0.0185(19) 0.038(2) 0.0064(18) C47 0.027(2) 0.106(4) 0.085(3) 0.051(3) -0.001(2) -0.003(2) C103 0.104(3) 0.082(3) 0.048(2) 0.009(2) 0.011(2) -0.039(3) C49 0.031(2) 0.103(4) 0.078(3) 0.033(2) 0.020(2) 0.012(2) C153 0.049(3) 0.032(2) 0.199(5) -0.010(3) 0.072(3) -0.0054(18) C154 0.094(4) 0.027(2) 0.249(7) -0.007(3) 0.134(5) -0.008(2) C105 0.073(3) 0.096(4) 0.050(3) 0.027(2) -0.009(2) -0.033(3) C157 0.135(4) 0.050(3) 0.331(8) -0.018(4) 0.191(5) -0.011(3) C155 0.119(4) 0.045(2) 0.166(5) 0.007(3) 0.122(4) 0.005(2) Cl1 0.0732(7) 0.0729(7) 0.1200(9) 0.0090(6) 0.0583(7) 0.0115(5) Cl2 0.1295(10) 0.0787(8) 0.1113(9) 0.0054(7) 0.0715(9) -0.0029(7) C1C 0.070(3) 0.057(3) 0.155(4) 0.006(3) 0.074(3) 0.002(2) C87 0.023(2) 0.153(4) 0.051(2) 0.026(3) 0.0117(18) -0.010(3) C202 0.040(3) 0.048(3) 0.030(3) -0.006(2) 0.010(2) -0.008(3) C205 0.092(6) 0.038(4) 0.047(4) 0.001(3) 0.014(5) -0.006(5) C203 0.042(3) 0.067(4) 0.040(3) -0.001(3) 0.010(3) -0.005(3) C206 0.055(4) 0.051(4) 0.034(3) 0.001(3) 0.011(3) -0.003(4) C208 0.024(5) 0.031(6) 0.033(5) 0.008(4) 0.008(5) 0.004(5) C211 0.081(9) 0.060(8) 0.035(6) 0.017(5) 0.021(6) -0.015(7) C210 0.080(9) 0.061(8) 0.028(6) -0.013(5) 0.015(6) -0.009(7) C209 0.044(8) 0.022(7) 0.047(7) -0.012(5) -0.007(7) 0.005(6) C36 0.115(5) 0.431(14) 0.067(4) -0.013(6) 0.027(4) -0.107(7) C31 0.022(2) 0.177(6) 0.047(3) -0.005(5) 0.000(2) -0.012(5) C32 0.075(4) 0.188(7) 0.035(3) 0.020(3) 0.016(3) 0.028(4) C33 0.097(6) 0.348(13) 0.043(4) 0.034(6) 0.015(4) 0.053(8) C34 0.054(4) 0.463(19) 0.058(5) -0.049(9) -0.024(4) 0.023(9) C35 0.074(5) 0.391(15) 0.058(5) -0.025(7) 0.020(4) -0.100(7) C2C 0.049(17) 0.040(18) 0.054(17) 0.021(16) 0.028(15) 0.027(18) Cl3 0.061(6) 0.036(5) 0.058(5) -0.012(4) 0.036(5) -0.018(4) Cl4 0.073(6) 0.111(8) 0.027(4) -0.008(5) 0.011(4) -0.003(6) _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 Ag1 C21 1.986(2) . ? Ag1 N24 2.029(2) . ? Ag1 N22 2.031(2) . ? Ag1 N23 2.059(2) . ? P O2 1.467(3) . ? P C32A 1.662(11) . ? P C45 1.803(4) . ? P C3 1.809(3) . ? P C31 1.891(5) . ? N23 C11 1.373(4) . ? N23 C14 1.377(3) . ? C101 C102 1.364(5) . ? C101 C106 1.376(4) . ? C101 C10 1.492(4) . ? N24 C16 1.387(3) . ? N24 C19 1.396(4) . ? N22 C9 1.380(3) . ? N22 C6 1.394(3) . ? N2 C3 1.310(4) . ? N2 C1 1.398(3) . ? C14 C15 1.384(4) . ? C14 C13 1.438(4) . ? C15 C16 1.403(4) . ? C15 C151 1.498(4) . ? C151 C152 1.384(4) . ? C151 C156 1.407(4) . ? C8 C7 1.351(4) . ? C8 C9 1.425(4) . ? C8 H8 0.9300 . ? C152 C153 1.394(5) . ? C152 H152 0.9300 . ? C19 C20 1.397(4) . ? C19 C18 1.431(4) . ? C4 C5 1.405(4) . ? C4 C21 1.415(4) . ? C4 C3 1.475(4) . ? C201 C206 1.228(6) . ? C201 C211 1.438(10) . ? C201 C202 1.459(5) . ? C201 C20 1.490(4) . ? C201 C208 1.554(10) . ? C10 C11 1.393(4) . ? C10 C9 1.397(4) . ? C51 C56 1.377(4) . ? C51 C52 1.385(4) . ? C51 C5 1.491(4) . ? C57 C54 1.515(4) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C107 C104 1.518(5) . ? C107 H10A 0.9600 . ? C107 H10B 0.9600 . ? C107 H10C 0.9600 . ? C204 C209 1.271(16) . ? C204 C210 1.306(12) . ? C204 C205 1.367(8) . ? C204 C203 1.466(6) . ? C204 C207 1.523(4) . ? C52 C53 1.363(4) . ? C52 H52 0.9300 . ? C1 C20 1.392(4) . ? C1 C21 1.397(4) . ? C13 C12 1.345(4) . ? C13 H13 0.9300 . ? C12 C11 1.457(4) . ? C12 H12 0.9300 . ? C55 C54 1.381(4) . ? C55 C56 1.398(4) . ? C55 H55 0.9300 . ? C27 C45 1.388(4) . ? C27 C49 1.401(5) . ? C27 H27 0.9300 . ? C16 C17 1.422(4) . ? C5 C6 1.394(4) . ? C7 C6 1.412(4) . ? C7 H7 0.9300 . ? C324 C49 1.362(5) . ? C324 C47 1.414(5) . ? C324 H324 0.9300 . ? C53 C54 1.383(4) . ? C53 H53 0.9300 . ? C102 C103 1.408(4) . ? C102 H102 0.9300 . ? C156 C155 1.395(5) . ? C156 H156 0.9300 . ? C207 H20A 0.9600 . ? C207 H20B 0.9600 . ? C207 H20C 0.9600 . ? C104 C105 1.340(6) . ? C104 C103 1.409(5) . ? C56 H56 0.9300 . ? C106 C105 1.374(5) . ? C106 H106 0.9300 . ? C18 C17 1.354(4) . ? C18 H18 0.9300 . ? C45 C87 1.409(5) . ? C17 H17 0.9300 . ? C47 C87 1.341(5) . ? C47 H47 0.9300 . ? C103 H103 0.9300 . ? C49 H49 0.9300 . ? C153 C154 1.396(6) . ? C153 H153 0.9300 . ? C154 C155 1.361(6) . ? C154 C157 1.529(5) . ? C105 H105 0.9300 . ? C157 H15A 0.9600 . ? C157 H15B 0.9600 . ? C157 H15C 0.9600 . ? C155 H155 0.9300 . ? Cl1 C1C 1.754(4) . ? Cl2 C1C 1.754(4) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C87 H87 0.9300 . ? C202 C203 1.391(6) . ? C202 H202 0.9300 . ? C205 C206 1.400(9) . ? C205 H205 0.9300 . ? C203 H203 0.9300 . ? C206 H206 0.9300 . ? C208 C209 1.371(16) . ? C208 H208 0.9300 . ? C211 C210 1.380(13) . ? C211 H211 0.9300 . ? C210 H210 0.9300 . ? C209 H209 0.9300 . ? C36 C31A 1.3994(10) . ? C36 C34A 1.3995(10) . ? C36 C34 1.3998(10) . ? C36 C35 1.4010(10) . ? C36 C33A 2.04(2) . ? C36 H36 0.9300 . ? C31 C35 1.3992(10) . ? C31 C32 1.4002(10) . ? C32 C33 1.3994(10) . ? C32 H32 0.9300 . ? C33 C34 1.4005(10) . ? C33 H33 0.9300 . ? C34 Cl4 2.139(12) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C32A C33A 1.3996(10) . ? C32A C35A 1.3997(10) . ? C33A C31A 1.4001(10) . ? C33A H33A 0.9300 . ? C35A C34A 1.3999(10) . ? C35A H35A 0.9300 . ? C31A H31A 0.9300 . ? C34A H34A 0.9300 . ? C2C Cl4 1.74(3) . ? C2C Cl3 1.75(3) . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? 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 C21 Ag1 N24 89.93(10) . . ? C21 Ag1 N22 88.82(10) . . ? N24 Ag1 N22 178.37(9) . . ? C21 Ag1 N23 177.20(11) . . ? N24 Ag1 N23 90.22(9) . . ? N22 Ag1 N23 91.09(9) . . ? O2 P C32A 90.5(4) . . ? O2 P C45 113.50(16) . . ? C32A P C45 117.3(4) . . ? O2 P C3 114.75(16) . . ? C32A P C3 111.1(5) . . ? C45 P C3 108.91(17) . . ? O2 P C31 116.9(2) . . ? C45 P C31 101.2(2) . . ? C3 P C31 99.91(17) . . ? C11 N23 C14 108.1(2) . . ? C11 N23 Ag1 125.29(19) . . ? C14 N23 Ag1 125.69(19) . . ? C102 C101 C106 117.4(3) . . ? C102 C101 C10 121.3(3) . . ? C106 C101 C10 121.2(3) . . ? C16 N24 C19 106.6(2) . . ? C16 N24 Ag1 125.1(2) . . ? C19 N24 Ag1 127.90(19) . . ? C9 N22 C6 107.2(2) . . ? C9 N22 Ag1 123.70(19) . . ? C6 N22 Ag1 127.68(19) . . ? C3 N2 C1 107.7(2) . . ? N23 C14 C15 125.3(3) . . ? N23 C14 C13 108.5(3) . . ? C15 C14 C13 126.0(3) . . ? C14 C15 C16 124.7(3) . . ? C14 C15 C151 117.9(3) . . ? C16 C15 C151 117.3(3) . . ? C152 C151 C156 118.0(3) . . ? C152 C151 C15 121.6(3) . . ? C156 C151 C15 120.4(3) . . ? C7 C8 C9 108.1(3) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? C151 C152 C153 121.1(4) . . ? C151 C152 H152 119.5 . . ? C153 C152 H152 119.5 . . ? N24 C19 C20 124.8(3) . . ? N24 C19 C18 108.4(3) . . ? C20 C19 C18 126.6(3) . . ? C5 C4 C21 126.6(2) . . ? C5 C4 C3 129.9(3) . . ? C21 C4 C3 103.4(2) . . ? C206 C201 C211 86.8(5) . . ? C206 C201 C202 121.8(4) . . ? C211 C201 C202 63.1(4) . . ? C206 C201 C20 122.3(4) . . ? C211 C201 C20 126.8(5) . . ? C202 C201 C20 115.5(3) . . ? C211 C201 C208 105.9(6) . . ? C202 C201 C208 101.8(4) . . ? C20 C201 C208 124.6(4) . . ? C11 C10 C9 125.0(3) . . ? C11 C10 C101 117.4(3) . . ? C9 C10 C101 117.6(3) . . ? C56 C51 C52 118.3(3) . . ? C56 C51 C5 118.8(3) . . ? C52 C51 C5 122.8(3) . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C104 C107 H10A 109.5 . . ? C104 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C104 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C209 C204 C210 121.1(8) . . ? C210 C204 C205 90.7(6) . . ? C209 C204 C203 107.0(7) . . ? C210 C204 C203 61.2(5) . . ? C205 C204 C203 113.1(5) . . ? C209 C204 C207 115.2(8) . . ? C210 C204 C207 119.5(5) . . ? C205 C204 C207 126.1(5) . . ? C203 C204 C207 120.5(4) . . ? C53 C52 C51 120.7(3) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C20 C1 C21 130.7(3) . . ? C20 C1 N2 119.5(3) . . ? C21 C1 N2 109.7(3) . . ? C12 C13 C14 107.8(3) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? C1 C21 C4 107.8(2) . . ? C1 C21 Ag1 124.0(2) . . ? C4 C21 Ag1 127.2(2) . . ? C13 C12 C11 107.5(3) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? N23 C11 C10 125.1(3) . . ? N23 C11 C12 107.9(3) . . ? C10 C11 C12 127.0(3) . . ? N2 C3 C4 111.3(2) . . ? N2 C3 P 111.0(2) . . ? C4 C3 P 137.7(3) . . ? C1 C20 C19 120.5(3) . . ? C1 C20 C201 118.2(3) . . ? C19 C20 C201 121.2(3) . . ? C54 C55 C56 120.7(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C45 C27 C49 119.2(4) . . ? C45 C27 H27 120.4 . . ? C49 C27 H27 120.4 . . ? N24 C16 C15 126.5(3) . . ? N24 C16 C17 109.0(3) . . ? C15 C16 C17 124.4(3) . . ? N22 C9 C10 127.2(3) . . ? N22 C9 C8 108.1(3) . . ? C10 C9 C8 124.6(3) . . ? C6 C5 C4 121.4(3) . . ? C6 C5 C51 117.6(3) . . ? C4 C5 C51 121.0(3) . . ? C8 C7 C6 108.2(3) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C49 C324 C47 119.6(4) . . ? C49 C324 H324 120.2 . . ? C47 C324 H324 120.2 . . ? C52 C53 C54 122.1(3) . . ? C52 C53 H53 119.0 . . ? C54 C53 H53 119.0 . . ? C5 C6 N22 125.9(3) . . ? C5 C6 C7 125.7(3) . . ? N22 C6 C7 108.3(2) . . ? C101 C102 C103 121.0(4) . . ? C101 C102 H102 119.5 . . ? C103 C102 H102 119.5 . . ? C155 C156 C151 119.8(4) . . ? C155 C156 H156 120.1 . . ? C151 C156 H156 120.1 . . ? C204 C207 H20A 109.5 . . ? C204 C207 H20B 109.5 . . ? H20A C207 H20B 109.5 . . ? C204 C207 H20C 109.5 . . ? H20A C207 H20C 109.5 . . ? H20B C207 H20C 109.5 . . ? C105 C104 C103 118.2(4) . . ? C105 C104 C107 121.3(4) . . ? C103 C104 C107 120.4(5) . . ? C51 C56 C55 120.7(3) . . ? C51 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C105 C106 C101 122.3(4) . . ? C105 C106 H106 118.9 . . ? C101 C106 H106 118.9 . . ? C55 C54 C53 117.5(3) . . ? C55 C54 C57 120.8(3) . . ? C53 C54 C57 121.6(3) . . ? C17 C18 C19 107.8(3) . . ? C17 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? C27 C45 C87 118.7(4) . . ? C27 C45 P 118.7(3) . . ? C87 C45 P 122.5(3) . . ? C18 C17 C16 108.0(3) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? C87 C47 C324 119.6(4) . . ? C87 C47 H47 120.2 . . ? C324 C47 H47 120.2 . . ? C102 C103 C104 119.6(4) . . ? C102 C103 H103 120.2 . . ? C104 C103 H103 120.2 . . ? C324 C49 C27 121.0(4) . . ? C324 C49 H49 119.5 . . ? C27 C49 H49 119.5 . . ? C152 C153 C154 120.6(4) . . ? C152 C153 H153 119.7 . . ? C154 C153 H153 119.7 . . ? C155 C154 C153 118.3(4) . . ? C155 C154 C157 121.2(6) . . ? C153 C154 C157 120.5(5) . . ? C104 C105 C106 121.4(4) . . ? C104 C105 H105 119.3 . . ? C106 C105 H105 119.3 . . ? C154 C157 H15A 109.5 . . ? C154 C157 H15B 109.5 . . ? H15A C157 H15B 109.5 . . ? C154 C157 H15C 109.5 . . ? H15A C157 H15C 109.5 . . ? H15B C157 H15C 109.5 . . ? C154 C155 C156 122.1(4) . . ? C154 C155 H155 118.9 . . ? C156 C155 H155 118.9 . . ? Cl1 C1C Cl2 111.1(2) . . ? Cl1 C1C H1C1 109.4 . . ? Cl2 C1C H1C1 109.4 . . ? Cl1 C1C H1C2 109.4 . . ? Cl2 C1C H1C2 109.4 . . ? H1C1 C1C H1C2 108.0 . . ? C47 C87 C45 121.7(4) . . ? C47 C87 H87 119.1 . . ? C45 C87 H87 119.1 . . ? C203 C202 C201 116.4(4) . . ? C203 C202 H202 121.8 . . ? C201 C202 H202 121.8 . . ? C204 C205 C206 123.9(7) . . ? C204 C205 H205 118.1 . . ? C206 C205 H205 118.1 . . ? C202 C203 C204 122.1(4) . . ? C202 C203 H203 118.9 . . ? C204 C203 H203 118.9 . . ? C201 C206 C205 122.2(6) . . ? C201 C206 H206 118.9 . . ? C205 C206 H206 118.9 . . ? C209 C208 C201 120.5(10) . . ? C209 C208 H208 119.8 . . ? C201 C208 H208 119.8 . . ? C210 C211 C201 122.8(9) . . ? C210 C211 H211 118.6 . . ? C201 C211 H211 118.6 . . ? C204 C210 C211 120.2(9) . . ? C204 C210 H210 119.9 . . ? C211 C210 H210 119.9 . . ? C204 C209 C208 120.7(13) . . ? C204 C209 H209 119.6 . . ? C208 C209 H209 119.6 . . ? C31A C36 C34A 149.3(9) . . ? C31A C36 C34 46.3(7) . . ? C34A C36 C34 139.6(9) . . ? C31A C36 C35 83.6(9) . . ? C34A C36 C35 67.2(6) . . ? C34 C36 C35 115.1(6) . . ? C34A C36 C33A 106.4(5) . . ? C34 C36 C33A 79.3(5) . . ? C31A C36 H36 138.4 . . ? C34A C36 H36 69.7 . . ? C34 C36 H36 122.5 . . ? C35 C36 H36 122.5 . . ? C33A C36 H36 151.9 . . ? C35 C31 C32 119.0(5) . . ? C35 C31 P 116.2(4) . . ? C32 C31 P 124.8(3) . . ? C33 C32 C31 121.2(6) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 116.7(6) . . ? C32 C33 H33 121.6 . . ? C34 C33 H33 121.6 . . ? C36 C34 C33 125.2(7) . . ? C36 C34 Cl4 137.5(7) . . ? C33 C34 Cl4 65.1(5) . . ? C36 C34 H34 117.4 . . ? C33 C34 H34 117.4 . . ? Cl4 C34 H34 69.9 . . ? C31 C35 C36 122.8(5) . . ? C31 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C33A C32A C35A 114.5(12) . . ? C33A C32A P 115.1(9) . . ? C35A C32A P 129.9(8) . . ? C32A C33A C31A 135.1(15) . . ? C32A C33A C36 91.9(10) . . ? C32A C33A H33A 112.5 . . ? C31A C33A H33A 112.5 . . ? C36 C33A H33A 155.4 . . ? C32A C35A C34A 124.5(9) . . ? C32A C35A H35A 117.7 . . ? C34A C35A H35A 117.7 . . ? C36 C31A C33A 93.3(13) . . ? C36 C31A H31A 133.4 . . ? C33A C31A H31A 133.4 . . ? C36 C34A C35A 102.6(7) . . ? C36 C34A H34A 128.7 . . ? C35A C34A H34A 128.7 . . ? Cl4 C2C Cl3 114.1(15) . . ? Cl4 C2C H2C1 108.7 . . ? Cl3 C2C H2C1 108.7 . . ? Cl4 C2C H2C2 108.7 . . ? Cl3 C2C H2C2 108.7 . . ? H2C1 C2C H2C2 107.6 . . ? C2C Cl4 C34 82.1(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N24 Ag1 N23 C11 177.3(2) . . . . ? N22 Ag1 N23 C11 -3.6(2) . . . . ? N24 Ag1 N23 C14 9.9(2) . . . . ? N22 Ag1 N23 C14 -171.0(2) . . . . ? C21 Ag1 N24 C16 -179.0(2) . . . . ? N23 Ag1 N24 C16 3.8(2) . . . . ? C21 Ag1 N24 C19 -6.3(2) . . . . ? N23 Ag1 N24 C19 176.5(2) . . . . ? C21 Ag1 N22 C9 172.3(2) . . . . ? N23 Ag1 N22 C9 -10.5(2) . . . . ? C21 Ag1 N22 C6 7.6(2) . . . . ? N23 Ag1 N22 C6 -175.2(2) . . . . ? C11 N23 C14 C15 174.0(3) . . . . ? Ag1 N23 C14 C15 -16.8(4) . . . . ? C11 N23 C14 C13 -3.2(3) . . . . ? Ag1 N23 C14 C13 166.06(17) . . . . ? N23 C14 C15 C16 7.5(5) . . . . ? C13 C14 C15 C16 -175.9(3) . . . . ? N23 C14 C15 C151 -173.5(3) . . . . ? C13 C14 C15 C151 3.2(4) . . . . ? C14 C15 C151 C152 60.4(4) . . . . ? C16 C15 C151 C152 -120.4(3) . . . . ? C14 C15 C151 C156 -118.8(3) . . . . ? C16 C15 C151 C156 60.3(4) . . . . ? C156 C151 C152 C153 0.1(5) . . . . ? C15 C151 C152 C153 -179.2(3) . . . . ? C16 N24 C19 C20 -172.0(3) . . . . ? Ag1 N24 C19 C20 14.2(4) . . . . ? C16 N24 C19 C18 3.4(3) . . . . ? Ag1 N24 C19 C18 -170.33(18) . . . . ? C102 C101 C10 C11 122.6(4) . . . . ? C106 C101 C10 C11 -59.9(4) . . . . ? C102 C101 C10 C9 -59.1(4) . . . . ? C106 C101 C10 C9 118.4(4) . . . . ? C56 C51 C52 C53 0.6(4) . . . . ? C5 C51 C52 C53 -176.3(3) . . . . ? C3 N2 C1 C20 176.4(3) . . . . ? C3 N2 C1 C21 0.4(4) . . . . ? N23 C14 C13 C12 2.9(3) . . . . ? C15 C14 C13 C12 -174.2(3) . . . . ? C20 C1 C21 C4 -174.5(3) . . . . ? N2 C1 C21 C4 1.0(3) . . . . ? C20 C1 C21 Ag1 15.8(5) . . . . ? N2 C1 C21 Ag1 -168.7(2) . . . . ? C5 C4 C21 C1 174.7(3) . . . . ? C3 C4 C21 C1 -1.7(3) . . . . ? C5 C4 C21 Ag1 -16.2(4) . . . . ? C3 C4 C21 Ag1 167.5(2) . . . . ? N24 Ag1 C21 C1 -7.0(3) . . . . ? N22 Ag1 C21 C1 174.0(3) . . . . ? N24 Ag1 C21 C4 -174.6(3) . . . . ? N22 Ag1 C21 C4 6.5(3) . . . . ? C14 C13 C12 C11 -1.5(3) . . . . ? C14 N23 C11 C10 -176.1(3) . . . . ? Ag1 N23 C11 C10 14.7(4) . . . . ? C14 N23 C11 C12 2.3(3) . . . . ? Ag1 N23 C11 C12 -167.02(17) . . . . ? C9 C10 C11 N23 -12.0(5) . . . . ? C101 C10 C11 N23 166.1(3) . . . . ? C9 C10 C11 C12 170.0(3) . . . . ? C101 C10 C11 C12 -11.9(4) . . . . ? C13 C12 C11 N23 -0.5(3) . . . . ? C13 C12 C11 C10 177.8(3) . . . . ? C1 N2 C3 C4 -1.5(4) . . . . ? C1 N2 C3 P 177.3(2) . . . . ? C5 C4 C3 N2 -174.2(3) . . . . ? C21 C4 C3 N2 2.1(3) . . . . ? C5 C4 C3 P 7.5(6) . . . . ? C21 C4 C3 P -176.3(3) . . . . ? O2 P C3 N2 94.4(3) . . . . ? C32A P C3 N2 -6.5(5) . . . . ? C45 P C3 N2 -137.1(2) . . . . ? C31 P C3 N2 -31.5(3) . . . . ? O2 P C3 C4 -87.2(4) . . . . ? C32A P C3 C4 171.9(5) . . . . ? C45 P C3 C4 41.2(4) . . . . ? C31 P C3 C4 146.8(4) . . . . ? C21 C1 C20 C19 -8.7(5) . . . . ? N2 C1 C20 C19 176.1(3) . . . . ? C21 C1 C20 C201 172.6(3) . . . . ? N2 C1 C20 C201 -2.5(4) . . . . ? N24 C19 C20 C1 -7.3(4) . . . . ? C18 C19 C20 C1 178.1(3) . . . . ? N24 C19 C20 C201 171.3(3) . . . . ? C18 C19 C20 C201 -3.3(5) . . . . ? C206 C201 C20 C1 -111.5(5) . . . . ? C211 C201 C20 C1 135.5(6) . . . . ? C202 C201 C20 C1 61.1(4) . . . . ? C208 C201 C20 C1 -66.0(6) . . . . ? C206 C201 C20 C19 69.8(5) . . . . ? C211 C201 C20 C19 -43.1(7) . . . . ? C202 C201 C20 C19 -117.5(4) . . . . ? C208 C201 C20 C19 115.3(5) . . . . ? C19 N24 C16 C15 172.9(3) . . . . ? Ag1 N24 C16 C15 -13.1(4) . . . . ? C19 N24 C16 C17 -3.7(3) . . . . ? Ag1 N24 C16 C17 170.22(18) . . . . ? C14 C15 C16 N24 8.7(5) . . . . ? C151 C15 C16 N24 -170.3(3) . . . . ? C14 C15 C16 C17 -175.1(3) . . . . ? C151 C15 C16 C17 5.8(4) . . . . ? C6 N22 C9 C10 -176.2(3) . . . . ? Ag1 N22 C9 C10 16.4(4) . . . . ? C6 N22 C9 C8 2.9(3) . . . . ? Ag1 N22 C9 C8 -164.58(18) . . . . ? C11 C10 C9 N22 -5.0(5) . . . . ? C101 C10 C9 N22 176.8(3) . . . . ? C11 C10 C9 C8 176.1(3) . . . . ? C101 C10 C9 C8 -2.0(4) . . . . ? C7 C8 C9 N22 -2.3(3) . . . . ? C7 C8 C9 C10 176.8(3) . . . . ? C21 C4 C5 C6 10.2(5) . . . . ? C3 C4 C5 C6 -174.4(3) . . . . ? C21 C4 C5 C51 -167.6(3) . . . . ? C3 C4 C5 C51 7.9(5) . . . . ? C56 C51 C5 C6 -121.2(3) . . . . ? C52 C51 C5 C6 55.7(4) . . . . ? C56 C51 C5 C4 56.7(4) . . . . ? C52 C51 C5 C4 -126.5(3) . . . . ? C9 C8 C7 C6 0.8(3) . . . . ? C51 C52 C53 C54 0.1(5) . . . . ? C4 C5 C6 N22 5.7(5) . . . . ? C51 C5 C6 N22 -176.4(3) . . . . ? C4 C5 C6 C7 -173.1(3) . . . . ? C51 C5 C6 C7 4.7(4) . . . . ? C9 N22 C6 C5 178.6(3) . . . . ? Ag1 N22 C6 C5 -14.7(4) . . . . ? C9 N22 C6 C7 -2.4(3) . . . . ? Ag1 N22 C6 C7 164.37(18) . . . . ? C8 C7 C6 C5 -180.0(3) . . . . ? C8 C7 C6 N22 1.0(3) . . . . ? C106 C101 C102 C103 1.1(5) . . . . ? C10 C101 C102 C103 178.7(3) . . . . ? C152 C151 C156 C155 -0.2(5) . . . . ? C15 C151 C156 C155 179.1(3) . . . . ? C52 C51 C56 C55 0.0(4) . . . . ? C5 C51 C56 C55 177.0(3) . . . . ? C54 C55 C56 C51 -1.4(4) . . . . ? C102 C101 C106 C105 -0.9(5) . . . . ? C10 C101 C106 C105 -178.4(3) . . . . ? C56 C55 C54 C53 2.1(4) . . . . ? C56 C55 C54 C57 179.8(3) . . . . ? C52 C53 C54 C55 -1.5(4) . . . . ? C52 C53 C54 C57 -179.2(3) . . . . ? N24 C19 C18 C17 -1.8(3) . . . . ? C20 C19 C18 C17 173.5(3) . . . . ? C49 C27 C45 C87 -0.3(5) . . . . ? C49 C27 C45 P -177.0(3) . . . . ? O2 P C45 C27 -16.8(3) . . . . ? C32A P C45 C27 86.8(6) . . . . ? C3 P C45 C27 -146.0(3) . . . . ? C31 P C45 C27 109.4(3) . . . . ? O2 P C45 C87 166.6(3) . . . . ? C32A P C45 C87 -89.7(6) . . . . ? C3 P C45 C87 37.5(3) . . . . ? C31 P C45 C87 -67.2(3) . . . . ? C19 C18 C17 C16 -0.5(3) . . . . ? N24 C16 C17 C18 2.7(3) . . . . ? C15 C16 C17 C18 -174.1(3) . . . . ? C49 C324 C47 C87 -2.0(6) . . . . ? C101 C102 C103 C104 0.7(6) . . . . ? C105 C104 C103 C102 -2.7(6) . . . . ? C107 C104 C103 C102 179.6(4) . . . . ? C47 C324 C49 C27 0.3(5) . . . . ? C45 C27 C49 C324 0.8(5) . . . . ? C151 C152 C153 C154 -0.2(5) . . . . ? C152 C153 C154 C155 0.5(6) . . . . ? C152 C153 C154 C157 -178.8(3) . . . . ? C103 C104 C105 C106 2.9(7) . . . . ? C107 C104 C105 C106 -179.3(4) . . . . ? C101 C106 C105 C104 -1.2(6) . . . . ? C153 C154 C155 C156 -0.6(6) . . . . ? C157 C154 C155 C156 178.6(3) . . . . ? C151 C156 C155 C154 0.5(6) . . . . ? C324 C47 C87 C45 2.6(6) . . . . ? C27 C45 C87 C47 -1.4(5) . . . . ? P C45 C87 C47 175.1(3) . . . . ? C206 C201 C202 C203 -4.2(7) . . . . ? C211 C201 C202 C203 62.9(6) . . . . ? C20 C201 C202 C203 -176.9(4) . . . . ? C208 C201 C202 C203 -39.0(6) . . . . ? C209 C204 C205 C206 -96.1(17) . . . . ? C210 C204 C205 C206 50.7(9) . . . . ? C203 C204 C205 C206 -8.1(10) . . . . ? C207 C204 C205 C206 178.9(5) . . . . ? C201 C202 C203 C204 0.5(7) . . . . ? C209 C204 C203 C202 44.4(9) . . . . ? C210 C204 C203 C202 -72.2(7) . . . . ? C205 C204 C203 C202 5.2(8) . . . . ? C207 C204 C203 C202 178.7(4) . . . . ? C211 C201 C206 C205 -53.7(8) . . . . ? C202 C201 C206 C205 1.7(9) . . . . ? C20 C201 C206 C205 173.9(5) . . . . ? C208 C201 C206 C205 67.6(9) . . . . ? C204 C205 C206 C201 5.1(11) . . . . ? C206 C201 C208 C209 -84.4(10) . . . . ? C211 C201 C208 C209 -21.9(10) . . . . ? C202 C201 C208 C209 43.2(8) . . . . ? C20 C201 C208 C209 175.9(6) . . . . ? C206 C201 C211 C210 57.8(10) . . . . ? C202 C201 C211 C210 -70.5(9) . . . . ? C20 C201 C211 C210 -173.4(7) . . . . ? C208 C201 C211 C210 24.9(11) . . . . ? C209 C204 C210 C211 -21.8(14) . . . . ? C205 C204 C210 C211 -44.6(10) . . . . ? C203 C204 C210 C211 71.6(9) . . . . ? C207 C204 C210 C211 -177.7(7) . . . . ? C201 C211 C210 C204 -6.1(14) . . . . ? C210 C204 C209 C208 24.4(13) . . . . ? C205 C204 C209 C208 64.1(13) . . . . ? C203 C204 C209 C208 -41.8(10) . . . . ? C207 C204 C209 C208 -178.8(7) . . . . ? C201 C208 C209 C204 -0.6(12) . . . . ? O2 P C31 C35 -1.1(6) . . . . ? C32A P C31 C35 5.4(11) . . . . ? C45 P C31 C35 -125.0(6) . . . . ? C3 P C31 C35 123.3(6) . . . . ? O2 P C31 C32 -179.6(5) . . . . ? C32A P C31 C32 -173.1(13) . . . . ? C45 P C31 C32 56.6(5) . . . . ? C3 P C31 C32 -55.2(6) . . . . ? C35 C31 C32 C33 1.1(10) . . . . ? P C31 C32 C33 179.6(5) . . . . ? C31 C32 C33 C34 -1.1(10) . . . . ? C31A C36 C34 C33 51.9(12) . . . . ? C34A C36 C34 C33 -83.5(14) . . . . ? C35 C36 C34 C33 0.1(14) . . . . ? C33A C36 C34 C33 19.4(10) . . . . ? C31A C36 C34 Cl4 142.3(13) . . . . ? C34A C36 C34 Cl4 7.0(15) . . . . ? C35 C36 C34 Cl4 90.6(11) . . . . ? C33A C36 C34 Cl4 109.8(9) . . . . ? C32 C33 C34 C36 0.4(13) . . . . ? C32 C33 C34 Cl4 -131.4(7) . . . . ? C32 C31 C35 C36 -0.6(12) . . . . ? P C31 C35 C36 -179.1(7) . . . . ? C31A C36 C35 C31 -34.9(12) . . . . ? C34A C36 C35 C31 135.6(10) . . . . ? C34 C36 C35 C31 -0.1(13) . . . . ? C33A C36 C35 C31 -30.0(7) . . . . ? O2 P C32A C33A 142.9(8) . . . . ? C45 P C32A C33A 25.9(10) . . . . ? C3 P C32A C33A -100.2(8) . . . . ? C31 P C32A C33A -31.3(8) . . . . ? O2 P C32A C35A -45.8(12) . . . . ? C45 P C32A C35A -162.8(10) . . . . ? C3 P C32A C35A 71.0(13) . . . . ? C31 P C32A C35A 140(2) . . . . ? C35A C32A C33A C31A -0.7(15) . . . . ? P C32A C33A C31A 171.9(13) . . . . ? C35A C32A C33A C36 3.1(10) . . . . ? P C32A C33A C36 175.8(8) . . . . ? C31A C36 C33A C32A -176.0(10) . . . . ? C34A C36 C33A C32A -2.8(10) . . . . ? C34 C36 C33A C32A -141.6(8) . . . . ? C35 C36 C33A C32A 11.0(8) . . . . ? C34A C36 C33A C31A 173.2(13) . . . . ? C34 C36 C33A C31A 34.5(10) . . . . ? C35 C36 C33A C31A -173.0(13) . . . . ? C33A C32A C35A C34A -3.4(16) . . . . ? P C32A C35A C34A -174.7(10) . . . . ? C34A C36 C31A C33A -13(3) . . . . ? C34 C36 C31A C33A -129.7(13) . . . . ? C35 C36 C31A C33A 4.6(9) . . . . ? C32A C33A C31A C36 5.6(14) . . . . ? C31A C36 C34A C35A 10(3) . . . . ? C34 C36 C34A C35A 94.0(11) . . . . ? C35 C36 C34A C35A -8.4(7) . . . . ? C33A C36 C34A C35A 1.3(10) . . . . ? C32A C35A C34A C36 0.8(14) . . . . ? Cl3 C2C Cl4 C34 -77.8(15) . . . . ? C36 C34 Cl4 C2C -75.5(13) . . . . ? C33 C34 Cl4 C2C 40.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.692 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.080 # Attachment '- PS.cif' data_ng07 _database_code_depnum_ccdc_archive 'CCDC 893467' #TrackingRef '- PS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,10,15,20-tetratolyl-2-aza-21-diphenylthiophosphoryl-21-carbaporphiryn 2.6 dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122.58 H99.16 Cl5.16 N8 P2 S2' _chemical_formula_weight 1993.20 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 14.482(3) _cell_length_b 13.250(3) _cell_length_c 29.776(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.67(3) _cell_angle_gamma 90.00 _cell_volume 5106(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2081 _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48890 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 36.95 _reflns_number_total 24762 _reflns_number_gt 16579 _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^)+(0.0900P)^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 0.47(6) _refine_ls_number_reflns 24762 _refine_ls_number_parameters 1322 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.001 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 S1 S 0.41223(10) 0.74533(7) 0.44747(5) 0.02571(19) Uani 1 1 d . . . P1 P 0.34693(10) 0.63740(6) 0.46799(5) 0.01885(17) Uani 1 1 d . . . N2 N 0.1624(2) 0.4119(2) 0.38897(12) 0.0262(7) Uani 1 1 d . . . N22 N 0.3628(2) 0.5861(2) 0.35748(11) 0.0190(6) Uani 1 1 d . . . H22 H 0.3018 0.6099 0.3486 0.023 Uiso 1 1 d R . . N23 N 0.2716(2) 0.7956(2) 0.32903(11) 0.0176(5) Uani 1 1 d . . . H23 H 0.2651 0.7510 0.3484 0.021 Uiso 1 1 d R . . N24 N 0.1355(2) 0.7633(2) 0.37481(11) 0.0174(6) Uani 1 1 d . . . C1 C 0.1408(2) 0.5633(3) 0.41736(13) 0.0195(7) Uani 1 1 d . . . C3 C 0.0979(3) 0.4670(2) 0.39860(13) 0.0179(6) Uani 1 1 d . . . H3 H 0.0329 0.4458 0.3938 0.022 Uiso 1 1 calc R . . C4 C 0.2537(3) 0.4684(2) 0.40254(13) 0.0193(7) Uani 1 1 d . . . C5 C 0.3374(2) 0.4295(2) 0.39509(13) 0.0185(6) Uani 1 1 d . . . C6 C 0.3971(2) 0.4953(2) 0.38188(13) 0.0181(7) Uani 1 1 d . . . C7 C 0.5005(3) 0.4848(3) 0.38911(15) 0.0235(7) Uani 1 1 d . . . H7 H 0.5439 0.4303 0.4041 0.028 Uiso 1 1 calc R . . C8 C 0.5250(3) 0.5687(3) 0.37013(14) 0.0228(7) Uani 1 1 d . . . H8 H 0.5886 0.5815 0.3707 0.027 Uiso 1 1 calc R . . C9 C 0.4371(2) 0.6335(3) 0.34929(13) 0.0180(6) Uani 1 1 d . . . C10 C 0.4277(2) 0.7254(2) 0.32473(13) 0.0175(6) Uani 1 1 d . . . C11 C 0.3452(2) 0.7945(3) 0.31132(13) 0.0180(6) Uani 1 1 d . . . C12 C 0.3234(3) 0.8770(3) 0.27731(13) 0.0200(7) Uani 1 1 d . . . H12 H 0.3591 0.8928 0.2589 0.024 Uiso 1 1 calc R . . C13 C 0.2414(3) 0.9287(3) 0.27635(13) 0.0188(7) Uani 1 1 d . . . H13 H 0.2109 0.9857 0.2572 0.023 Uiso 1 1 calc R . . C14 C 0.2105(2) 0.8788(2) 0.31052(13) 0.0169(6) Uani 1 1 d . . . C15 C 0.1355(2) 0.9119(2) 0.32471(13) 0.0163(6) Uani 1 1 d . . . C16 C 0.1082(2) 0.8598(3) 0.35865(14) 0.0186(6) Uani 1 1 d . . . C17 C 0.0444(3) 0.9021(3) 0.38028(14) 0.0217(7) Uani 1 1 d . . . H17 H 0.0170 0.9669 0.3754 0.026 Uiso 1 1 calc R . . C18 C 0.0328(3) 0.8290(3) 0.40880(14) 0.0209(7) Uani 1 1 d . . . H18 H -0.0034 0.8343 0.4278 0.025 Uiso 1 1 calc R . . C19 C 0.0870(3) 0.7410(2) 0.40447(13) 0.0185(6) Uani 1 1 d . . . C20 C 0.0791(3) 0.6431(2) 0.42060(13) 0.0174(6) Uani 1 1 d . . . C21 C 0.2434(3) 0.5637(2) 0.42212(13) 0.0170(6) Uani 1 1 d . . . C22 C 0.4420(3) 0.5438(3) 0.50548(13) 0.0200(7) Uani 1 1 d . . . C23 C 0.4137(3) 0.4498(3) 0.51657(14) 0.0219(7) Uani 1 1 d . . . H1 H 0.3441 0.4329 0.5033 0.026 Uiso 1 1 calc R . . C24 C 0.4875(3) 0.3814(3) 0.54692(14) 0.0251(8) Uani 1 1 d . . . H24 H 0.4675 0.3180 0.5528 0.030 Uiso 1 1 calc R . . C25 C 0.5912(3) 0.4073(3) 0.56857(15) 0.0306(9) Uani 1 1 d . . . H25 H 0.6408 0.3623 0.5899 0.037 Uiso 1 1 calc R . . C26 C 0.6203(3) 0.4992(3) 0.55845(16) 0.0338(9) Uani 1 1 d . . . H26 H 0.6900 0.5163 0.5728 0.041 Uiso 1 1 calc R . . C27 C 0.5459(3) 0.5687(3) 0.52644(14) 0.0257(8) Uani 1 1 d . . . H27 H 0.5665 0.6308 0.5195 0.031 Uiso 1 1 calc R . . C28 C 0.3024(3) 0.6865(3) 0.51230(13) 0.0204(7) Uani 1 1 d . . . C29 C 0.2799(3) 0.6244(3) 0.54371(15) 0.0248(7) Uani 1 1 d . . . H29 H 0.2803 0.5548 0.5399 0.030 Uiso 1 1 calc R . . C30 C 0.2568(3) 0.6637(3) 0.58038(16) 0.0324(9) Uani 1 1 d . . . H30 H 0.2410 0.6209 0.6007 0.039 Uiso 1 1 calc R . . C31 C 0.2573(3) 0.7674(3) 0.58679(16) 0.0335(9) Uani 1 1 d . . . H31 H 0.2435 0.7944 0.6119 0.040 Uiso 1 1 calc R . . C32 C 0.2786(3) 0.8302(3) 0.55556(17) 0.0347(9) Uani 1 1 d . . . H32 H 0.2779 0.8998 0.5595 0.042 Uiso 1 1 calc R . . C33 C 0.3009(3) 0.7908(3) 0.51855(15) 0.0286(8) Uani 1 1 d . . . H33 H 0.3150 0.8340 0.4977 0.034 Uiso 1 1 calc R . . C51 C 0.3597(3) 0.3218(3) 0.39875(14) 0.0212(7) Uani 1 1 d . . . C52 C 0.3403(3) 0.2597(3) 0.43194(15) 0.0250(7) Uani 1 1 d . . . H52 H 0.3097 0.2871 0.4508 0.030 Uiso 1 1 calc R . . C53 C 0.3660(3) 0.1588(3) 0.43684(15) 0.0272(8) Uani 1 1 d . . . H53 H 0.3527 0.1196 0.4592 0.033 Uiso 1 1 calc R . . C54 C 0.4107(3) 0.1140(3) 0.40960(16) 0.0292(8) Uani 1 1 d . . . C55 C 0.4271(3) 0.1743(3) 0.37572(15) 0.0270(8) Uani 1 1 d . . . H55 H 0.4558 0.1454 0.3564 0.032 Uiso 1 1 calc R . . C56 C 0.4023(3) 0.2753(3) 0.36971(15) 0.0244(7) Uani 1 1 d . . . H56 H 0.4137 0.3131 0.3464 0.029 Uiso 1 1 calc R . . C57 C 0.4385(4) 0.0034(3) 0.41557(18) 0.0404(10) Uani 1 1 d . . . H57A H 0.4200 -0.0260 0.4399 0.061 Uiso 1 1 calc R . . H57B H 0.5115 -0.0040 0.4267 0.061 Uiso 1 1 calc R . . H57C H 0.4016 -0.0302 0.3839 0.061 Uiso 1 1 calc R . . C61 C 0.5150(2) 0.7561(3) 0.31369(13) 0.0192(7) Uani 1 1 d . . . C62 C 0.5520(3) 0.6914(3) 0.28864(14) 0.0212(7) Uani 1 1 d . . . H62 H 0.5215 0.6285 0.2781 0.025 Uiso 1 1 calc R . . C63 C 0.6341(3) 0.7199(3) 0.27930(14) 0.0252(8) Uani 1 1 d . . . H63 H 0.6572 0.6758 0.2622 0.030 Uiso 1 1 calc R . . C64 C 0.6823(3) 0.8130(3) 0.29495(16) 0.0302(9) Uani 1 1 d . . . C65 C 0.6479(3) 0.8747(3) 0.32202(17) 0.0306(9) Uani 1 1 d . . . H65 H 0.6808 0.9360 0.3344 0.037 Uiso 1 1 calc R . . C66 C 0.5658(3) 0.8468(3) 0.33086(16) 0.0252(8) Uani 1 1 d . . . H66 H 0.5441 0.8900 0.3488 0.030 Uiso 1 1 calc R . . C67 C 0.7707(3) 0.8444(4) 0.28453(18) 0.0388(10) Uani 1 1 d . . . H67A H 0.8189 0.7897 0.2924 0.058 Uiso 1 1 calc R . . H67B H 0.8049 0.9018 0.3049 0.058 Uiso 1 1 calc R . . H67C H 0.7448 0.8618 0.2497 0.058 Uiso 1 1 calc R . . C71 C 0.0840(3) 1.0102(2) 0.30666(13) 0.0177(6) Uani 1 1 d . . . C72 C 0.1384(3) 1.1013(3) 0.31634(14) 0.0219(7) Uani 1 1 d . . . H72 H 0.2102 1.1004 0.3308 0.026 Uiso 1 1 calc R . . C73 C 0.0874(3) 1.1917(3) 0.30483(16) 0.0267(8) Uani 1 1 d . . . H73 H 0.1258 1.2510 0.3119 0.032 Uiso 1 1 calc R . . C74 C -0.0203(3) 1.1982(3) 0.28288(15) 0.0247(7) Uani 1 1 d . . . C75 C -0.0744(3) 1.1068(3) 0.27100(15) 0.0256(8) Uani 1 1 d . . . H75 H -0.1463 1.1077 0.2548 0.031 Uiso 1 1 calc R . . C76 C -0.0234(3) 1.0153(3) 0.28286(14) 0.0214(7) Uani 1 1 d . . . H76 H -0.0616 0.9559 0.2748 0.026 Uiso 1 1 calc R . . C77 C -0.0765(3) 1.2978(3) 0.27251(18) 0.0353(9) Uani 1 1 d . . . H77A H -0.1307 1.2941 0.2826 0.053 Uiso 1 1 calc R . . H77B H -0.1056 1.3125 0.2372 0.053 Uiso 1 1 calc R . . H77C H -0.0289 1.3502 0.2911 0.053 Uiso 1 1 calc R . . C81 C -0.0034(2) 0.6208(2) 0.43559(13) 0.0184(7) Uani 1 1 d . . . C82 C -0.1018(3) 0.6639(3) 0.41054(14) 0.0207(7) Uani 1 1 d . . . H82 H -0.1171 0.7062 0.3832 0.025 Uiso 1 1 calc R . . C83 C -0.1777(3) 0.6433(3) 0.42669(14) 0.0254(8) Uani 1 1 d . . . H83 H -0.2423 0.6737 0.4105 0.030 Uiso 1 1 calc R . . C84 C -0.1570(3) 0.5790(3) 0.46610(15) 0.0265(8) Uani 1 1 d . . . C85 C -0.0607(3) 0.5337(3) 0.48982(15) 0.0271(8) Uani 1 1 d . . . H85 H -0.0468 0.4890 0.5162 0.033 Uiso 1 1 calc R . . C86 C 0.0154(3) 0.5539(3) 0.47482(14) 0.0215(7) Uani 1 1 d . . . H86 H 0.0794 0.5225 0.4911 0.026 Uiso 1 1 calc R . . C87 C -0.2363(3) 0.5567(4) 0.48475(17) 0.0426(11) Uani 1 1 d . . . H87A H -0.2072 0.5706 0.5201 0.064 Uiso 1 1 calc R . . H87B H -0.2560 0.4869 0.4789 0.064 Uiso 1 1 calc R . . H87C H -0.2960 0.5984 0.4671 0.064 Uiso 1 1 calc R . . S2 S 0.15166(10) 0.60323(7) 0.08730(5) 0.0282(2) Uani 1 1 d . . . P2 P 0.11495(10) 0.74582(7) 0.08113(5) 0.01984(18) Uani 1 1 d . . . N2A N 0.2395(2) 1.0001(2) 0.15334(12) 0.0241(6) Uani 1 1 d . . . N22A N 0.3390(2) 0.6500(2) 0.18634(11) 0.0183(6) Uani 1 1 d . . . H22A H 0.2997 0.6853 0.1950 0.022 Uiso 1 1 d R . . N23A N 0.1802(2) 0.6021(2) 0.22047(12) 0.0198(6) Uani 1 1 d . . . N24A N 0.0642(2) 0.7919(2) 0.18496(11) 0.0184(6) Uani 1 1 d . . . H24A H 0.1205 0.7671 0.1866 0.022 Uiso 1 1 d R . . C1A C 0.1609(3) 0.9265(2) 0.14110(13) 0.0184(7) Uani 1 1 d . . . C3A C 0.3179(3) 0.9538(3) 0.15153(13) 0.0200(7) Uani 1 1 d . . . H3A H 0.3798 0.9856 0.1579 0.024 Uiso 1 1 calc R . . C4A C 0.2986(2) 0.8508(3) 0.13891(13) 0.0192(7) Uani 1 1 d . . . C5A C 0.3760(3) 0.7843(3) 0.14009(13) 0.0198(7) Uani 1 1 d . . . C6A C 0.3878(2) 0.6867(3) 0.15934(14) 0.0201(7) Uani 1 1 d . . . C7A C 0.4478(3) 0.6052(3) 0.15525(15) 0.0253(8) Uani 1 1 d . . . H7A H 0.4912 0.6077 0.1398 0.030 Uiso 1 1 calc R . . C8A C 0.4306(3) 0.5233(3) 0.17771(14) 0.0237(7) Uani 1 1 d . . . H8A H 0.4592 0.4595 0.1800 0.028 Uiso 1 1 calc R . . C9A C 0.3606(2) 0.5525(3) 0.19731(13) 0.0188(7) Uani 1 1 d . . . C10A C 0.3195(2) 0.4898(3) 0.22274(13) 0.0180(7) Uani 1 1 d . . . C11A C 0.2392(2) 0.5159(3) 0.23468(13) 0.0202(7) Uani 1 1 d . . . C12A C 0.2021(3) 0.4481(3) 0.26122(14) 0.0223(7) Uani 1 1 d . . . H12A H 0.2305 0.3861 0.2753 0.027 Uiso 1 1 calc R . . C13A C 0.1195(3) 0.4917(3) 0.26164(14) 0.0216(7) Uani 1 1 d . . . H13A H 0.0791 0.4659 0.2759 0.026 Uiso 1 1 calc R . . C14A C 0.1048(2) 0.5872(2) 0.23548(13) 0.0182(7) Uani 1 1 d . . . C15A C 0.0188(2) 0.6496(2) 0.22458(13) 0.0175(6) Uani 1 1 d . . . C16A C 0.0019(3) 0.7438(3) 0.20158(13) 0.0183(7) Uani 1 1 d . . . C17A C -0.0829(3) 0.8107(3) 0.19143(14) 0.0237(7) Uani 1 1 d . . . H17A H -0.1384 0.7984 0.1984 0.028 Uiso 1 1 calc R . . C18A C -0.0679(3) 0.8950(3) 0.16991(14) 0.0224(7) Uani 1 1 d . . . H18A H -0.1118 0.9505 0.1597 0.027 Uiso 1 1 calc R . . C19A C 0.0251(3) 0.8855(2) 0.16542(13) 0.0185(7) Uani 1 1 d . . . C20A C 0.0729(3) 0.9542(3) 0.14707(13) 0.0188(7) Uani 1 1 d . . . C21A C 0.1951(2) 0.8315(2) 0.13073(13) 0.0173(6) Uani 1 1 d . . . C22A C 0.1192(3) 0.8005(3) 0.02625(14) 0.0249(7) Uani 1 1 d . . . C23A C 0.1354(3) 0.9044(3) 0.02283(15) 0.0248(7) Uani 1 1 d . . . H23A H 0.1443 0.9470 0.0493 0.030 Uiso 1 1 calc R . . C24A C 0.1381(3) 0.9433(3) -0.01954(16) 0.0324(9) Uani 1 1 d . . . H2 H 0.1480 1.0122 -0.0216 0.039 Uiso 1 1 calc R . . C25A C 0.1266(4) 0.8814(4) -0.05848(19) 0.0498(13) Uani 1 1 d . . . H25A H 0.1280 0.9081 -0.0871 0.060 Uiso 1 1 calc R . . C26A C 0.1130(5) 0.7812(4) -0.05517(19) 0.0619(17) Uani 1 1 d . . . H26A H 0.1066 0.7391 -0.0814 0.074 Uiso 1 1 calc R . . C27A C 0.1086(4) 0.7402(3) -0.01366(17) 0.0460(12) Uani 1 1 d . . . H27A H 0.0983 0.6711 -0.0125 0.055 Uiso 1 1 calc R . . C28A C -0.0205(3) 0.7596(3) 0.06727(14) 0.0251(7) Uani 1 1 d . . . C29A C -0.0813(3) 0.8403(4) 0.03961(16) 0.0374(10) Uani 1 1 d . . . H29A H -0.0499 0.8935 0.0313 0.045 Uiso 1 1 calc R . . C30A C -0.1840(3) 0.8438(4) 0.02451(19) 0.0471(12) Uani 1 1 d . . . H30A H -0.2231 0.8978 0.0055 0.056 Uiso 1 1 calc R . . C31A C -0.2316(4) 0.7640(5) 0.0380(2) 0.0569(15) Uani 1 1 d . . . H31A H -0.3023 0.7657 0.0282 0.068 Uiso 1 1 calc R . . C32A C -0.1738(4) 0.6847(4) 0.06548(19) 0.0443(11) Uani 1 1 d . . . H32A H -0.2050 0.6320 0.0742 0.053 Uiso 1 1 calc R . . C33A C -0.0681(3) 0.6828(3) 0.08037(16) 0.0338(9) Uani 1 1 d . . . H33A H -0.0288 0.6290 0.0995 0.041 Uiso 1 1 calc R . . C51A C 0.4517(3) 0.8273(3) 0.12393(14) 0.0227(7) Uani 1 1 d . . . C52A C 0.4139(3) 0.8930(3) 0.08238(15) 0.0252(8) Uani 1 1 d . . . H52A H 0.3433 0.9048 0.0649 0.030 Uiso 1 1 calc R . . C53A C 0.4798(3) 0.9398(3) 0.06730(16) 0.0320(9) Uani 1 1 d . . . H53A H 0.4530 0.9840 0.0402 0.038 Uiso 1 1 calc R . . C54A C 0.5861(3) 0.9226(4) 0.09160(18) 0.0427(11) Uani 1 1 d . . . C55A C 0.6223(3) 0.8571(4) 0.13195(19) 0.0468(12) Uani 1 1 d . . . H55A H 0.6929 0.8444 0.1488 0.056 Uiso 1 1 calc R . . C56A C 0.5568(3) 0.8086(3) 0.14855(16) 0.0335(9) Uani 1 1 d . . . H56A H 0.5838 0.7645 0.1757 0.040 Uiso 1 1 calc R . . C57A C 0.6583(4) 0.9773(5) 0.0763(2) 0.0732(19) Uani 1 1 d . . . H57D H 0.6200 1.0046 0.0432 0.110 Uiso 1 1 calc R . . H57E H 0.7095 0.9311 0.0764 0.110 Uiso 1 1 calc R . . H57F H 0.6917 1.0311 0.0996 0.110 Uiso 1 1 calc R . . C61A C 0.3657(3) 0.3868(3) 0.23606(14) 0.0205(7) Uani 1 1 d . . . C62A C 0.4714(3) 0.3761(3) 0.26789(15) 0.0240(7) Uani 1 1 d . . . H62A H 0.5123 0.4331 0.2809 0.029 Uiso 1 1 calc R . . C63A C 0.5149(3) 0.2815(3) 0.27994(15) 0.0284(8) Uani 1 1 d . . . H63A H 0.5852 0.2752 0.3013 0.034 Uiso 1 1 calc R . . C64A C 0.4560(3) 0.1955(3) 0.26080(16) 0.0330(9) Uani 1 1 d . . . C65A C 0.3517(3) 0.2060(3) 0.22982(17) 0.0356(9) Uani 1 1 d . . . H65A H 0.3107 0.1489 0.2173 0.043 Uiso 1 1 calc R . . C66A C 0.3079(3) 0.3005(3) 0.21734(16) 0.0303(8) Uani 1 1 d . . . H66A H 0.2377 0.3062 0.1958 0.036 Uiso 1 1 calc R . . C67A C 0.5053(4) 0.0910(3) 0.2737(2) 0.0486(12) Uani 1 1 d . . . H67D H 0.5757 0.0971 0.2988 0.073 Uiso 1 1 calc R . . H67E H 0.5033 0.0605 0.2441 0.073 Uiso 1 1 calc R . . H67F H 0.4678 0.0497 0.2864 0.073 Uiso 1 1 calc R . . C71A C -0.0636(2) 0.6098(2) 0.23700(13) 0.0179(7) Uani 1 1 d . . . C72A C -0.0494(3) 0.6021(3) 0.28609(14) 0.0242(7) Uani 1 1 d . . . H72A H 0.0101 0.6280 0.3123 0.029 Uiso 1 1 calc R . . C73A C -0.1242(3) 0.5556(3) 0.29625(15) 0.0280(8) Uani 1 1 d . . . H73A H -0.1126 0.5496 0.3295 0.034 Uiso 1 1 calc R . . C74A C -0.2151(3) 0.5181(3) 0.25858(15) 0.0220(7) Uani 1 1 d . . . C75A C -0.2299(3) 0.5288(3) 0.20904(16) 0.0331(9) Uani 1 1 d . . . H75A H -0.2906 0.5052 0.1828 0.040 Uiso 1 1 calc R . . C76A C -0.1557(3) 0.5739(3) 0.19861(14) 0.0272(8) Uani 1 1 d . . . H76A H -0.1674 0.5805 0.1654 0.033 Uiso 1 1 calc R . . C77A C -0.2910(3) 0.4639(3) 0.27066(18) 0.0336(9) Uani 1 1 d . . . H77D H -0.3587 0.4701 0.2430 0.050 Uiso 1 1 calc R . . H77E H -0.2909 0.4927 0.3003 0.050 Uiso 1 1 calc R . . H77F H -0.2724 0.3939 0.2765 0.050 Uiso 1 1 calc R . . C81A C 0.0409(3) 1.0621(3) 0.13972(14) 0.0203(7) Uani 1 1 d . . . C82A C 0.0223(3) 1.1154(3) 0.17477(15) 0.0272(8) Uani 1 1 d . . . H82A H 0.0219 1.0815 0.2020 0.033 Uiso 1 1 calc R . . C83A C 0.0041(3) 1.2189(3) 0.16992(15) 0.0304(8) Uani 1 1 d . . . H83A H -0.0078 1.2534 0.1940 0.037 Uiso 1 1 calc R . . C84A C 0.0035(3) 1.2716(3) 0.12903(15) 0.0271(8) Uani 1 1 d . . . C85A C 0.0217(3) 1.2177(3) 0.09440(16) 0.0320(9) Uani 1 1 d . . . H85A H 0.0210 1.2512 0.0668 0.038 Uiso 1 1 calc R . . C86A C 0.0410(3) 1.1158(3) 0.09923(15) 0.0294(8) Uani 1 1 d . . . H86A H 0.0542 1.0821 0.0753 0.035 Uiso 1 1 calc R . . C87A C -0.0144(4) 1.3843(3) 0.12472(17) 0.0390(10) Uani 1 1 d . . . H87D H -0.0510 1.4027 0.0899 0.058 Uiso 1 1 calc R . . H87E H 0.0508 1.4187 0.1398 0.058 Uiso 1 1 calc R . . H87F H -0.0546 1.4031 0.1417 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.66566(15) 0.82546(17) 0.47470(9) 0.1020(7) Uani 1 1 d D . . Cl2 Cl 0.83252(18) 0.91994(16) 0.46004(9) 0.1067(7) Uani 1 1 d D . . C1S C 0.7938(4) 0.8463(6) 0.4995(2) 0.094(2) Uani 1 1 d D . . H3S H 0.8291 0.7818 0.5061 0.113 Uiso 1 1 calc R . . H4S H 0.8160 0.8808 0.5314 0.113 Uiso 1 1 calc R . . Cl7 Cl 0.5534(2) 1.2430(3) 0.17040(12) 0.0779(12) Uani 0.524(5) 1 d PD . . Cl8 Cl 0.7047(2) 1.2503(2) 0.13066(12) 0.0712(11) Uani 0.524(5) 1 d PD . . C4S C 0.5716(5) 1.2395(10) 0.1184(2) 0.065(3) Uiso 0.524(5) 1 d PD . . H4S1 H 0.5327 1.2941 0.0962 0.078 Uiso 0.524(5) 1 calc PR . . H4S2 H 0.5441 1.1765 0.1009 0.078 Uiso 0.524(5) 1 calc PR . . Cl3 Cl 0.8194(4) 1.1419(3) 0.35337(15) 0.0684(15) Uani 0.429(6) 1 d PD . . Cl4 Cl 0.8239(5) 1.3255(3) 0.4084(2) 0.105(2) Uani 0.429(6) 1 d PD . . C2S C 0.8309(12) 1.1900(5) 0.4080(3) 0.080(5) Uani 0.429(6) 1 d PD . . H2S1 H 0.8966 1.1688 0.4349 0.096 Uiso 0.429(6) 1 calc PR . . H2S2 H 0.7766 1.1623 0.4149 0.096 Uiso 0.429(6) 1 calc PR . . Cl5 Cl 0.8216(9) 1.1975(9) 0.3655(4) 0.131(5) Uani 0.273(7) 1 d PD . . Cl6 Cl 0.7263(6) 1.3553(7) 0.3991(3) 0.111(4) Uani 0.273(7) 1 d PD . . C3S C 0.8381(11) 1.3110(15) 0.3935(12) 0.072(9) Uiso 0.273(7) 1 d PD . . H3S1 H 0.8559 1.3599 0.3745 0.086 Uiso 0.273(7) 1 calc PR . . H3S2 H 0.8958 1.3068 0.4268 0.086 Uiso 0.273(7) 1 calc PR . . Cl9 Cl 0.6265(9) 1.1172(9) 0.1991(5) 0.196(6) Uani 0.355(7) 1 d PD . . Cl10 Cl 0.5580(11) 1.2970(7) 0.1380(5) 0.199(6) Uani 0.355(7) 1 d PD . . C5S C 0.5336(12) 1.1689(13) 0.1595(7) 0.066(5) Uiso 0.355(7) 1 d PD . . H5S1 H 0.5266 1.1563 0.1260 0.079 Uiso 0.355(7) 1 calc PR . . H5S2 H 0.4705 1.1493 0.1610 0.079 Uiso 0.355(7) 1 calc PR . . 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 S1 0.0281(4) 0.0234(4) 0.0240(5) 0.0027(4) 0.0103(3) -0.0085(3) P1 0.0201(4) 0.0165(4) 0.0207(4) 0.0017(4) 0.0098(3) -0.0010(3) N2 0.0256(15) 0.0281(17) 0.0240(16) 0.0029(13) 0.0102(12) -0.0022(12) N22 0.0185(12) 0.0175(14) 0.0225(15) 0.0029(11) 0.0106(11) 0.0025(10) N23 0.0196(12) 0.0169(14) 0.0198(14) 0.0037(11) 0.0120(11) 0.0001(10) N24 0.0185(12) 0.0211(15) 0.0149(13) 0.0028(11) 0.0094(10) -0.0016(10) C1 0.0204(15) 0.0217(17) 0.0192(17) 0.0034(14) 0.0114(13) -0.0028(12) C3 0.0199(14) 0.0162(16) 0.0178(16) 0.0024(13) 0.0086(12) -0.0028(12) C4 0.0255(16) 0.0127(16) 0.0215(17) 0.0046(13) 0.0123(13) -0.0015(12) C5 0.0210(15) 0.0185(16) 0.0174(16) 0.0000(13) 0.0099(12) -0.0008(12) C6 0.0192(14) 0.0124(15) 0.0230(17) 0.0008(13) 0.0097(12) 0.0019(11) C7 0.0235(16) 0.0196(18) 0.030(2) 0.0033(15) 0.0148(14) 0.0019(13) C8 0.0192(15) 0.0247(18) 0.0269(19) 0.0017(15) 0.0125(13) -0.0001(13) C9 0.0171(14) 0.0196(16) 0.0195(17) -0.0004(13) 0.0102(12) -0.0023(12) C10 0.0162(13) 0.0181(16) 0.0185(17) 0.0006(13) 0.0079(12) -0.0013(12) C11 0.0146(13) 0.0199(17) 0.0224(17) -0.0019(13) 0.0109(12) 0.0000(12) C12 0.0186(14) 0.0239(18) 0.0208(18) 0.0038(14) 0.0117(13) 0.0016(12) C13 0.0221(15) 0.0202(18) 0.0168(16) 0.0024(13) 0.0110(12) 0.0006(12) C14 0.0168(13) 0.0133(16) 0.0204(17) 0.0012(13) 0.0082(12) -0.0022(11) C15 0.0202(14) 0.0134(16) 0.0162(16) -0.0004(12) 0.0088(12) -0.0021(11) C16 0.0176(14) 0.0166(16) 0.0236(18) -0.0035(13) 0.0111(13) -0.0011(12) C17 0.0255(16) 0.0210(17) 0.0227(18) -0.0002(14) 0.0144(14) 0.0010(13) C18 0.0215(15) 0.0195(17) 0.0251(18) -0.0026(14) 0.0134(14) 0.0001(12) C19 0.0194(14) 0.0192(17) 0.0186(16) 0.0010(13) 0.0101(12) -0.0001(12) C20 0.0218(15) 0.0145(15) 0.0178(16) -0.0018(13) 0.0106(13) -0.0027(12) C21 0.0236(15) 0.0130(15) 0.0177(16) 0.0036(13) 0.0121(13) -0.0003(12) C22 0.0225(15) 0.0199(17) 0.0206(17) 0.0002(14) 0.0123(13) 0.0009(12) C23 0.0249(16) 0.0204(18) 0.0234(18) 0.0008(14) 0.0135(14) 0.0001(13) C24 0.0369(19) 0.0216(18) 0.0226(18) 0.0031(14) 0.0184(15) 0.0057(14) C25 0.0268(18) 0.037(2) 0.030(2) 0.0058(17) 0.0145(15) 0.0131(15) C26 0.0214(17) 0.045(2) 0.038(2) 0.0077(19) 0.0162(16) 0.0058(16) C27 0.0237(16) 0.034(2) 0.0240(19) 0.0031(16) 0.0144(14) 0.0007(14) C28 0.0197(15) 0.0244(18) 0.0184(17) -0.0032(14) 0.0097(13) 0.0018(13) C29 0.0305(18) 0.0192(18) 0.0272(19) -0.0039(15) 0.0153(15) 0.0019(14) C30 0.034(2) 0.041(2) 0.029(2) 0.0038(18) 0.0196(17) 0.0086(17) C31 0.034(2) 0.038(2) 0.026(2) -0.0112(17) 0.0113(16) 0.0059(17) C32 0.041(2) 0.021(2) 0.040(2) -0.0078(17) 0.0168(19) 0.0069(16) C33 0.0344(19) 0.0209(18) 0.029(2) -0.0020(16) 0.0125(16) 0.0000(15) C51 0.0218(15) 0.0201(17) 0.0246(18) 0.0007(14) 0.0131(14) 0.0005(12) C52 0.0308(18) 0.0223(18) 0.0239(19) 0.0017(15) 0.0140(15) -0.0013(14) C53 0.0346(19) 0.0227(19) 0.0239(19) 0.0040(15) 0.0129(16) -0.0017(14) C54 0.0323(19) 0.0182(18) 0.032(2) -0.0016(15) 0.0093(16) -0.0014(14) C55 0.0328(19) 0.0223(18) 0.029(2) 0.0018(15) 0.0167(16) 0.0033(14) C56 0.0296(18) 0.0196(18) 0.0265(19) 0.0027(14) 0.0147(15) 0.0018(14) C57 0.057(3) 0.022(2) 0.042(3) 0.0026(18) 0.023(2) 0.0074(18) C61 0.0179(14) 0.0200(17) 0.0205(17) 0.0057(14) 0.0094(12) 0.0034(12) C62 0.0195(15) 0.0230(18) 0.0229(18) 0.0028(14) 0.0111(13) 0.0020(13) C63 0.0199(15) 0.033(2) 0.0248(19) 0.0049(15) 0.0122(14) 0.0057(14) C64 0.0237(17) 0.035(2) 0.038(2) 0.0190(18) 0.0193(16) 0.0077(15) C65 0.0305(18) 0.0173(18) 0.048(2) 0.0057(17) 0.0208(18) -0.0003(14) C66 0.0245(16) 0.0155(17) 0.041(2) 0.0008(15) 0.0192(16) -0.0013(13) C67 0.0255(19) 0.053(3) 0.047(3) 0.016(2) 0.0240(19) 0.0054(18) C71 0.0214(15) 0.0154(16) 0.0193(17) 0.0002(13) 0.0119(13) 0.0020(12) C72 0.0205(15) 0.0217(17) 0.0264(19) 0.0008(14) 0.0130(14) -0.0008(13) C73 0.0300(18) 0.0169(18) 0.035(2) 0.0020(15) 0.0156(16) -0.0062(14) C74 0.0279(17) 0.0261(19) 0.0260(19) 0.0069(15) 0.0172(15) 0.0038(14) C75 0.0218(16) 0.029(2) 0.028(2) 0.0013(16) 0.0131(14) 0.0049(14) C76 0.0192(15) 0.0208(17) 0.0250(18) 0.0005(14) 0.0106(13) -0.0048(12) C77 0.041(2) 0.023(2) 0.050(3) 0.0014(19) 0.028(2) 0.0062(17) C81 0.0193(14) 0.0182(17) 0.0197(17) -0.0004(13) 0.0106(12) -0.0011(12) C82 0.0210(15) 0.0214(17) 0.0199(17) 0.0019(14) 0.0094(13) -0.0017(12) C83 0.0205(15) 0.034(2) 0.0234(19) 0.0023(16) 0.0112(13) 0.0001(14) C84 0.0208(15) 0.035(2) 0.0255(19) 0.0000(16) 0.0118(13) -0.0051(15) C85 0.0295(17) 0.030(2) 0.0220(19) 0.0084(15) 0.0119(14) -0.0013(15) C86 0.0194(15) 0.0224(18) 0.0243(18) 0.0002(14) 0.0111(13) -0.0002(13) C87 0.0252(18) 0.076(3) 0.032(2) 0.015(2) 0.0172(17) -0.0014(19) S2 0.0341(5) 0.0174(4) 0.0248(5) -0.0011(4) 0.0059(4) -0.0016(4) P2 0.0218(4) 0.0188(4) 0.0179(4) -0.0013(3) 0.0080(3) -0.0013(3) N2A 0.0253(14) 0.0232(16) 0.0229(16) 0.0034(12) 0.0101(12) -0.0008(12) N22A 0.0191(12) 0.0201(14) 0.0178(14) 0.0002(11) 0.0101(11) -0.0010(10) N23A 0.0177(12) 0.0219(15) 0.0206(15) 0.0015(12) 0.0094(11) -0.0005(11) N24A 0.0180(12) 0.0199(14) 0.0191(14) 0.0020(12) 0.0100(11) 0.0005(10) C1A 0.0224(15) 0.0164(16) 0.0164(16) 0.0040(13) 0.0087(12) 0.0003(12) C3A 0.0222(15) 0.0203(17) 0.0221(18) -0.0001(14) 0.0139(13) -0.0034(12) C4A 0.0184(14) 0.0227(18) 0.0166(16) 0.0037(13) 0.0079(12) 0.0011(12) C5A 0.0206(15) 0.0222(17) 0.0187(17) 0.0013(14) 0.0107(12) -0.0018(13) C6A 0.0161(14) 0.0248(18) 0.0214(17) -0.0020(14) 0.0100(12) -0.0008(12) C7A 0.0273(17) 0.0260(19) 0.026(2) 0.0017(15) 0.0153(15) 0.0028(14) C8A 0.0228(16) 0.0233(18) 0.0253(19) 0.0010(15) 0.0111(14) 0.0044(13) C9A 0.0158(14) 0.0206(17) 0.0176(17) -0.0013(14) 0.0054(12) -0.0002(12) C10A 0.0156(14) 0.0178(17) 0.0200(17) 0.0005(13) 0.0075(12) -0.0016(11) C11A 0.0162(14) 0.0239(18) 0.0200(17) -0.0001(14) 0.0076(12) -0.0040(12) C12A 0.0226(15) 0.0202(18) 0.0234(18) 0.0032(14) 0.0097(13) -0.0013(13) C13A 0.0185(14) 0.0245(18) 0.0229(18) 0.0052(14) 0.0103(13) -0.0015(12) C14A 0.0182(14) 0.0185(17) 0.0189(17) -0.0011(13) 0.0092(12) -0.0039(12) C15A 0.0167(14) 0.0212(17) 0.0167(16) -0.0029(13) 0.0093(12) -0.0036(12) C16A 0.0184(14) 0.0219(17) 0.0179(16) 0.0008(13) 0.0111(12) 0.0005(12) C17A 0.0185(15) 0.0275(19) 0.029(2) 0.0016(15) 0.0145(14) 0.0014(13) C18A 0.0227(16) 0.0206(17) 0.0258(19) -0.0016(14) 0.0125(14) 0.0032(13) C19A 0.0210(15) 0.0182(17) 0.0186(16) -0.0030(13) 0.0108(12) -0.0014(12) C20A 0.0214(15) 0.0194(17) 0.0154(16) -0.0028(13) 0.0082(12) -0.0023(12) C21A 0.0170(14) 0.0175(16) 0.0189(16) -0.0010(13) 0.0096(12) -0.0022(11) C22A 0.0258(16) 0.0267(19) 0.0227(19) 0.0036(15) 0.0114(14) 0.0092(14) C23A 0.0243(16) 0.028(2) 0.0238(19) 0.0000(15) 0.0118(14) -0.0031(14) C24A 0.033(2) 0.036(2) 0.032(2) 0.0145(18) 0.0181(17) 0.0066(17) C25A 0.071(3) 0.054(3) 0.040(3) 0.025(2) 0.039(2) 0.033(2) C26A 0.124(5) 0.038(3) 0.032(3) 0.006(2) 0.043(3) 0.040(3) C27A 0.085(4) 0.027(2) 0.028(2) 0.0039(18) 0.027(2) 0.022(2) C28A 0.0218(15) 0.033(2) 0.0206(18) -0.0038(15) 0.0098(13) -0.0042(14) C29A 0.0262(19) 0.054(3) 0.032(2) -0.0006(19) 0.0134(17) -0.0037(17) C30A 0.026(2) 0.067(3) 0.043(3) 0.004(2) 0.0107(18) 0.008(2) C31A 0.028(2) 0.100(5) 0.045(3) -0.020(3) 0.017(2) -0.014(2) C32A 0.039(2) 0.060(3) 0.044(3) -0.017(2) 0.027(2) -0.017(2) C33A 0.038(2) 0.035(2) 0.030(2) -0.0121(18) 0.0179(18) -0.0141(17) C51A 0.0232(16) 0.0277(19) 0.0227(18) 0.0015(15) 0.0152(14) 0.0005(13) C52A 0.0233(16) 0.029(2) 0.027(2) 0.0031(15) 0.0150(14) 0.0001(14) C53A 0.036(2) 0.040(2) 0.024(2) 0.0066(17) 0.0173(16) 0.0002(17) C54A 0.032(2) 0.064(3) 0.041(3) 0.010(2) 0.0249(19) -0.001(2) C55A 0.0181(17) 0.073(3) 0.051(3) 0.019(2) 0.0168(18) -0.0002(19) C56A 0.0216(17) 0.046(2) 0.035(2) 0.0095(18) 0.0142(16) 0.0013(16) C57A 0.040(3) 0.115(5) 0.072(4) 0.043(4) 0.032(3) -0.005(3) C61A 0.0217(15) 0.0207(18) 0.0232(18) 0.0010(14) 0.0139(13) 0.0015(12) C62A 0.0204(15) 0.0263(19) 0.0287(19) 0.0022(15) 0.0140(14) -0.0001(13) C63A 0.0298(18) 0.0257(19) 0.029(2) 0.0056(16) 0.0129(16) 0.0110(15) C64A 0.051(2) 0.0202(19) 0.028(2) -0.0004(16) 0.0178(18) 0.0019(17) C65A 0.044(2) 0.020(2) 0.037(2) -0.0025(17) 0.0127(18) -0.0039(16) C66A 0.0290(18) 0.028(2) 0.030(2) -0.0051(16) 0.0103(16) -0.0034(15) C67A 0.065(3) 0.019(2) 0.050(3) 0.000(2) 0.015(2) 0.012(2) C71A 0.0165(14) 0.0185(16) 0.0217(17) 0.0004(13) 0.0112(12) -0.0016(12) C72A 0.0240(16) 0.0285(19) 0.0237(18) -0.0050(15) 0.0140(14) -0.0060(14) C73A 0.0314(19) 0.034(2) 0.025(2) -0.0011(16) 0.0190(16) -0.0019(15) C74A 0.0187(15) 0.0176(17) 0.036(2) 0.0057(15) 0.0178(14) 0.0042(12) C75A 0.0209(16) 0.038(2) 0.033(2) 0.0042(18) 0.0054(15) -0.0086(15) C76A 0.0203(16) 0.040(2) 0.0206(18) 0.0013(16) 0.0082(13) -0.0034(14) C77A 0.0230(17) 0.031(2) 0.055(3) 0.0101(19) 0.0246(18) 0.0039(15) C81A 0.0214(15) 0.0184(17) 0.0248(18) -0.0002(14) 0.0137(13) 0.0024(12) C82A 0.037(2) 0.0254(19) 0.024(2) 0.0041(15) 0.0179(16) 0.0040(15) C83A 0.045(2) 0.0238(19) 0.026(2) -0.0019(16) 0.0193(17) 0.0083(16) C84A 0.0291(18) 0.0177(18) 0.030(2) 0.0038(15) 0.0091(15) 0.0024(14) C85A 0.041(2) 0.034(2) 0.028(2) 0.0121(17) 0.0208(17) 0.0047(17) C86A 0.040(2) 0.030(2) 0.024(2) 0.0038(16) 0.0203(17) 0.0077(16) C87A 0.056(3) 0.023(2) 0.030(2) 0.0054(17) 0.013(2) 0.0055(18) Cl1 0.0655(10) 0.1260(17) 0.0929(14) -0.0128(12) 0.0163(9) 0.0249(10) Cl2 0.1113(15) 0.1006(15) 0.1061(16) -0.0394(12) 0.0469(13) -0.0054(12) C1S 0.060(4) 0.113(6) 0.097(6) -0.007(5) 0.023(4) -0.009(4) Cl7 0.091(2) 0.081(3) 0.068(2) 0.0054(17) 0.0420(18) 0.0061(18) Cl8 0.0551(16) 0.069(2) 0.069(2) -0.0005(14) 0.0094(13) -0.0055(12) Cl3 0.084(3) 0.082(3) 0.043(2) -0.0259(19) 0.0319(18) -0.016(2) Cl4 0.149(6) 0.061(3) 0.078(4) -0.030(2) 0.028(3) -0.001(3) C2S 0.077(10) 0.090(12) 0.074(12) 0.024(9) 0.034(9) 0.018(8) Cl5 0.125(8) 0.195(12) 0.075(7) 0.011(7) 0.047(6) 0.094(8) Cl6 0.093(6) 0.156(8) 0.073(5) -0.030(5) 0.029(4) 0.017(5) Cl9 0.181(9) 0.222(12) 0.264(14) 0.054(9) 0.169(10) 0.071(8) Cl10 0.305(15) 0.141(8) 0.262(13) 0.059(8) 0.225(13) 0.090(9) _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 S1 P1 1.9574(12) . ? P1 C21 1.797(3) . ? P1 C22 1.817(3) . ? P1 C28 1.828(3) . ? N2 C3 1.315(4) . ? N2 C4 1.412(4) . ? N22 C9 1.360(4) . ? N22 C6 1.377(4) . ? N22 H22 0.8600 . ? N23 C14 1.365(4) . ? N23 C11 1.386(4) . ? N23 H23 0.8600 . ? N24 C16 1.360(4) . ? N24 C19 1.385(4) . ? C1 C20 1.415(5) . ? C1 C3 1.420(5) . ? C1 C21 1.427(4) . ? C3 H3 0.9300 . ? C4 C5 1.423(5) . ? C4 C21 1.427(5) . ? C5 C6 1.402(4) . ? C5 C51 1.456(5) . ? C6 C7 1.421(5) . ? C7 C8 1.364(5) . ? C7 H7 0.9300 . ? C8 C9 1.426(5) . ? C8 H8 0.9300 . ? C9 C10 1.394(5) . ? C10 C11 1.413(4) . ? C10 C61 1.499(4) . ? C11 C12 1.426(5) . ? C12 C13 1.359(5) . ? C12 H12 0.9300 . ? C13 C14 1.443(4) . ? C13 H13 0.9300 . ? C14 C15 1.402(4) . ? C15 C16 1.419(5) . ? C15 C71 1.477(4) . ? C16 C17 1.455(5) . ? C17 C18 1.347(5) . ? C17 H17 0.9300 . ? C18 C19 1.444(5) . ? C18 H18 0.9300 . ? C19 C20 1.405(5) . ? C20 C81 1.481(4) . ? C22 C27 1.385(5) . ? C22 C23 1.397(5) . ? C23 C24 1.382(5) . ? C23 H1 0.9300 . ? C24 C25 1.386(5) . ? C24 H24 0.9300 . ? C25 C26 1.366(6) . ? C25 H25 0.9300 . ? C26 C27 1.412(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.390(5) . ? C28 C33 1.396(5) . ? C29 C30 1.379(5) . ? C29 H29 0.9300 . ? C30 C31 1.386(6) . ? C30 H30 0.9300 . ? C31 C32 1.382(6) . ? C31 H31 0.9300 . ? C32 C33 1.383(6) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C51 C52 1.408(5) . ? C51 C56 1.409(5) . ? C52 C53 1.378(5) . ? C52 H52 0.9300 . ? C53 C54 1.379(5) . ? C53 H53 0.9300 . ? C54 C55 1.388(5) . ? C54 C57 1.510(5) . ? C55 C56 1.376(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C61 C66 1.382(5) . ? C61 C62 1.392(5) . ? C62 C63 1.388(5) . ? C62 H62 0.9300 . ? C63 C64 1.391(6) . ? C63 H63 0.9300 . ? C64 C65 1.388(6) . ? C64 C67 1.506(5) . ? C65 C66 1.379(5) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C71 C76 1.391(4) . ? C71 C72 1.399(5) . ? C72 C73 1.367(5) . ? C72 H72 0.9300 . ? C73 C74 1.398(5) . ? C73 H73 0.9300 . ? C74 C75 1.399(5) . ? C74 C77 1.507(5) . ? C75 C76 1.380(5) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C81 C86 1.393(5) . ? C81 C82 1.399(5) . ? C82 C83 1.410(5) . ? C82 H82 0.9300 . ? C83 C84 1.371(5) . ? C83 H83 0.9300 . ? C84 C85 1.386(5) . ? C84 C87 1.512(5) . ? C85 C86 1.387(5) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? S2 P2 1.9489(13) . ? P2 C21A 1.811(3) . ? P2 C22A 1.814(4) . ? P2 C28A 1.823(4) . ? N2A C3A 1.312(4) . ? N2A C1A 1.416(4) . ? N22A C9A 1.335(4) . ? N22A C6A 1.376(4) . ? N22A H22A 0.8601 . ? N23A C14A 1.367(4) . ? N23A C11A 1.374(4) . ? N24A C16A 1.366(4) . ? N24A C19A 1.378(4) . ? N24A H24A 0.8600 . ? C1A C20A 1.412(4) . ? C1A C21A 1.437(5) . ? C3A C4A 1.409(5) . ? C3A H3A 0.9300 . ? C4A C5A 1.414(5) . ? C4A C21A 1.430(4) . ? C5A C6A 1.393(5) . ? C5A C51A 1.495(5) . ? C6A C7A 1.425(5) . ? C7A C8A 1.354(5) . ? C7A H7A 0.9300 . ? C8A C9A 1.432(5) . ? C8A H8A 0.9300 . ? C9A C10A 1.422(5) . ? C10A C11A 1.405(4) . ? C10A C61A 1.493(5) . ? C11A C12A 1.449(5) . ? C12A C13A 1.334(5) . ? C12A H12A 0.9300 . ? C13A C14A 1.450(5) . ? C13A H13A 0.9300 . ? C14A C15A 1.406(4) . ? C15A C16A 1.392(5) . ? C15A C71A 1.495(4) . ? C16A C17A 1.433(5) . ? C17A C18A 1.352(5) . ? C17A H17A 0.9300 . ? C18A C19A 1.419(4) . ? C18A H18A 0.9300 . ? C19A C20A 1.395(5) . ? C20A C81A 1.489(5) . ? C22A C27A 1.382(6) . ? C22A C23A 1.407(5) . ? C23A C24A 1.381(5) . ? C23A H23A 0.9300 . ? C24A C25A 1.368(7) . ? C24A H2 0.9300 . ? C25A C26A 1.353(7) . ? C25A H25A 0.9300 . ? C26A C27A 1.378(6) . ? C26A H26A 0.9300 . ? C27A H27A 0.9300 . ? C28A C33A 1.379(5) . ? C28A C29A 1.395(6) . ? C29A C30A 1.349(6) . ? C29A H29A 0.9300 . ? C30A C31A 1.414(7) . ? C30A H30A 0.9300 . ? C31A C32A 1.364(8) . ? C31A H31A 0.9300 . ? C32A C33A 1.390(6) . ? C32A H32A 0.9300 . ? C33A H33A 0.9300 . ? C51A C56A 1.383(5) . ? C51A C52A 1.407(5) . ? C52A C53A 1.372(5) . ? C52A H52A 0.9300 . ? C53A C54A 1.394(6) . ? C53A H53A 0.9300 . ? C54A C55A 1.381(6) . ? C54A C57A 1.501(6) . ? C55A C56A 1.406(5) . ? C55A H55A 0.9300 . ? C56A H56A 0.9300 . ? C57A H57D 0.9600 . ? C57A H57E 0.9600 . ? C57A H57F 0.9600 . ? C61A C66A 1.378(5) . ? C61A C62A 1.400(5) . ? C62A C63A 1.377(5) . ? C62A H62A 0.9300 . ? C63A C64A 1.383(6) . ? C63A H63A 0.9300 . ? C64A C65A 1.379(6) . ? C64A C67A 1.525(5) . ? C65A C66A 1.378(6) . ? C65A H65A 0.9300 . ? C66A H66A 0.9300 . ? C67A H67D 0.9600 . ? C67A H67E 0.9600 . ? C67A H67F 0.9600 . ? C71A C72A 1.386(5) . ? C71A C76A 1.394(5) . ? C72A C73A 1.391(5) . ? C72A H72A 0.9300 . ? C73A C74A 1.383(5) . ? C73A H73A 0.9300 . ? C74A C75A 1.399(6) . ? C74A C77A 1.486(5) . ? C75A C76A 1.381(5) . ? C75A H75A 0.9300 . ? C76A H76A 0.9300 . ? C77A H77D 0.9600 . ? C77A H77E 0.9600 . ? C77A H77F 0.9600 . ? C81A C82A 1.383(5) . ? C81A C86A 1.400(5) . ? C82A C83A 1.392(5) . ? C82A H82A 0.9300 . ? C83A C84A 1.400(5) . ? C83A H83A 0.9300 . ? C84A C85A 1.374(6) . ? C84A C87A 1.512(5) . ? C85A C86A 1.372(5) . ? C85A H85A 0.9300 . ? C86A H86A 0.9300 . ? C87A H87D 0.9600 . ? C87A H87E 0.9600 . ? C87A H87F 0.9600 . ? Cl1 C1S 1.684(6) . ? Cl2 C1S 1.799(6) . ? C1S H3S 0.9700 . ? C1S H4S 0.9700 . ? Cl7 C5S 1.034(17) . ? Cl7 Cl10 1.227(9) . ? Cl7 C4S 1.684(6) . ? Cl7 Cl9 1.953(11) . ? Cl8 C4S 1.799(6) . ? Cl8 Cl10 2.315(10) . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? Cl3 Cl5 0.815(10) . ? Cl3 C2S 1.684(6) . ? Cl4 Cl6 1.370(9) . ? Cl4 C2S 1.799(6) . ? Cl4 Cl5 2.117(10) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? Cl5 C3S 1.684(6) . ? Cl6 C3S 1.799(6) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? Cl9 C5S 1.498(15) . ? Cl10 C5S 1.903(15) . ? C5S H5S1 0.9700 . ? C5S H5S2 0.9700 . ? 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 C21 P1 C22 103.89(15) . . ? C21 P1 C28 107.32(15) . . ? C22 P1 C28 102.41(16) . . ? C21 P1 S1 121.01(11) . . ? C22 P1 S1 110.55(12) . . ? C28 P1 S1 109.96(12) . . ? C3 N2 C4 108.0(3) . . ? C9 N22 C6 111.8(3) . . ? C9 N22 H22 124.1 . . ? C6 N22 H22 124.1 . . ? C14 N23 C11 109.0(3) . . ? C14 N23 H23 125.5 . . ? C11 N23 H23 125.5 . . ? C16 N24 C19 106.1(3) . . ? C20 C1 C3 121.3(3) . . ? C20 C1 C21 130.7(3) . . ? C3 C1 C21 107.1(3) . . ? N2 C3 C1 110.9(3) . . ? N2 C3 H3 124.6 . . ? C1 C3 H3 124.6 . . ? N2 C4 C5 121.2(3) . . ? N2 C4 C21 109.2(3) . . ? C5 C4 C21 129.6(3) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 C51 119.2(3) . . ? C4 C5 C51 121.2(3) . . ? N22 C6 C5 124.7(3) . . ? N22 C6 C7 105.7(3) . . ? C5 C6 C7 129.5(3) . . ? C8 C7 C6 108.1(3) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? C7 C8 C9 108.9(3) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? N22 C9 C10 126.8(3) . . ? N22 C9 C8 105.5(3) . . ? C10 C9 C8 127.7(3) . . ? C9 C10 C11 125.8(3) . . ? C9 C10 C61 117.3(3) . . ? C11 C10 C61 116.8(3) . . ? N23 C11 C10 126.6(3) . . ? N23 C11 C12 107.3(3) . . ? C10 C11 C12 126.0(3) . . ? C13 C12 C11 108.4(3) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? C12 C13 C14 107.3(3) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? N23 C14 C15 125.5(3) . . ? N23 C14 C13 107.8(3) . . ? C15 C14 C13 126.6(3) . . ? C14 C15 C16 124.3(3) . . ? C14 C15 C71 120.0(3) . . ? C16 C15 C71 115.6(3) . . ? N24 C16 C15 125.5(3) . . ? N24 C16 C17 110.3(3) . . ? C15 C16 C17 124.2(3) . . ? C18 C17 C16 106.6(3) . . ? C18 C17 H17 126.7 . . ? C16 C17 H17 126.7 . . ? C17 C18 C19 107.3(3) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N24 C19 C20 123.9(3) . . ? N24 C19 C18 109.6(3) . . ? C20 C19 C18 125.7(3) . . ? C19 C20 C1 121.0(3) . . ? C19 C20 C81 119.2(3) . . ? C1 C20 C81 119.4(3) . . ? C1 C21 C4 104.6(3) . . ? C1 C21 P1 123.6(3) . . ? C4 C21 P1 125.9(2) . . ? C27 C22 C23 118.7(3) . . ? C27 C22 P1 119.0(3) . . ? C23 C22 P1 122.2(2) . . ? C24 C23 C22 121.1(3) . . ? C24 C23 H1 119.4 . . ? C22 C23 H1 119.4 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 119.7(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.9(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 119.6(4) . . ? C22 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C33 118.3(3) . . ? C29 C28 P1 122.7(3) . . ? C33 C28 P1 118.7(3) . . ? C30 C29 C28 121.5(3) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.7(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 119.6(4) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C28 120.2(4) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C52 C51 C56 117.1(3) . . ? C52 C51 C5 121.2(3) . . ? C56 C51 C5 121.7(3) . . ? C53 C52 C51 120.8(3) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 122.0(4) . . ? C52 C53 H53 119.0 . . ? C54 C53 H53 119.0 . . ? C53 C54 C55 117.3(3) . . ? C53 C54 C57 121.3(4) . . ? C55 C54 C57 121.4(4) . . ? C56 C55 C54 122.3(3) . . ? C56 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C55 C56 C51 120.4(3) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C66 C61 C62 117.7(3) . . ? C66 C61 C10 121.1(3) . . ? C62 C61 C10 121.1(3) . . ? C63 C62 C61 120.7(3) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C62 C63 C64 121.3(3) . . ? C62 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? C65 C64 C63 117.4(3) . . ? C65 C64 C67 121.1(4) . . ? C63 C64 C67 121.5(4) . . ? C66 C65 C64 121.1(4) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C65 C66 C61 121.6(4) . . ? C65 C66 H66 119.2 . . ? C61 C66 H66 119.2 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C76 C71 C72 117.4(3) . . ? C76 C71 C15 119.7(3) . . ? C72 C71 C15 122.7(3) . . ? C73 C72 C71 120.9(3) . . ? C73 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? C72 C73 C74 122.3(3) . . ? C72 C73 H73 118.8 . . ? C74 C73 H73 118.8 . . ? C73 C74 C75 116.5(3) . . ? C73 C74 C77 122.4(3) . . ? C75 C74 C77 121.1(3) . . ? C76 C75 C74 121.3(3) . . ? C76 C75 H75 119.3 . . ? C74 C75 H75 119.3 . . ? C75 C76 C71 121.4(3) . . ? C75 C76 H76 119.3 . . ? C71 C76 H76 119.3 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C86 C81 C82 118.4(3) . . ? C86 C81 C20 120.0(3) . . ? C82 C81 C20 121.6(3) . . ? C81 C82 C83 120.1(3) . . ? C81 C82 H82 119.9 . . ? C83 C82 H82 119.9 . . ? C84 C83 C82 120.6(3) . . ? C84 C83 H83 119.7 . . ? C82 C83 H83 119.7 . . ? C83 C84 C85 119.2(3) . . ? C83 C84 C87 121.8(3) . . ? C85 C84 C87 119.0(3) . . ? C84 C85 C86 121.0(3) . . ? C84 C85 H85 119.5 . . ? C86 C85 H85 119.5 . . ? C85 C86 C81 120.6(3) . . ? C85 C86 H86 119.7 . . ? C81 C86 H86 119.7 . . ? C84 C87 H87A 109.5 . . ? C84 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C84 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C21A P2 C22A 102.46(17) . . ? C21A P2 C28A 110.66(16) . . ? C22A P2 C28A 102.95(17) . . ? C21A P2 S2 118.87(12) . . ? C22A P2 S2 110.74(13) . . ? C28A P2 S2 109.80(13) . . ? C3A N2A C1A 106.1(3) . . ? C9A N22A C6A 111.1(3) . . ? C9A N22A H22A 124.5 . . ? C6A N22A H22A 124.5 . . ? C14A N23A C11A 104.8(3) . . ? C16A N24A C19A 111.1(3) . . ? C16A N24A H24A 124.4 . . ? C19A N24A H24A 124.5 . . ? C20A C1A N2A 117.1(3) . . ? C20A C1A C21A 132.3(3) . . ? N2A C1A C21A 110.1(3) . . ? N2A C3A C4A 113.1(3) . . ? N2A C3A H3A 123.4 . . ? C4A C3A H3A 123.4 . . ? C3A C4A C5A 122.5(3) . . ? C3A C4A C21A 106.6(3) . . ? C5A C4A C21A 130.6(3) . . ? C6A C5A C4A 122.6(3) . . ? C6A C5A C51A 120.9(3) . . ? C4A C5A C51A 116.2(3) . . ? N22A C6A C5A 124.6(3) . . ? N22A C6A C7A 105.9(3) . . ? C5A C6A C7A 129.5(3) . . ? C8A C7A C6A 108.1(3) . . ? C8A C7A H7A 125.9 . . ? C6A C7A H7A 125.9 . . ? C7A C8A C9A 107.8(3) . . ? C7A C8A H8A 126.1 . . ? C9A C8A H8A 126.1 . . ? N22A C9A C10A 126.0(3) . . ? N22A C9A C8A 107.0(3) . . ? C10A C9A C8A 126.9(3) . . ? C11A C10A C9A 125.6(3) . . ? C11A C10A C61A 118.8(3) . . ? C9A C10A C61A 115.6(3) . . ? N23A C11A C10A 126.7(3) . . ? N23A C11A C12A 110.6(3) . . ? C10A C11A C12A 122.5(3) . . ? C13A C12A C11A 106.9(3) . . ? C13A C12A H12A 126.6 . . ? C11A C12A H12A 126.6 . . ? C12A C13A C14A 106.8(3) . . ? C12A C13A H13A 126.6 . . ? C14A C13A H13A 126.6 . . ? N23A C14A C15A 126.4(3) . . ? N23A C14A C13A 110.9(3) . . ? C15A C14A C13A 122.6(3) . . ? C16A C15A C14A 125.7(3) . . ? C16A C15A C71A 117.0(3) . . ? C14A C15A C71A 117.3(3) . . ? N24A C16A C15A 126.7(3) . . ? N24A C16A C17A 106.1(3) . . ? C15A C16A C17A 127.2(3) . . ? C18A C17A C16A 107.9(3) . . ? C18A C17A H17A 126.1 . . ? C16A C17A H17A 126.1 . . ? C17A C18A C19A 109.4(3) . . ? C17A C18A H18A 125.3 . . ? C19A C18A H18A 125.3 . . ? N24A C19A C20A 124.8(3) . . ? N24A C19A C18A 105.5(3) . . ? C20A C19A C18A 129.7(3) . . ? C19A C20A C1A 121.0(3) . . ? C19A C20A C81A 120.5(3) . . ? C1A C20A C81A 118.1(3) . . ? C4A C21A C1A 104.0(3) . . ? C4A C21A P2 119.4(2) . . ? C1A C21A P2 124.6(2) . . ? C27A C22A C23A 117.5(4) . . ? C27A C22A P2 120.5(3) . . ? C23A C22A P2 122.0(3) . . ? C24A C23A C22A 120.4(4) . . ? C24A C23A H23A 119.8 . . ? C22A C23A H23A 119.8 . . ? C25A C24A C23A 120.5(4) . . ? C25A C24A H2 119.7 . . ? C23A C24A H2 119.7 . . ? C26A C25A C24A 119.6(4) . . ? C26A C25A H25A 120.2 . . ? C24A C25A H25A 120.2 . . ? C25A C26A C27A 121.3(4) . . ? C25A C26A H26A 119.4 . . ? C27A C26A H26A 119.4 . . ? C26A C27A C22A 120.7(4) . . ? C26A C27A H27A 119.6 . . ? C22A C27A H27A 119.6 . . ? C33A C28A C29A 118.0(4) . . ? C33A C28A P2 119.0(3) . . ? C29A C28A P2 122.7(3) . . ? C30A C29A C28A 122.2(4) . . ? C30A C29A H29A 118.9 . . ? C28A C29A H29A 118.9 . . ? C29A C30A C31A 119.0(5) . . ? C29A C30A H30A 120.5 . . ? C31A C30A H30A 120.5 . . ? C32A C31A C30A 120.0(4) . . ? C32A C31A H31A 120.0 . . ? C30A C31A H31A 120.0 . . ? C31A C32A C33A 119.7(4) . . ? C31A C32A H32A 120.1 . . ? C33A C32A H32A 120.1 . . ? C28A C33A C32A 121.0(4) . . ? C28A C33A H33A 119.5 . . ? C32A C33A H33A 119.5 . . ? C56A C51A C52A 118.6(3) . . ? C56A C51A C5A 123.6(3) . . ? C52A C51A C5A 117.8(3) . . ? C53A C52A C51A 120.9(3) . . ? C53A C52A H52A 119.5 . . ? C51A C52A H52A 119.5 . . ? C52A C53A C54A 121.6(4) . . ? C52A C53A H53A 119.2 . . ? C54A C53A H53A 119.2 . . ? C55A C54A C53A 117.0(4) . . ? C55A C54A C57A 121.5(4) . . ? C53A C54A C57A 121.4(4) . . ? C54A C55A C56A 122.7(4) . . ? C54A C55A H55A 118.7 . . ? C56A C55A H55A 118.7 . . ? C51A C56A C55A 119.2(4) . . ? C51A C56A H56A 120.4 . . ? C55A C56A H56A 120.4 . . ? C54A C57A H57D 109.5 . . ? C54A C57A H57E 109.5 . . ? H57D C57A H57E 109.5 . . ? C54A C57A H57F 109.5 . . ? H57D C57A H57F 109.5 . . ? H57E C57A H57F 109.5 . . ? C66A C61A C62A 118.2(3) . . ? C66A C61A C10A 122.1(3) . . ? C62A C61A C10A 119.7(3) . . ? C63A C62A C61A 120.1(3) . . ? C63A C62A H62A 119.9 . . ? C61A C62A H62A 119.9 . . ? C62A C63A C64A 121.2(4) . . ? C62A C63A H63A 119.4 . . ? C64A C63A H63A 119.4 . . ? C65A C64A C63A 118.7(4) . . ? C65A C64A C67A 120.5(4) . . ? C63A C64A C67A 120.8(4) . . ? C66A C65A C64A 120.4(4) . . ? C66A C65A H65A 119.8 . . ? C64A C65A H65A 119.8 . . ? C65A C66A C61A 121.4(4) . . ? C65A C66A H66A 119.3 . . ? C61A C66A H66A 119.3 . . ? C64A C67A H67D 109.5 . . ? C64A C67A H67E 109.5 . . ? H67D C67A H67E 109.5 . . ? C64A C67A H67F 109.5 . . ? H67D C67A H67F 109.5 . . ? H67E C67A H67F 109.5 . . ? C72A C71A C76A 118.3(3) . . ? C72A C71A C15A 122.0(3) . . ? C76A C71A C15A 119.6(3) . . ? C71A C72A C73A 120.0(3) . . ? C71A C72A H72A 120.0 . . ? C73A C72A H72A 120.0 . . ? C74A C73A C72A 122.2(3) . . ? C74A C73A H73A 118.9 . . ? C72A C73A H73A 118.9 . . ? C73A C74A C75A 117.2(3) . . ? C73A C74A C77A 121.1(3) . . ? C75A C74A C77A 121.6(3) . . ? C76A C75A C74A 121.0(3) . . ? C76A C75A H75A 119.5 . . ? C74A C75A H75A 119.5 . . ? C75A C76A C71A 121.2(3) . . ? C75A C76A H76A 119.4 . . ? C71A C76A H76A 119.4 . . ? C74A C77A H77D 109.5 . . ? C74A C77A H77E 109.5 . . ? H77D C77A H77E 109.5 . . ? C74A C77A H77F 109.5 . . ? H77D C77A H77F 109.5 . . ? H77E C77A H77F 109.5 . . ? C82A C81A C86A 117.8(3) . . ? C82A C81A C20A 122.2(3) . . ? C86A C81A C20A 119.6(3) . . ? C81A C82A C83A 121.1(3) . . ? C81A C82A H82A 119.5 . . ? C83A C82A H82A 119.5 . . ? C82A C83A C84A 120.6(3) . . ? C82A C83A H83A 119.7 . . ? C84A C83A H83A 119.7 . . ? C85A C84A C83A 117.7(3) . . ? C85A C84A C87A 122.3(4) . . ? C83A C84A C87A 120.0(4) . . ? C86A C85A C84A 122.1(4) . . ? C86A C85A H85A 119.0 . . ? C84A C85A H85A 119.0 . . ? C85A C86A C81A 120.7(3) . . ? C85A C86A H86A 119.6 . . ? C81A C86A H86A 119.6 . . ? C84A C87A H87D 109.5 . . ? C84A C87A H87E 109.5 . . ? H87D C87A H87E 109.5 . . ? C84A C87A H87F 109.5 . . ? H87D C87A H87F 109.5 . . ? H87E C87A H87F 109.5 . . ? Cl1 C1S Cl2 114.1(3) . . ? Cl1 C1S H3S 108.7 . . ? Cl2 C1S H3S 108.7 . . ? Cl1 C1S H4S 108.7 . . ? Cl2 C1S H4S 108.7 . . ? H3S C1S H4S 107.6 . . ? C5S Cl7 Cl10 114.3(12) . . ? C5S Cl7 C4S 79.7(11) . . ? C5S Cl7 Cl9 49.2(9) . . ? Cl10 Cl7 Cl9 129.2(5) . . ? C4S Cl7 Cl9 95.8(5) . . ? Cl7 C4S Cl8 114.0(4) . . ? Cl7 C4S H4S1 108.8 . . ? Cl8 C4S H4S1 108.8 . . ? Cl7 C4S H4S2 108.8 . . ? Cl8 C4S H4S2 108.8 . . ? H4S1 C4S H4S2 107.7 . . ? Cl6 Cl4 C2S 110.1(7) . . ? Cl6 Cl4 Cl5 112.0(5) . . ? Cl3 C2S Cl4 113.9(4) . . ? Cl3 C2S H2S1 108.8 . . ? Cl4 C2S H2S1 108.8 . . ? Cl3 C2S H2S2 108.8 . . ? Cl4 C2S H2S2 108.8 . . ? H2S1 C2S H2S2 107.7 . . ? Cl3 Cl5 C3S 174.7(14) . . ? Cl3 Cl5 Cl4 168.3(13) . . ? Cl5 C3S Cl6 113.9(4) . . ? Cl5 C3S H3S1 108.8 . . ? Cl6 C3S H3S1 108.8 . . ? Cl5 C3S H3S2 108.8 . . ? Cl6 C3S H3S2 108.8 . . ? H3S1 C3S H3S2 107.7 . . ? Cl7 Cl10 Cl8 107.1(6) . . ? C5S Cl10 Cl8 96.3(6) . . ? Cl7 C5S Cl9 99.3(13) . . ? Cl9 C5S Cl10 115.8(11) . . ? Cl7 C5S H5S1 111.9 . . ? Cl9 C5S H5S1 111.9 . . ? Cl10 C5S H5S1 76.0 . . ? Cl7 C5S H5S2 111.9 . . ? Cl9 C5S H5S2 111.9 . . ? Cl10 C5S H5S2 125.1 . . ? H5S1 C5S H5S2 109.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N2 C3 C1 1.9(4) . . . . ? C20 C1 C3 N2 166.7(3) . . . . ? C21 C1 C3 N2 -3.6(4) . . . . ? C3 N2 C4 C5 -178.2(3) . . . . ? C3 N2 C4 C21 0.6(4) . . . . ? N2 C4 C5 C6 145.0(3) . . . . ? C21 C4 C5 C6 -33.4(5) . . . . ? N2 C4 C5 C51 -32.2(5) . . . . ? C21 C4 C5 C51 149.3(4) . . . . ? C9 N22 C6 C5 -179.6(3) . . . . ? C9 N22 C6 C7 -0.6(4) . . . . ? C4 C5 C6 N22 -25.5(5) . . . . ? C51 C5 C6 N22 151.8(3) . . . . ? C4 C5 C6 C7 155.7(4) . . . . ? C51 C5 C6 C7 -27.0(5) . . . . ? N22 C6 C7 C8 1.2(4) . . . . ? C5 C6 C7 C8 -179.8(4) . . . . ? C6 C7 C8 C9 -1.4(4) . . . . ? C6 N22 C9 C10 178.6(3) . . . . ? C6 N22 C9 C8 -0.3(4) . . . . ? C7 C8 C9 N22 1.0(4) . . . . ? C7 C8 C9 C10 -177.8(3) . . . . ? N22 C9 C10 C11 11.5(6) . . . . ? C8 C9 C10 C11 -169.9(3) . . . . ? N22 C9 C10 C61 -171.6(3) . . . . ? C8 C9 C10 C61 7.0(5) . . . . ? C14 N23 C11 C10 174.9(3) . . . . ? C14 N23 C11 C12 -4.4(4) . . . . ? C9 C10 C11 N23 15.1(6) . . . . ? C61 C10 C11 N23 -161.8(3) . . . . ? C9 C10 C11 C12 -165.7(3) . . . . ? C61 C10 C11 C12 17.3(5) . . . . ? N23 C11 C12 C13 2.5(4) . . . . ? C10 C11 C12 C13 -176.8(3) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C11 N23 C14 C15 -172.1(3) . . . . ? C11 N23 C14 C13 4.6(4) . . . . ? C12 C13 C14 N23 -3.0(4) . . . . ? C12 C13 C14 C15 173.6(3) . . . . ? N23 C14 C15 C16 -3.8(5) . . . . ? C13 C14 C15 C16 -179.9(3) . . . . ? N23 C14 C15 C71 172.2(3) . . . . ? C13 C14 C15 C71 -3.9(5) . . . . ? C19 N24 C16 C15 -176.0(3) . . . . ? C19 N24 C16 C17 2.6(4) . . . . ? C14 C15 C16 N24 -12.9(5) . . . . ? C71 C15 C16 N24 171.0(3) . . . . ? C14 C15 C16 C17 168.6(3) . . . . ? C71 C15 C16 C17 -7.5(5) . . . . ? N24 C16 C17 C18 -1.0(4) . . . . ? C15 C16 C17 C18 177.7(3) . . . . ? C16 C17 C18 C19 -1.1(4) . . . . ? C16 N24 C19 C20 167.4(3) . . . . ? C16 N24 C19 C18 -3.3(4) . . . . ? C17 C18 C19 N24 2.7(4) . . . . ? C17 C18 C19 C20 -167.7(3) . . . . ? N24 C19 C20 C1 14.9(5) . . . . ? C18 C19 C20 C1 -176.0(3) . . . . ? N24 C19 C20 C81 -157.9(3) . . . . ? C18 C19 C20 C81 11.2(5) . . . . ? C3 C1 C20 C19 -134.8(3) . . . . ? C21 C1 C20 C19 33.0(5) . . . . ? C3 C1 C20 C81 38.0(5) . . . . ? C21 C1 C20 C81 -154.3(3) . . . . ? C20 C1 C21 C4 -165.4(3) . . . . ? C3 C1 C21 C4 3.7(4) . . . . ? C20 C1 C21 P1 40.4(5) . . . . ? C3 C1 C21 P1 -150.6(2) . . . . ? N2 C4 C21 C1 -2.7(4) . . . . ? C5 C4 C21 C1 175.9(3) . . . . ? N2 C4 C21 P1 150.8(3) . . . . ? C5 C4 C21 P1 -30.6(5) . . . . ? C22 P1 C21 C1 119.2(3) . . . . ? C28 P1 C21 C1 11.2(3) . . . . ? S1 P1 C21 C1 -116.0(3) . . . . ? C22 P1 C21 C4 -29.6(3) . . . . ? C28 P1 C21 C4 -137.6(3) . . . . ? S1 P1 C21 C4 95.2(3) . . . . ? C21 P1 C22 C27 148.3(3) . . . . ? C28 P1 C22 C27 -100.0(3) . . . . ? S1 P1 C22 C27 17.1(3) . . . . ? C21 P1 C22 C23 -35.8(3) . . . . ? C28 P1 C22 C23 75.8(3) . . . . ? S1 P1 C22 C23 -167.1(3) . . . . ? C27 C22 C23 C24 -1.5(5) . . . . ? P1 C22 C23 C24 -177.3(3) . . . . ? C22 C23 C24 C25 2.7(5) . . . . ? C23 C24 C25 C26 -2.1(6) . . . . ? C24 C25 C26 C27 0.5(6) . . . . ? C23 C22 C27 C26 -0.2(5) . . . . ? P1 C22 C27 C26 175.7(3) . . . . ? C25 C26 C27 C22 0.7(6) . . . . ? C21 P1 C28 C29 65.0(3) . . . . ? C22 P1 C28 C29 -44.0(3) . . . . ? S1 P1 C28 C29 -161.6(3) . . . . ? C21 P1 C28 C33 -121.6(3) . . . . ? C22 P1 C28 C33 129.4(3) . . . . ? S1 P1 C28 C33 11.8(3) . . . . ? C33 C28 C29 C30 -0.3(5) . . . . ? P1 C28 C29 C30 173.2(3) . . . . ? C28 C29 C30 C31 -0.9(6) . . . . ? C29 C30 C31 C32 1.5(6) . . . . ? C30 C31 C32 C33 -1.0(6) . . . . ? C31 C32 C33 C28 -0.1(6) . . . . ? C29 C28 C33 C32 0.7(5) . . . . ? P1 C28 C33 C32 -172.9(3) . . . . ? C6 C5 C51 C52 150.5(3) . . . . ? C4 C5 C51 C52 -32.2(5) . . . . ? C6 C5 C51 C56 -28.9(5) . . . . ? C4 C5 C51 C56 148.4(3) . . . . ? C56 C51 C52 C53 2.5(5) . . . . ? C5 C51 C52 C53 -177.0(3) . . . . ? C51 C52 C53 C54 -0.5(6) . . . . ? C52 C53 C54 C55 -1.5(6) . . . . ? C52 C53 C54 C57 179.9(4) . . . . ? C53 C54 C55 C56 1.4(6) . . . . ? C57 C54 C55 C56 -180.0(4) . . . . ? C54 C55 C56 C51 0.7(6) . . . . ? C52 C51 C56 C55 -2.6(5) . . . . ? C5 C51 C56 C55 176.9(3) . . . . ? C9 C10 C61 C66 -123.3(4) . . . . ? C11 C10 C61 C66 53.9(5) . . . . ? C9 C10 C61 C62 52.5(4) . . . . ? C11 C10 C61 C62 -130.3(3) . . . . ? C66 C61 C62 C63 -3.1(5) . . . . ? C10 C61 C62 C63 -178.9(3) . . . . ? C61 C62 C63 C64 0.6(5) . . . . ? C62 C63 C64 C65 2.5(5) . . . . ? C62 C63 C64 C67 -179.5(3) . . . . ? C63 C64 C65 C66 -3.1(6) . . . . ? C67 C64 C65 C66 178.9(4) . . . . ? C64 C65 C66 C61 0.7(6) . . . . ? C62 C61 C66 C65 2.5(5) . . . . ? C10 C61 C66 C65 178.4(3) . . . . ? C14 C15 C71 C76 127.2(3) . . . . ? C16 C15 C71 C76 -56.5(4) . . . . ? C14 C15 C71 C72 -58.7(5) . . . . ? C16 C15 C71 C72 117.6(4) . . . . ? C76 C71 C72 C73 2.9(5) . . . . ? C15 C71 C72 C73 -171.3(3) . . . . ? C71 C72 C73 C74 -0.3(6) . . . . ? C72 C73 C74 C75 -2.8(6) . . . . ? C72 C73 C74 C77 176.9(4) . . . . ? C73 C74 C75 C76 3.3(5) . . . . ? C77 C74 C75 C76 -176.5(4) . . . . ? C74 C75 C76 C71 -0.6(6) . . . . ? C72 C71 C76 C75 -2.5(5) . . . . ? C15 C71 C76 C75 171.9(3) . . . . ? C19 C20 C81 C86 -144.4(3) . . . . ? C1 C20 C81 C86 42.6(5) . . . . ? C19 C20 C81 C82 36.9(5) . . . . ? C1 C20 C81 C82 -136.0(3) . . . . ? C86 C81 C82 C83 3.1(5) . . . . ? C20 C81 C82 C83 -178.2(3) . . . . ? C81 C82 C83 C84 -1.7(5) . . . . ? C82 C83 C84 C85 -0.4(6) . . . . ? C82 C83 C84 C87 179.1(4) . . . . ? C83 C84 C85 C86 1.2(6) . . . . ? C87 C84 C85 C86 -178.3(4) . . . . ? C84 C85 C86 C81 0.3(6) . . . . ? C82 C81 C86 C85 -2.4(5) . . . . ? C20 C81 C86 C85 178.9(3) . . . . ? C3A N2A C1A C20A 171.6(3) . . . . ? C3A N2A C1A C21A -0.9(4) . . . . ? C1A N2A C3A C4A -0.4(4) . . . . ? N2A C3A C4A C5A -173.1(3) . . . . ? N2A C3A C4A C21A 1.5(4) . . . . ? C3A C4A C5A C6A 137.7(4) . . . . ? C21A C4A C5A C6A -35.5(6) . . . . ? C3A C4A C5A C51A -36.6(5) . . . . ? C21A C4A C5A C51A 150.2(4) . . . . ? C9A N22A C6A C5A 176.4(3) . . . . ? C9A N22A C6A C7A -2.5(4) . . . . ? C4A C5A C6A N22A -11.2(5) . . . . ? C51A C5A C6A N22A 162.9(3) . . . . ? C4A C5A C6A C7A 167.4(4) . . . . ? C51A C5A C6A C7A -18.5(6) . . . . ? N22A C6A C7A C8A 2.1(4) . . . . ? C5A C6A C7A C8A -176.6(4) . . . . ? C6A C7A C8A C9A -1.1(4) . . . . ? C6A N22A C9A C10A -176.9(3) . . . . ? C6A N22A C9A C8A 1.8(4) . . . . ? C7A C8A C9A N22A -0.4(4) . . . . ? C7A C8A C9A C10A 178.3(3) . . . . ? N22A C9A C10A C11A 9.0(5) . . . . ? C8A C9A C10A C11A -169.5(3) . . . . ? N22A C9A C10A C61A -172.7(3) . . . . ? C8A C9A C10A C61A 8.7(5) . . . . ? C14A N23A C11A C10A 172.5(3) . . . . ? C14A N23A C11A C12A -2.8(4) . . . . ? C9A C10A C11A N23A 6.0(6) . . . . ? C61A C10A C11A N23A -172.2(3) . . . . ? C9A C10A C11A C12A -179.3(3) . . . . ? C61A C10A C11A C12A 2.5(5) . . . . ? N23A C11A C12A C13A 1.9(4) . . . . ? C10A C11A C12A C13A -173.6(3) . . . . ? C11A C12A C13A C14A -0.2(4) . . . . ? C11A N23A C14A C15A -172.7(3) . . . . ? C11A N23A C14A C13A 2.6(4) . . . . ? C12A C13A C14A N23A -1.5(4) . . . . ? C12A C13A C14A C15A 174.0(3) . . . . ? N23A C14A C15A C16A -8.1(5) . . . . ? C13A C14A C15A C16A 177.1(3) . . . . ? N23A C14A C15A C71A 169.5(3) . . . . ? C13A C14A C15A C71A -5.3(5) . . . . ? C19A N24A C16A C15A -178.2(3) . . . . ? C19A N24A C16A C17A 0.7(4) . . . . ? C14A C15A C16A N24A 0.9(6) . . . . ? C71A C15A C16A N24A -176.7(3) . . . . ? C14A C15A C16A C17A -177.8(3) . . . . ? C71A C15A C16A C17A 4.6(5) . . . . ? N24A C16A C17A C18A -0.5(4) . . . . ? C15A C16A C17A C18A 178.4(3) . . . . ? C16A C17A C18A C19A 0.1(4) . . . . ? C16A N24A C19A C20A 177.7(3) . . . . ? C16A N24A C19A C18A -0.6(4) . . . . ? C17A C18A C19A N24A 0.3(4) . . . . ? C17A C18A C19A C20A -177.9(3) . . . . ? N24A C19A C20A C1A 8.5(5) . . . . ? C18A C19A C20A C1A -173.7(3) . . . . ? N24A C19A C20A C81A -163.4(3) . . . . ? C18A C19A C20A C81A 14.4(5) . . . . ? N2A C1A C20A C19A -141.4(3) . . . . ? C21A C1A C20A C19A 29.2(5) . . . . ? N2A C1A C20A C81A 30.7(4) . . . . ? C21A C1A C20A C81A -158.8(3) . . . . ? C3A C4A C21A C1A -1.9(4) . . . . ? C5A C4A C21A C1A 172.1(3) . . . . ? C3A C4A C21A P2 142.4(3) . . . . ? C5A C4A C21A P2 -43.6(5) . . . . ? C20A C1A C21A C4A -169.3(4) . . . . ? N2A C1A C21A C4A 1.8(4) . . . . ? C20A C1A C21A P2 48.8(5) . . . . ? N2A C1A C21A P2 -140.1(3) . . . . ? C22A P2 C21A C4A -55.6(3) . . . . ? C28A P2 C21A C4A -164.7(3) . . . . ? S2 P2 C21A C4A 66.9(3) . . . . ? C22A P2 C21A C1A 81.1(3) . . . . ? C28A P2 C21A C1A -28.1(3) . . . . ? S2 P2 C21A C1A -156.5(2) . . . . ? C21A P2 C22A C27A 151.2(3) . . . . ? C28A P2 C22A C27A -93.8(4) . . . . ? S2 P2 C22A C27A 23.5(4) . . . . ? C21A P2 C22A C23A -27.4(3) . . . . ? C28A P2 C22A C23A 87.5(3) . . . . ? S2 P2 C22A C23A -155.2(3) . . . . ? C27A C22A C23A C24A 1.3(6) . . . . ? P2 C22A C23A C24A 180.0(3) . . . . ? C22A C23A C24A C25A -0.9(6) . . . . ? C23A C24A C25A C26A -0.5(7) . . . . ? C24A C25A C26A C27A 1.3(9) . . . . ? C25A C26A C27A C22A -0.9(9) . . . . ? C23A C22A C27A C26A -0.5(7) . . . . ? P2 C22A C27A C26A -179.2(4) . . . . ? C21A P2 C28A C33A -110.0(3) . . . . ? C22A P2 C28A C33A 141.2(3) . . . . ? S2 P2 C28A C33A 23.2(3) . . . . ? C21A P2 C28A C29A 76.4(4) . . . . ? C22A P2 C28A C29A -32.5(4) . . . . ? S2 P2 C28A C29A -150.5(3) . . . . ? C33A C28A C29A C30A -1.7(6) . . . . ? P2 C28A C29A C30A 172.0(4) . . . . ? C28A C29A C30A C31A 1.3(7) . . . . ? C29A C30A C31A C32A -0.6(7) . . . . ? C30A C31A C32A C33A 0.4(7) . . . . ? C29A C28A C33A C32A 1.5(6) . . . . ? P2 C28A C33A C32A -172.5(3) . . . . ? C31A C32A C33A C28A -0.8(7) . . . . ? C6A C5A C51A C56A -36.9(5) . . . . ? C4A C5A C51A C56A 137.5(4) . . . . ? C6A C5A C51A C52A 145.2(4) . . . . ? C4A C5A C51A C52A -40.3(5) . . . . ? C56A C51A C52A C53A -1.8(6) . . . . ? C5A C51A C52A C53A 176.2(3) . . . . ? C51A C52A C53A C54A 1.5(6) . . . . ? C52A C53A C54A C55A -0.6(7) . . . . ? C52A C53A C54A C57A -177.4(5) . . . . ? C53A C54A C55A C56A 0.1(8) . . . . ? C57A C54A C55A C56A 176.9(5) . . . . ? C52A C51A C56A C55A 1.2(6) . . . . ? C5A C51A C56A C55A -176.6(4) . . . . ? C54A C55A C56A C51A -0.4(8) . . . . ? C11A C10A C61A C66A 59.9(5) . . . . ? C9A C10A C61A C66A -118.4(4) . . . . ? C11A C10A C61A C62A -121.1(4) . . . . ? C9A C10A C61A C62A 60.5(4) . . . . ? C66A C61A C62A C63A -0.3(5) . . . . ? C10A C61A C62A C63A -179.3(3) . . . . ? C61A C62A C63A C64A 0.5(6) . . . . ? C62A C63A C64A C65A -1.1(6) . . . . ? C62A C63A C64A C67A 179.0(4) . . . . ? C63A C64A C65A C66A 1.5(6) . . . . ? C67A C64A C65A C66A -178.6(4) . . . . ? C64A C65A C66A C61A -1.4(6) . . . . ? C62A C61A C66A C65A 0.8(6) . . . . ? C10A C61A C66A C65A 179.7(4) . . . . ? C16A C15A C71A C72A -109.7(4) . . . . ? C14A C15A C71A C72A 72.5(4) . . . . ? C16A C15A C71A C76A 74.0(4) . . . . ? C14A C15A C71A C76A -103.8(4) . . . . ? C76A C71A C72A C73A 2.7(5) . . . . ? C15A C71A C72A C73A -173.7(3) . . . . ? C71A C72A C73A C74A -1.6(6) . . . . ? C72A C73A C74A C75A -0.1(5) . . . . ? C72A C73A C74A C77A 176.7(3) . . . . ? C73A C74A C75A C76A 0.8(6) . . . . ? C77A C74A C75A C76A -176.0(4) . . . . ? C74A C75A C76A C71A 0.3(6) . . . . ? C72A C71A C76A C75A -2.0(6) . . . . ? C15A C71A C76A C75A 174.4(3) . . . . ? C19A C20A C81A C82A 43.2(5) . . . . ? C1A C20A C81A C82A -128.9(4) . . . . ? C19A C20A C81A C86A -144.6(3) . . . . ? C1A C20A C81A C86A 43.3(5) . . . . ? C86A C81A C82A C83A 0.1(5) . . . . ? C20A C81A C82A C83A 172.5(3) . . . . ? C81A C82A C83A C84A 0.4(6) . . . . ? C82A C83A C84A C85A -0.2(6) . . . . ? C82A C83A C84A C87A -178.9(4) . . . . ? C83A C84A C85A C86A -0.6(6) . . . . ? C87A C84A C85A C86A 178.1(4) . . . . ? C84A C85A C86A C81A 1.2(6) . . . . ? C82A C81A C86A C85A -0.9(6) . . . . ? C20A C81A C86A C85A -173.5(3) . . . . ? C5S Cl7 C4S Cl8 -111.7(12) . . . . ? Cl10 Cl7 C4S Cl8 90.5(14) . . . . ? Cl9 Cl7 C4S Cl8 -65.1(8) . . . . ? Cl10 Cl8 C4S Cl7 -49.1(7) . . . . ? Cl5 Cl3 C2S Cl4 2.9(14) . . . . ? Cl6 Cl4 C2S Cl3 98.6(10) . . . . ? Cl5 Cl4 C2S Cl3 -1.3(7) . . . . ? C2S Cl3 Cl5 Cl4 -11(5) . . . . ? Cl6 Cl4 Cl5 Cl3 -81(6) . . . . ? C2S Cl4 Cl5 Cl3 13(6) . . . . ? Cl6 Cl4 Cl5 C3S 123(5) . . . . ? C2S Cl4 Cl5 C3S -143(5) . . . . ? C2S Cl4 Cl6 C3S -78(3) . . . . ? Cl5 Cl4 Cl6 C3S -40(3) . . . . ? Cl4 Cl5 C3S Cl6 -40(3) . . . . ? Cl4 Cl6 C3S Cl5 125(5) . . . . ? Cl10 Cl7 Cl9 C5S -89.9(17) . . . . ? C4S Cl7 Cl9 C5S -71.0(14) . . . . ? C4S Cl7 Cl10 C5S 24.1(17) . . . . ? Cl9 Cl7 Cl10 C5S 56.2(11) . . . . ? C5S Cl7 Cl10 Cl8 -72.1(13) . . . . ? C4S Cl7 Cl10 Cl8 -48.0(6) . . . . ? Cl9 Cl7 Cl10 Cl8 -15.9(14) . . . . ? C4S Cl8 Cl10 Cl7 82.7(10) . . . . ? C4S Cl8 Cl10 C5S 54.4(10) . . . . ? Cl10 Cl7 C5S Cl9 121.7(10) . . . . ? C4S Cl7 C5S Cl9 107.1(11) . . . . ? C4S Cl7 C5S Cl10 -14.6(9) . . . . ? Cl9 Cl7 C5S Cl10 -121.7(10) . . . . ? Cl7 Cl9 C5S Cl10 33.7(7) . . . . ? Cl8 Cl10 C5S Cl7 113.8(13) . . . . ? Cl7 Cl10 C5S Cl9 -68.9(13) . . . . ? Cl8 Cl10 C5S Cl9 44.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.649 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.685 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.077 # Attachment '- PSS.CIF' data_ng08 _database_code_depnum_ccdc_archive 'CCDC 893468' #TrackingRef '- PSS.CIF' _audit_update_record ; 2012-03-16 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,10,15,20-Tetratolyl-2-aza-21-carbaporphiryno-21-diphenylphosphinodithioate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H47 N4 P S2' _chemical_formula_weight 919.11 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.678(4) _cell_length_b 15.687(4) _cell_length_c 20.796(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.53(3) _cell_angle_gamma 90.00 _cell_volume 4708(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57874 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.65 _diffrn_reflns_theta_max 35.00 _reflns_number_total 19138 _reflns_number_gt 9965 _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^)+(0.0440P)^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_number_reflns 19138 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 S1 S 0.48514(2) 0.76463(2) 0.677629(17) 0.01737(8) Uani 1 1 d . . . S2 S 0.27389(3) 0.74989(3) 0.727801(19) 0.02658(10) Uani 1 1 d . . . P P 0.40076(3) 0.79084(3) 0.747355(18) 0.01890(9) Uani 1 1 d . . . N24 N 0.47541(8) 0.61507(8) 0.58496(6) 0.0180(3) Uani 1 1 d . . . H24 H 0.5021 0.6606 0.5748 0.022 Uiso 1 1 calc R . . N2 N 0.28863(8) 0.81773(9) 0.52297(6) 0.0224(3) Uani 1 1 d . . . C206 C 0.19070(10) 0.58473(10) 0.49572(7) 0.0230(3) Uani 1 1 d . . . H206 H 0.2356 0.5504 0.4825 0.028 Uiso 1 1 calc R . . N23 N 0.66309(8) 0.68366(8) 0.60356(6) 0.0174(3) Uani 1 1 d . . . C201 C 0.21740(9) 0.64939(10) 0.54132(7) 0.0189(3) Uani 1 1 d . . . N22 N 0.61201(7) 0.86684(8) 0.59946(6) 0.0165(2) Uani 1 1 d . . . H22 H 0.5827 0.8193 0.5921 0.020 Uiso 1 1 calc R . . C102 C 0.89279(10) 0.87198(10) 0.55072(8) 0.0247(3) Uani 1 1 d . . . H102 H 0.8496 0.8775 0.5122 0.030 Uiso 1 1 calc R . . C204 C 0.02896(10) 0.62050(11) 0.48928(7) 0.0238(3) Uani 1 1 d . . . C202 C 0.14752(10) 0.69730(10) 0.56208(7) 0.0200(3) Uani 1 1 d . . . H202 H 0.1635 0.7398 0.5933 0.024 Uiso 1 1 calc R . . C207 C -0.07117(10) 0.61123(12) 0.45616(8) 0.0300(4) Uani 1 1 d . . . H20A H -0.1103 0.6139 0.4884 0.045 Uiso 1 1 calc R . . H20B H -0.0796 0.5574 0.4340 0.045 Uiso 1 1 calc R . . H20C H -0.0872 0.6565 0.4251 0.045 Uiso 1 1 calc R . . C20 C 0.31586(9) 0.67169(10) 0.56414(7) 0.0172(3) Uani 1 1 d . . . C3 C 0.32945(9) 0.89244(10) 0.53418(6) 0.0166(3) Uani 1 1 d . . . H3 H 0.3074 0.9424 0.5127 0.020 Uiso 1 1 calc R . . C203 C 0.05548(10) 0.68215(10) 0.53682(7) 0.0216(3) Uani 1 1 d . . . H203 H 0.0102 0.7139 0.5519 0.026 Uiso 1 1 calc R . . C156 C 0.62973(10) 0.37287(10) 0.60533(7) 0.0224(3) Uani 1 1 d . . . H156 H 0.5907 0.3768 0.5648 0.027 Uiso 1 1 calc R . . C155 C 0.66235(10) 0.29347(10) 0.62872(7) 0.0232(3) Uani 1 1 d . . . H155 H 0.6449 0.2452 0.6035 0.028 Uiso 1 1 calc R . . C152 C 0.71435(10) 0.43785(10) 0.70182(7) 0.0214(3) Uani 1 1 d . . . H152 H 0.7323 0.4860 0.7271 0.026 Uiso 1 1 calc R . . C101 C 0.86685(9) 0.83560(9) 0.60602(7) 0.0193(3) Uani 1 1 d . . . C151 C 0.65459(9) 0.44671(10) 0.64163(7) 0.0184(3) Uani 1 1 d . . . C23 C 0.33351(11) 0.94690(11) 0.78227(7) 0.0257(4) Uani 1 1 d . . . H23 H 0.2790 0.9174 0.7840 0.031 Uiso 1 1 calc R . . C106 C 0.93359(10) 0.82786(10) 0.66270(8) 0.0245(3) Uani 1 1 d . . . H106 H 0.9179 0.8030 0.6998 0.029 Uiso 1 1 calc R . . C31 C 0.59460(12) 0.63837(12) 0.90359(8) 0.0353(4) Uani 1 1 d . . . H31 H 0.6326 0.6068 0.9357 0.042 Uiso 1 1 calc R . . C154 C 0.72064(10) 0.28481(10) 0.68922(7) 0.0221(3) Uani 1 1 d . . . C16 C 0.52101(10) 0.54231(10) 0.60703(7) 0.0193(3) Uani 1 1 d . . . C21 C 0.41805(9) 0.80210(9) 0.60405(7) 0.0156(3) Uani 1 1 d . . . C105 C 1.02362(10) 0.85699(11) 0.66438(9) 0.0283(4) Uani 1 1 d . . . H105 H 1.0674 0.8512 0.7026 0.034 Uiso 1 1 calc R . . C7 C 0.64416(9) 1.00461(10) 0.62090(7) 0.0185(3) Uani 1 1 d . . . H7 H 0.6379 1.0622 0.6297 0.022 Uiso 1 1 calc R . . C153 C 0.74719(10) 0.35877(10) 0.72447(7) 0.0219(3) Uani 1 1 d . . . H153 H 0.7880 0.3550 0.7642 0.026 Uiso 1 1 calc R . . C57 C 0.30262(12) 1.29174(11) 0.57831(10) 0.0390(4) Uani 1 1 d . . . H57A H 0.3381 1.3311 0.5575 0.058 Uiso 1 1 calc R . . H57B H 0.2982 1.3124 0.6211 0.058 Uiso 1 1 calc R . . H57C H 0.2416 1.2863 0.5525 0.058 Uiso 1 1 calc R . . C22 C 0.40933(10) 0.90373(10) 0.76484(7) 0.0205(3) Uani 1 1 d . . . C8 C 0.72568(10) 0.96325(9) 0.61932(7) 0.0196(3) Uani 1 1 d . . . H8 H 0.7842 0.9881 0.6262 0.024 Uiso 1 1 calc R . . C17 C 0.45146(10) 0.48240(10) 0.61620(8) 0.0259(4) Uani 1 1 d . . . H17 H 0.4617 0.4267 0.6311 0.031 Uiso 1 1 calc R . . C205 C 0.09789(10) 0.57114(10) 0.46996(8) 0.0249(3) Uani 1 1 d . . . H205 H 0.0814 0.5282 0.4392 0.030 Uiso 1 1 calc R . . C51 C 0.43483(9) 1.04413(9) 0.59221(7) 0.0164(3) Uani 1 1 d . . . C13 C 0.77995(9) 0.58132(10) 0.61813(7) 0.0180(3) Uani 1 1 d . . . H13 H 0.8091 0.5286 0.6246 0.022 Uiso 1 1 calc R . . C29 C 0.54749(11) 0.77212(11) 0.85342(8) 0.0275(4) Uani 1 1 d . . . H29 H 0.5573 0.8304 0.8500 0.033 Uiso 1 1 calc R . . C30 C 0.60650(11) 0.72474(11) 0.89992(8) 0.0293(4) Uani 1 1 d . . . H30 H 0.6540 0.7516 0.9285 0.035 Uiso 1 1 calc R . . C1 C 0.34156(9) 0.75856(9) 0.56574(7) 0.0164(3) Uani 1 1 d . . . C107 C 1.14479(11) 0.93156(12) 0.61332(10) 0.0384(5) Uani 1 1 d . . . H10A H 1.1558 0.9419 0.5699 0.058 Uiso 1 1 calc R . . H10B H 1.1901 0.8921 0.6352 0.058 Uiso 1 1 calc R . . H10C H 1.1494 0.9842 0.6372 0.058 Uiso 1 1 calc R . . C104 C 1.04897(10) 0.89459(10) 0.60972(9) 0.0265(4) Uani 1 1 d . . . C53 C 0.42809(10) 1.19149(10) 0.55724(7) 0.0238(3) Uani 1 1 d . . . H53 H 0.4530 1.2358 0.5363 0.029 Uiso 1 1 calc R . . C54 C 0.34944(10) 1.20634(10) 0.58421(8) 0.0251(3) Uani 1 1 d . . . C56 C 0.35600(9) 1.05956(10) 0.61980(7) 0.0203(3) Uani 1 1 d . . . H56 H 0.3311 1.0155 0.6410 0.024 Uiso 1 1 calc R . . C5 C 0.47426(9) 0.95763(9) 0.59633(6) 0.0160(3) Uani 1 1 d . . . C4 C 0.41160(9) 0.88799(9) 0.58307(7) 0.0161(3) Uani 1 1 d . . . C19 C 0.38117(10) 0.60671(10) 0.58098(7) 0.0196(3) Uani 1 1 d . . . C52 C 0.46998(10) 1.11207(10) 0.56098(7) 0.0197(3) Uani 1 1 d . . . H52 H 0.5223 1.1039 0.5424 0.024 Uiso 1 1 calc R . . C26 C 0.49485(11) 1.03646(11) 0.77693(8) 0.0279(4) Uani 1 1 d . . . H26 H 0.5489 1.0667 0.7753 0.033 Uiso 1 1 calc R . . C18 C 0.36695(10) 0.52131(10) 0.59926(8) 0.0255(3) Uani 1 1 d . . . H18 H 0.3098 0.4960 0.5997 0.031 Uiso 1 1 calc R . . C25 C 0.42046(13) 1.07760(12) 0.79426(8) 0.0343(4) Uani 1 1 d . . . H25 H 0.4241 1.1354 0.8043 0.041 Uiso 1 1 calc R . . C157 C 0.75276(12) 0.19874(10) 0.71660(8) 0.0290(4) Uani 1 1 d . . . H15A H 0.8070 0.2055 0.7498 0.043 Uiso 1 1 calc R . . H15B H 0.7672 0.1633 0.6822 0.043 Uiso 1 1 calc R . . H15C H 0.7045 0.1725 0.7353 0.043 Uiso 1 1 calc R . . C24 C 0.33942(13) 1.03234(12) 0.79672(8) 0.0331(4) Uani 1 1 d . . . H24A H 0.2889 1.0603 0.8083 0.040 Uiso 1 1 calc R . . C15 C 0.61816(9) 0.53241(9) 0.61887(7) 0.0181(3) Uani 1 1 d . . . C6 C 0.57022(9) 0.94450(9) 0.60676(7) 0.0163(3) Uani 1 1 d . . . C28 C 0.47495(10) 0.73409(10) 0.81255(7) 0.0226(3) Uani 1 1 d . . . C33 C 0.46572(14) 0.64606(13) 0.81528(10) 0.0528(6) Uani 1 1 d . . . H33 H 0.4183 0.6188 0.7870 0.063 Uiso 1 1 calc R . . C9 C 0.70580(9) 0.87554(10) 0.60541(7) 0.0172(3) Uani 1 1 d . . . C32 C 0.52715(15) 0.59870(14) 0.86025(11) 0.0587(6) Uani 1 1 d . . . H32 H 0.5222 0.5396 0.8607 0.070 Uiso 1 1 calc R . . C27 C 0.49021(11) 0.95002(10) 0.76177(7) 0.0239(3) Uani 1 1 d . . . H27 H 0.5408 0.9229 0.7496 0.029 Uiso 1 1 calc R . . C10 C 0.76851(9) 0.80831(10) 0.60399(7) 0.0178(3) Uani 1 1 d . . . C14 C 0.68146(9) 0.59788(9) 0.61332(7) 0.0170(3) Uani 1 1 d . . . C12 C 0.82078(9) 0.65646(10) 0.61146(7) 0.0188(3) Uani 1 1 d . . . H12 H 0.8834 0.6656 0.6114 0.023 Uiso 1 1 calc R . . C55 C 0.31474(10) 1.13877(10) 0.61601(8) 0.0251(3) Uani 1 1 d . . . H55 H 0.2628 1.1473 0.6350 0.030 Uiso 1 1 calc R . . C103 C 0.98306(11) 0.89991(10) 0.55326(8) 0.0280(4) Uani 1 1 d . . . H103 H 0.9997 0.9229 0.5158 0.034 Uiso 1 1 calc R . . C11 C 0.74820(9) 0.72098(10) 0.60434(7) 0.0176(3) 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 S1 0.01508(16) 0.01814(19) 0.01863(16) 0.00094(14) 0.00238(13) 0.00116(14) S2 0.01842(18) 0.0337(3) 0.0282(2) 0.00117(18) 0.00580(15) -0.00495(17) P 0.01751(18) 0.0208(2) 0.01868(18) 0.00166(16) 0.00415(15) -0.00092(16) N24 0.0141(6) 0.0154(7) 0.0252(6) -0.0009(5) 0.0053(5) -0.0031(5) N2 0.0195(6) 0.0255(8) 0.0231(6) 0.0015(5) 0.0061(5) 0.0014(5) C206 0.0178(7) 0.0217(9) 0.0309(8) -0.0064(7) 0.0078(6) -0.0003(6) N23 0.0148(6) 0.0172(7) 0.0207(6) 0.0001(5) 0.0043(5) -0.0003(5) C201 0.0143(6) 0.0175(8) 0.0247(7) -0.0005(6) 0.0036(6) -0.0031(6) N22 0.0123(5) 0.0135(6) 0.0239(6) -0.0008(5) 0.0037(5) -0.0014(5) C102 0.0220(8) 0.0237(9) 0.0298(8) 0.0024(7) 0.0081(7) 0.0005(6) C204 0.0151(7) 0.0284(9) 0.0279(8) 0.0025(7) 0.0037(6) -0.0029(6) C202 0.0187(7) 0.0190(8) 0.0229(7) -0.0029(6) 0.0057(6) -0.0005(6) C207 0.0183(8) 0.0393(11) 0.0321(9) -0.0004(8) 0.0034(7) -0.0039(7) C20 0.0147(7) 0.0192(8) 0.0180(7) -0.0021(6) 0.0036(5) -0.0013(6) C3 0.0142(6) 0.0192(8) 0.0169(6) 0.0031(6) 0.0040(5) 0.0024(6) C203 0.0159(7) 0.0228(9) 0.0275(8) -0.0005(7) 0.0080(6) 0.0010(6) C156 0.0189(7) 0.0226(9) 0.0243(7) -0.0031(7) 0.0005(6) -0.0001(6) C155 0.0237(8) 0.0174(8) 0.0283(8) -0.0048(7) 0.0043(6) -0.0017(6) C152 0.0231(8) 0.0200(8) 0.0216(7) -0.0047(6) 0.0054(6) -0.0022(6) C101 0.0152(7) 0.0163(8) 0.0275(8) -0.0006(6) 0.0069(6) 0.0006(6) C151 0.0149(7) 0.0172(8) 0.0248(7) -0.0008(6) 0.0074(6) 0.0004(6) C23 0.0294(8) 0.0276(10) 0.0211(7) 0.0012(7) 0.0077(7) 0.0041(7) C106 0.0182(7) 0.0263(9) 0.0296(8) 0.0031(7) 0.0057(6) -0.0017(6) C31 0.0364(10) 0.0369(11) 0.0307(9) 0.0141(8) 0.0012(8) 0.0056(8) C154 0.0212(7) 0.0201(8) 0.0270(8) 0.0012(6) 0.0095(6) 0.0009(6) C16 0.0179(7) 0.0156(8) 0.0246(7) -0.0014(6) 0.0044(6) 0.0005(6) C21 0.0123(6) 0.0170(8) 0.0178(6) 0.0001(6) 0.0037(5) 0.0008(5) C105 0.0163(7) 0.0269(10) 0.0401(9) -0.0006(8) 0.0012(7) -0.0005(7) C7 0.0201(7) 0.0131(8) 0.0220(7) 0.0022(6) 0.0028(6) -0.0026(6) C153 0.0236(7) 0.0226(9) 0.0190(7) 0.0005(6) 0.0027(6) -0.0009(6) C57 0.0328(9) 0.0228(10) 0.0589(12) -0.0018(9) 0.0021(9) 0.0066(8) C22 0.0240(8) 0.0216(8) 0.0156(7) 0.0003(6) 0.0028(6) 0.0025(6) C8 0.0168(7) 0.0176(8) 0.0244(7) 0.0028(6) 0.0035(6) -0.0033(6) C17 0.0207(7) 0.0158(8) 0.0421(9) 0.0022(7) 0.0078(7) 0.0001(6) C205 0.0223(8) 0.0241(9) 0.0286(8) -0.0073(7) 0.0050(6) -0.0055(7) C51 0.0152(7) 0.0155(8) 0.0177(7) -0.0005(6) 0.0004(5) -0.0001(6) C13 0.0152(7) 0.0177(8) 0.0214(7) -0.0020(6) 0.0042(6) 0.0030(6) C29 0.0305(8) 0.0224(9) 0.0286(8) 0.0008(7) 0.0025(7) 0.0020(7) C30 0.0281(8) 0.0346(11) 0.0235(8) -0.0008(7) 0.0002(7) 0.0055(8) C1 0.0130(6) 0.0176(8) 0.0196(7) -0.0008(6) 0.0053(5) 0.0012(6) C107 0.0220(8) 0.0280(10) 0.0690(13) -0.0023(9) 0.0186(9) -0.0044(7) C104 0.0180(7) 0.0176(8) 0.0471(10) -0.0030(7) 0.0144(7) 0.0001(6) C53 0.0245(8) 0.0178(8) 0.0274(8) 0.0032(6) 0.0002(6) -0.0016(6) C54 0.0230(8) 0.0191(8) 0.0304(8) -0.0039(7) -0.0022(6) 0.0044(6) C56 0.0159(7) 0.0210(8) 0.0239(7) 0.0004(6) 0.0036(6) -0.0015(6) C5 0.0156(7) 0.0174(8) 0.0152(6) 0.0010(6) 0.0033(5) -0.0001(6) C4 0.0144(6) 0.0174(8) 0.0170(6) -0.0020(6) 0.0048(5) 0.0003(6) C19 0.0163(7) 0.0182(8) 0.0246(7) -0.0034(6) 0.0049(6) -0.0029(6) C52 0.0188(7) 0.0199(8) 0.0210(7) 0.0005(6) 0.0048(6) -0.0001(6) C26 0.0296(9) 0.0226(9) 0.0276(8) -0.0007(7) -0.0051(7) -0.0041(7) C18 0.0185(7) 0.0181(8) 0.0407(9) -0.0004(7) 0.0073(7) -0.0029(6) C25 0.0540(12) 0.0219(10) 0.0254(8) -0.0051(7) 0.0029(8) 0.0047(9) C157 0.0328(9) 0.0225(9) 0.0317(9) 0.0021(7) 0.0061(7) 0.0026(7) C24 0.0446(10) 0.0309(10) 0.0263(8) 0.0015(7) 0.0130(8) 0.0143(8) C15 0.0170(7) 0.0175(8) 0.0202(7) -0.0038(6) 0.0046(6) 0.0002(6) C6 0.0157(6) 0.0150(8) 0.0183(7) 0.0016(6) 0.0032(5) -0.0007(6) C28 0.0241(7) 0.0247(9) 0.0197(7) 0.0051(6) 0.0055(6) 0.0009(7) C33 0.0509(12) 0.0331(12) 0.0620(13) 0.0210(10) -0.0222(10) -0.0169(10) C9 0.0131(6) 0.0204(8) 0.0185(7) 0.0036(6) 0.0038(5) -0.0011(6) C32 0.0600(14) 0.0301(12) 0.0745(15) 0.0291(11) -0.0177(12) -0.0121(10) C27 0.0254(8) 0.0241(9) 0.0208(7) -0.0016(7) 0.0008(6) 0.0015(7) C10 0.0147(7) 0.0204(8) 0.0189(7) 0.0017(6) 0.0047(5) 0.0008(6) C14 0.0171(7) 0.0170(8) 0.0171(6) -0.0037(6) 0.0038(5) 0.0002(6) C12 0.0133(6) 0.0209(8) 0.0227(7) -0.0017(6) 0.0051(6) 0.0021(6) C55 0.0184(7) 0.0247(9) 0.0321(8) -0.0044(7) 0.0046(6) 0.0032(6) C103 0.0276(8) 0.0225(9) 0.0385(9) 0.0054(7) 0.0181(7) -0.0008(7) C11 0.0147(6) 0.0199(8) 0.0188(7) 0.0011(6) 0.0047(5) 0.0008(6) _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 S1 C21 1.7623(15) . ? S1 P 2.1124(8) . ? S2 P 1.9413(7) . ? P C22 1.8076(17) . ? P C28 1.8102(16) . ? N24 C16 1.3598(19) . ? N24 C19 1.3769(18) . ? N2 C3 1.3176(19) . ? N2 C1 1.4154(19) . ? C206 C205 1.386(2) . ? C206 C201 1.395(2) . ? N23 C11 1.3770(18) . ? N23 C14 1.3801(19) . ? C201 C202 1.402(2) . ? C201 C20 1.4784(19) . ? N22 C9 1.3664(17) . ? N22 C6 1.3848(18) . ? C102 C103 1.387(2) . ? C102 C101 1.398(2) . ? C204 C203 1.387(2) . ? C204 C205 1.390(2) . ? C204 C207 1.512(2) . ? C202 C203 1.378(2) . ? C20 C19 1.399(2) . ? C20 C1 1.413(2) . ? C3 C4 1.4297(19) . ? C156 C155 1.390(2) . ? C156 C151 1.394(2) . ? C155 C154 1.393(2) . ? C152 C153 1.382(2) . ? C152 C151 1.398(2) . ? C101 C106 1.394(2) . ? C101 C10 1.4988(19) . ? C151 C15 1.492(2) . ? C23 C24 1.373(2) . ? C23 C22 1.406(2) . ? C106 C105 1.393(2) . ? C31 C32 1.361(3) . ? C31 C30 1.370(2) . ? C154 C153 1.390(2) . ? C154 C157 1.507(2) . ? C16 C15 1.4105(19) . ? C16 C17 1.426(2) . ? C21 C4 1.414(2) . ? C21 C1 1.4265(19) . ? C105 C104 1.390(2) . ? C7 C8 1.367(2) . ? C7 C6 1.4273(19) . ? C57 C54 1.500(2) . ? C22 C27 1.403(2) . ? C8 C9 1.425(2) . ? C17 C18 1.370(2) . ? C51 C52 1.395(2) . ? C51 C56 1.403(2) . ? C51 C5 1.472(2) . ? C13 C12 1.341(2) . ? C13 C14 1.4542(19) . ? C29 C28 1.372(2) . ? C29 C30 1.390(2) . ? C107 C104 1.510(2) . ? C104 C103 1.381(2) . ? C53 C52 1.385(2) . ? C53 C54 1.392(2) . ? C54 C55 1.394(2) . ? C56 C55 1.378(2) . ? C5 C6 1.4005(19) . ? C5 C4 1.422(2) . ? C19 C18 1.418(2) . ? C26 C25 1.372(2) . ? C26 C27 1.391(2) . ? C25 C24 1.394(3) . ? C15 C14 1.404(2) . ? C28 C33 1.390(2) . ? C33 C32 1.390(3) . ? C9 C10 1.404(2) . ? C10 C11 1.402(2) . ? C12 C11 1.4574(19) . ? 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 C21 S1 P 103.08(5) . . ? C22 P C28 108.71(7) . . ? C22 P S2 113.27(5) . . ? C28 P S2 114.64(6) . . ? C22 P S1 107.50(5) . . ? C28 P S1 94.04(5) . . ? S2 P S1 116.88(3) . . ? C16 N24 C19 111.56(12) . . ? C3 N2 C1 107.00(12) . . ? C205 C206 C201 120.58(14) . . ? C11 N23 C14 105.09(11) . . ? C206 C201 C202 117.95(13) . . ? C206 C201 C20 121.80(13) . . ? C202 C201 C20 120.11(13) . . ? C9 N22 C6 111.18(12) . . ? C103 C102 C101 119.96(15) . . ? C203 C204 C205 118.03(13) . . ? C203 C204 C207 120.98(14) . . ? C205 C204 C207 120.86(14) . . ? C203 C202 C201 120.78(14) . . ? C19 C20 C1 121.95(13) . . ? C19 C20 C201 119.52(13) . . ? C1 C20 C201 118.49(12) . . ? N2 C3 C4 112.31(13) . . ? C202 C203 C204 121.33(14) . . ? C155 C156 C151 121.04(14) . . ? C156 C155 C154 121.26(14) . . ? C153 C152 C151 121.14(14) . . ? C106 C101 C102 118.46(13) . . ? C106 C101 C10 121.56(13) . . ? C102 C101 C10 119.95(13) . . ? C156 C151 C152 117.48(14) . . ? C156 C151 C15 122.26(13) . . ? C152 C151 C15 120.24(13) . . ? C24 C23 C22 120.37(16) . . ? C105 C106 C101 120.64(15) . . ? C32 C31 C30 119.99(17) . . ? C153 C154 C155 117.51(14) . . ? C153 C154 C157 120.70(14) . . ? C155 C154 C157 121.78(14) . . ? N24 C16 C15 124.81(13) . . ? N24 C16 C17 106.14(12) . . ? C15 C16 C17 129.03(14) . . ? C4 C21 C1 106.40(12) . . ? C4 C21 S1 125.52(11) . . ? C1 C21 S1 125.68(11) . . ? C104 C105 C106 120.89(15) . . ? C8 C7 C6 108.51(13) . . ? C152 C153 C154 121.52(14) . . ? C27 C22 C23 118.60(15) . . ? C27 C22 P 121.76(12) . . ? C23 C22 P 119.65(12) . . ? C7 C8 C9 108.40(13) . . ? C18 C17 C16 107.99(14) . . ? C206 C205 C204 121.23(14) . . ? C52 C51 C56 117.47(13) . . ? C52 C51 C5 123.82(13) . . ? C56 C51 C5 118.70(13) . . ? C12 C13 C14 107.06(13) . . ? C28 C29 C30 120.87(16) . . ? C31 C30 C29 119.87(16) . . ? C20 C1 N2 120.28(12) . . ? C20 C1 C21 130.88(13) . . ? N2 C1 C21 108.82(13) . . ? C103 C104 C105 118.05(14) . . ? C103 C104 C107 121.36(15) . . ? C105 C104 C107 120.55(16) . . ? C52 C53 C54 121.33(14) . . ? C53 C54 C55 117.76(14) . . ? C53 C54 C57 121.16(15) . . ? C55 C54 C57 121.07(15) . . ? C55 C56 C51 121.25(14) . . ? C6 C5 C4 120.90(13) . . ? C6 C5 C51 121.22(13) . . ? C4 C5 C51 117.61(12) . . ? C21 C4 C5 131.88(13) . . ? C21 C4 C3 105.43(12) . . ? C5 C4 C3 122.13(13) . . ? N24 C19 C20 125.48(13) . . ? N24 C19 C18 105.62(13) . . ? C20 C19 C18 128.87(13) . . ? C53 C52 C51 121.01(14) . . ? C25 C26 C27 120.64(16) . . ? C17 C18 C19 108.61(13) . . ? C26 C25 C24 119.69(16) . . ? C23 C24 C25 120.62(16) . . ? C14 C15 C16 124.63(14) . . ? C14 C15 C151 118.76(12) . . ? C16 C15 C151 116.55(13) . . ? N22 C6 C5 124.44(13) . . ? N22 C6 C7 105.57(12) . . ? C5 C6 C7 129.80(14) . . ? C29 C28 C33 118.51(15) . . ? C29 C28 P 122.88(13) . . ? C33 C28 P 118.00(13) . . ? C32 C33 C28 120.17(18) . . ? N22 C9 C10 125.22(14) . . ? N22 C9 C8 106.28(12) . . ? C10 C9 C8 128.24(13) . . ? C31 C32 C33 120.3(2) . . ? C26 C27 C22 120.07(15) . . ? C11 C10 C9 126.37(13) . . ? C11 C10 C101 118.92(13) . . ? C9 C10 C101 114.62(13) . . ? N23 C14 C15 127.66(13) . . ? N23 C14 C13 110.45(12) . . ? C15 C14 C13 121.89(13) . . ? C13 C12 C11 106.78(12) . . ? C56 C55 C54 121.18(14) . . ? C104 C103 C102 121.96(15) . . ? N23 C11 C10 127.49(13) . . ? N23 C11 C12 110.53(13) . . ? C10 C11 C12 121.79(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 S1 P C22 -76.76(7) . . . . ? C21 S1 P C28 172.17(7) . . . . ? C21 S1 P S2 51.88(6) . . . . ? C205 C206 C201 C202 2.7(2) . . . . ? C205 C206 C201 C20 -173.10(14) . . . . ? C206 C201 C202 C203 -1.6(2) . . . . ? C20 C201 C202 C203 174.21(14) . . . . ? C206 C201 C20 C19 -44.8(2) . . . . ? C202 C201 C20 C19 139.52(15) . . . . ? C206 C201 C20 C1 132.71(15) . . . . ? C202 C201 C20 C1 -43.0(2) . . . . ? C1 N2 C3 C4 1.22(15) . . . . ? C201 C202 C203 C204 -1.3(2) . . . . ? C205 C204 C203 C202 3.1(2) . . . . ? C207 C204 C203 C202 -172.79(15) . . . . ? C151 C156 C155 C154 0.2(2) . . . . ? C103 C102 C101 C106 -0.4(2) . . . . ? C103 C102 C101 C10 177.80(14) . . . . ? C155 C156 C151 C152 0.8(2) . . . . ? C155 C156 C151 C15 -177.86(13) . . . . ? C153 C152 C151 C156 -0.2(2) . . . . ? C153 C152 C151 C15 178.50(13) . . . . ? C102 C101 C106 C105 1.0(2) . . . . ? C10 C101 C106 C105 -177.21(15) . . . . ? C156 C155 C154 C153 -1.9(2) . . . . ? C156 C155 C154 C157 176.99(14) . . . . ? C19 N24 C16 C15 -177.20(13) . . . . ? C19 N24 C16 C17 1.63(16) . . . . ? P S1 C21 C4 81.32(12) . . . . ? P S1 C21 C1 -78.65(12) . . . . ? C101 C106 C105 C104 0.2(2) . . . . ? C151 C152 C153 C154 -1.5(2) . . . . ? C155 C154 C153 C152 2.5(2) . . . . ? C157 C154 C153 C152 -176.37(14) . . . . ? C24 C23 C22 C27 -0.8(2) . . . . ? C24 C23 C22 P 178.96(12) . . . . ? C28 P C22 C27 69.78(13) . . . . ? S2 P C22 C27 -161.55(10) . . . . ? S1 P C22 C27 -30.87(13) . . . . ? C28 P C22 C23 -109.99(12) . . . . ? S2 P C22 C23 18.69(13) . . . . ? S1 P C22 C23 149.36(11) . . . . ? C6 C7 C8 C9 -1.12(16) . . . . ? N24 C16 C17 C18 0.07(17) . . . . ? C15 C16 C17 C18 178.84(15) . . . . ? C201 C206 C205 C204 -0.8(2) . . . . ? C203 C204 C205 C206 -2.1(2) . . . . ? C207 C204 C205 C206 173.85(15) . . . . ? C32 C31 C30 C29 2.3(3) . . . . ? C28 C29 C30 C31 2.5(2) . . . . ? C19 C20 C1 N2 150.92(13) . . . . ? C201 C20 C1 N2 -26.53(19) . . . . ? C19 C20 C1 C21 -27.2(2) . . . . ? C201 C20 C1 C21 155.33(14) . . . . ? C3 N2 C1 C20 -178.62(12) . . . . ? C3 N2 C1 C21 -0.10(15) . . . . ? C4 C21 C1 C20 177.28(14) . . . . ? S1 C21 C1 C20 -19.6(2) . . . . ? C4 C21 C1 N2 -1.03(15) . . . . ? S1 C21 C1 N2 162.07(10) . . . . ? C106 C105 C104 C103 -1.9(2) . . . . ? C106 C105 C104 C107 175.70(15) . . . . ? C52 C53 C54 C55 0.9(2) . . . . ? C52 C53 C54 C57 -178.16(15) . . . . ? C52 C51 C56 C55 0.2(2) . . . . ? C5 C51 C56 C55 -178.39(13) . . . . ? C52 C51 C5 C6 39.1(2) . . . . ? C56 C51 C5 C6 -142.38(14) . . . . ? C52 C51 C5 C4 -134.90(14) . . . . ? C56 C51 C5 C4 43.58(18) . . . . ? C1 C21 C4 C5 -169.67(14) . . . . ? S1 C21 C4 C5 27.2(2) . . . . ? C1 C21 C4 C3 1.67(14) . . . . ? S1 C21 C4 C3 -161.47(10) . . . . ? C6 C5 C4 C21 32.4(2) . . . . ? C51 C5 C4 C21 -153.53(14) . . . . ? C6 C5 C4 C3 -137.73(14) . . . . ? C51 C5 C4 C3 36.34(18) . . . . ? N2 C3 C4 C21 -1.86(15) . . . . ? N2 C3 C4 C5 170.53(12) . . . . ? C16 N24 C19 C20 175.59(14) . . . . ? C16 N24 C19 C18 -2.62(16) . . . . ? C1 C20 C19 N24 -16.8(2) . . . . ? C201 C20 C19 N24 160.58(13) . . . . ? C1 C20 C19 C18 160.94(15) . . . . ? C201 C20 C19 C18 -21.6(2) . . . . ? C54 C53 C52 C51 -0.2(2) . . . . ? C56 C51 C52 C53 -0.3(2) . . . . ? C5 C51 C52 C53 178.20(13) . . . . ? C16 C17 C18 C19 -1.66(18) . . . . ? N24 C19 C18 C17 2.59(17) . . . . ? C20 C19 C18 C17 -175.54(15) . . . . ? C27 C26 C25 C24 0.0(2) . . . . ? C22 C23 C24 C25 0.1(2) . . . . ? C26 C25 C24 C23 0.3(2) . . . . ? N24 C16 C15 C14 4.1(2) . . . . ? C17 C16 C15 C14 -174.47(15) . . . . ? N24 C16 C15 C151 -178.67(13) . . . . ? C17 C16 C15 C151 2.8(2) . . . . ? C156 C151 C15 C14 -124.34(15) . . . . ? C152 C151 C15 C14 57.02(19) . . . . ? C156 C151 C15 C16 58.26(19) . . . . ? C152 C151 C15 C16 -120.39(15) . . . . ? C9 N22 C6 C5 172.86(13) . . . . ? C9 N22 C6 C7 -2.51(15) . . . . ? C4 C5 C6 N22 6.1(2) . . . . ? C51 C5 C6 N22 -167.70(12) . . . . ? C4 C5 C6 C7 -179.67(13) . . . . ? C51 C5 C6 C7 6.5(2) . . . . ? C8 C7 C6 N22 2.19(15) . . . . ? C8 C7 C6 C5 -172.84(14) . . . . ? C30 C29 C28 C33 -4.7(2) . . . . ? C30 C29 C28 P -175.55(12) . . . . ? C22 P C28 C29 -21.00(15) . . . . ? S2 P C28 C29 -148.91(12) . . . . ? S1 P C28 C29 89.02(13) . . . . ? C22 P C28 C33 168.11(14) . . . . ? S2 P C28 C33 40.21(16) . . . . ? S1 P C28 C33 -81.87(15) . . . . ? C29 C28 C33 C32 2.2(3) . . . . ? P C28 C33 C32 173.53(18) . . . . ? C6 N22 C9 C10 176.40(13) . . . . ? C6 N22 C9 C8 1.85(15) . . . . ? C7 C8 C9 N22 -0.41(16) . . . . ? C7 C8 C9 C10 -174.74(14) . . . . ? C30 C31 C32 C33 -4.8(3) . . . . ? C28 C33 C32 C31 2.5(3) . . . . ? C25 C26 C27 C22 -0.8(2) . . . . ? C23 C22 C27 C26 1.1(2) . . . . ? P C22 C27 C26 -178.63(11) . . . . ? N22 C9 C10 C11 -8.3(2) . . . . ? C8 C9 C10 C11 165.00(14) . . . . ? N22 C9 C10 C101 175.19(13) . . . . ? C8 C9 C10 C101 -11.5(2) . . . . ? C106 C101 C10 C11 -72.41(19) . . . . ? C102 C101 C10 C11 109.40(16) . . . . ? C106 C101 C10 C9 104.35(16) . . . . ? C102 C101 C10 C9 -73.84(18) . . . . ? C11 N23 C14 C15 177.59(13) . . . . ? C11 N23 C14 C13 -1.90(15) . . . . ? C16 C15 C14 N23 8.5(2) . . . . ? C151 C15 C14 N23 -168.73(13) . . . . ? C16 C15 C14 C13 -172.11(13) . . . . ? C151 C15 C14 C13 10.7(2) . . . . ? C12 C13 C14 N23 0.12(16) . . . . ? C12 C13 C14 C15 -179.41(13) . . . . ? C14 C13 C12 C11 1.63(15) . . . . ? C51 C56 C55 C54 0.5(2) . . . . ? C53 C54 C55 C56 -1.0(2) . . . . ? C57 C54 C55 C56 178.04(15) . . . . ? C105 C104 C103 C102 2.4(2) . . . . ? C107 C104 C103 C102 -175.08(16) . . . . ? C101 C102 C103 C104 -1.3(2) . . . . ? C14 N23 C11 C10 -172.08(14) . . . . ? C14 N23 C11 C12 2.93(15) . . . . ? C9 C10 C11 N23 2.7(2) . . . . ? C101 C10 C11 N23 179.09(13) . . . . ? C9 C10 C11 C12 -171.75(13) . . . . ? C101 C10 C11 C12 4.6(2) . . . . ? C13 C12 C11 N23 -2.95(16) . . . . ? C13 C12 C11 C10 172.39(13) . . . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.631 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.073