# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Takahiko Kojima' _publ_contact_author_email kojima@chem.tsukuba.ac.jp loop_ _publ_author_name T.Kojima T.Ishizuka M.Sankar Y.Yamada S.Fukuzumi # Attachment 'H4DPP2(ClO4)-rev2.CIF' data_sankar65 _database_code_depnum_ccdc_archive 'CCDC 866776' #TrackingRef 'H4DPP2(ClO4)-rev2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H80 Cl2 N4 O11' _chemical_formula_weight 1560.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0586(16) _cell_length_b 15.9050(18) _cell_length_c 18.483(2) _cell_angle_alpha 96.275(2) _cell_angle_beta 98.0870(10) _cell_angle_gamma 109.4310(10) _cell_volume 4075.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9576 _exptl_absorpt_correction_T_max 0.9827 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker APEXII' _diffrn_measurement_method '2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22945 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.45 _reflns_number_total 17635 _reflns_number_gt 11614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2009, 11, 0, 0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009' _computing_publication_material 'Mercury CSD 3.0.1' _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/[?^2^(Fo^2^)+(0.0956P)^2^+1.6927P] 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 17635 _refine_ls_number_parameters 963 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2060 _refine_ls_wR_factor_gt 0.1922 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 Cl1 Cl 0.20109(4) 0.34266(4) 0.45757(4) 0.03459(16) Uani 1 1 d . . . Cl2 Cl 0.12567(5) 0.32395(6) 0.08377(5) 0.0548(2) Uani 1 1 d . . . O1 O 0.27743(18) 0.3371(2) 0.42184(14) 0.0689(7) Uani 1 1 d . . . O2 O 0.2419(3) 0.4116(2) 0.52142(19) 0.0933(11) Uani 0.90 1 d P . . O3 O 0.13761(18) 0.37179(18) 0.41011(14) 0.0583(7) Uani 0.90 1 d P . . O4 O 0.1590(2) 0.2654(2) 0.4835(3) 0.1188(16) Uani 1 1 d . . . O5 O 0.1080(2) 0.2414(3) 0.1144(2) 0.1056(12) Uani 1 1 d . . . O6 O 0.1902(2) 0.32616(19) 0.03705(18) 0.0842(9) Uani 1 1 d . . . O7 O 0.1633(3) 0.3995(4) 0.1369(2) 0.170(2) Uani 1 1 d . . . O8 O 0.03818(19) 0.3204(2) 0.0460(2) 0.0950(10) Uani 1 1 d . . . N1 N 0.31274(14) 0.35170(14) 0.27816(12) 0.0305(5) Uani 1 1 d . . . H1 H 0.2719 0.3447 0.3087 0.037 Uiso 1 1 calc R . . N2 N 0.20056(14) 0.47743(14) 0.28924(13) 0.0333(5) Uani 1 1 d . . . H2 H 0.1851 0.4308 0.2536 0.040 Uiso 1 1 calc R . . N3 N 0.01904(14) 0.31778(15) 0.26949(13) 0.0353(5) Uani 1 1 d . . . H3 H 0.0723 0.3248 0.3001 0.042 Uiso 1 1 calc R . . N4 N 0.12826(14) 0.19319(14) 0.25393(13) 0.0327(5) Uani 1 1 d . . . H4 H 0.1351 0.2418 0.2335 0.039 Uiso 1 1 calc R . . C1 C 0.32684(16) 0.28248(16) 0.23642(14) 0.0279(5) Uani 1 1 d . . . C2 C 0.39254(16) 0.32224(16) 0.18901(14) 0.0284(5) Uani 1 1 d . . . C3 C 0.42126(17) 0.41587(16) 0.20878(15) 0.0293(5) Uani 1 1 d . . . C4 C 0.37126(16) 0.43401(16) 0.26582(15) 0.0294(5) Uani 1 1 d . . . C5 C 0.37402(17) 0.51658(17) 0.30351(14) 0.0305(5) Uani 1 1 d . . . C6 C 0.29173(17) 0.52579(16) 0.32712(15) 0.0306(5) Uani 1 1 d . . . C7 C 0.28448(17) 0.58956(16) 0.38466(15) 0.0311(5) Uani 1 1 d . . . C8 C 0.18922(18) 0.58341(17) 0.37603(16) 0.0338(6) Uani 1 1 d . . . C9 C 0.13693(18) 0.51222(18) 0.31494(16) 0.0354(6) Uani 1 1 d . . . C10 C 0.03818(19) 0.47785(19) 0.28230(16) 0.0390(6) Uani 1 1 d . . . C11 C -0.00831(18) 0.38775(19) 0.24883(15) 0.0352(6) Uani 1 1 d . . . C12 C -0.09447(17) 0.34653(18) 0.19307(15) 0.0318(6) Uani 1 1 d . . . C13 C -0.11949(17) 0.25391(17) 0.18596(15) 0.0313(6) Uani 1 1 d . . . C14 C -0.04804(17) 0.23597(19) 0.23574(15) 0.0345(6) Uani 1 1 d . . . C15 C -0.04342(17) 0.15265(19) 0.25160(16) 0.0362(6) Uani 1 1 d . . . C16 C 0.04495(17) 0.14162(17) 0.27374(15) 0.0322(6) Uani 1 1 d . . . C17 C 0.06785(17) 0.07514(16) 0.31291(15) 0.0312(5) Uani 1 1 d . . . C18 C 0.16239(17) 0.08548(16) 0.31025(15) 0.0304(5) Uani 1 1 d . . . C19 C 0.19922(17) 0.15847(17) 0.27040(14) 0.0299(5) Uani 1 1 d . . . C20 C 0.28723(17) 0.19100(16) 0.24605(14) 0.0281(5) Uani 1 1 d . . . C21 C 0.40986(17) 0.27347(16) 0.12369(14) 0.0287(5) Uani 1 1 d . . . C22 C 0.33277(19) 0.21142(17) 0.07205(15) 0.0345(6) Uani 1 1 d . . . H5 H 0.2693 0.1991 0.0806 0.041 Uiso 1 1 calc R . . C23 C 0.3480(2) 0.16777(19) 0.00859(16) 0.0401(6) Uani 1 1 d . . . H6 H 0.2949 0.1255 -0.0259 0.048 Uiso 1 1 calc R . . C24 C 0.4399(2) 0.1854(2) -0.00491(17) 0.0435(7) Uani 1 1 d . . . H7 H 0.4501 0.1559 -0.0489 0.052 Uiso 1 1 calc R . . C25 C 0.5167(2) 0.24595(19) 0.04578(17) 0.0397(6) Uani 1 1 d . . . H8 H 0.5800 0.2571 0.0371 0.048 Uiso 1 1 calc R . . C26 C 0.50230(19) 0.29080(18) 0.10944(16) 0.0342(6) Uani 1 1 d . . . H9 H 0.5557 0.3335 0.1434 0.041 Uiso 1 1 calc R . . C27 C 0.47582(17) 0.48546(16) 0.16823(15) 0.0303(5) Uani 1 1 d . . . C28 C 0.57496(19) 0.52308(19) 0.18291(19) 0.0450(7) Uani 1 1 d . . . H10 H 0.6107 0.5040 0.2200 0.054 Uiso 1 1 calc R . . C29 C 0.6230(2) 0.5887(2) 0.1437(2) 0.0515(8) Uani 1 1 d . . . H11 H 0.6910 0.6140 0.1542 0.062 Uiso 1 1 calc R . . C30 C 0.5722(2) 0.6165(2) 0.0903(2) 0.0534(8) Uani 1 1 d . . . H12 H 0.6049 0.6610 0.0635 0.064 Uiso 1 1 calc R . . C31 C 0.4732(3) 0.5800(3) 0.0753(2) 0.0648(10) Uani 1 1 d . . . H13 H 0.4378 0.5998 0.0386 0.078 Uiso 1 1 calc R . . C32 C 0.4256(2) 0.5144(2) 0.11389(18) 0.0506(8) Uani 1 1 d . . . H14 H 0.3575 0.4890 0.1029 0.061 Uiso 1 1 calc R . . C33 C 0.46239(18) 0.59784(17) 0.31725(15) 0.0327(6) Uani 1 1 d . . . C34 C 0.5520(2) 0.5954(2) 0.34690(17) 0.0447(7) Uani 1 1 d . . . H15 H 0.5574 0.5400 0.3576 0.054 Uiso 1 1 calc R . . C35 C 0.6330(2) 0.6732(2) 0.36076(19) 0.0537(8) Uani 1 1 d . . . H16 H 0.6934 0.6709 0.3815 0.064 Uiso 1 1 calc R . . C36 C 0.6265(2) 0.7536(2) 0.3447(2) 0.0585(9) Uani 1 1 d . . . H17 H 0.6826 0.8063 0.3529 0.070 Uiso 1 1 calc R . . C37 C 0.5384(2) 0.7576(2) 0.3166(2) 0.0608(9) Uani 1 1 d . . . H18 H 0.5335 0.8133 0.3063 0.073 Uiso 1 1 calc R . . C38 C 0.4569(2) 0.6802(2) 0.30338(18) 0.0455(7) Uani 1 1 d . . . H19 H 0.3964 0.6837 0.2845 0.055 Uiso 1 1 calc R . . C39 C 0.36316(19) 0.63928(18) 0.44837(16) 0.0374(6) Uani 1 1 d . . . C40 C 0.4172(2) 0.5936(2) 0.48246(18) 0.0464(7) Uani 1 1 d . . . H20 H 0.4017 0.5308 0.4659 0.056 Uiso 1 1 calc R . . C41 C 0.4934(2) 0.6388(3) 0.54018(18) 0.0551(8) Uani 1 1 d . . . H21 H 0.5306 0.6074 0.5627 0.066 Uiso 1 1 calc R . . C42 C 0.5150(3) 0.7287(3) 0.5648(2) 0.0719(11) Uani 1 1 d . . . H22 H 0.5688 0.7599 0.6034 0.086 Uiso 1 1 calc R . . C43 C 0.4601(3) 0.7746(3) 0.5347(2) 0.0729(11) Uani 1 1 d . . . H23 H 0.4740 0.8364 0.5539 0.087 Uiso 1 1 calc R . . C44 C 0.3835(2) 0.7297(2) 0.4754(2) 0.0566(9) Uani 1 1 d . . . H24 H 0.3456 0.7611 0.4540 0.068 Uiso 1 1 calc R . . C45 C 0.14649(18) 0.62853(17) 0.42887(17) 0.0365(6) Uani 1 1 d . . . C46 C 0.1404(3) 0.7117(2) 0.4223(3) 0.0734(11) Uani 1 1 d . . . H25 H 0.1640 0.7418 0.3835 0.088 Uiso 1 1 calc R . . C47 C 0.0994(3) 0.7521(3) 0.4731(3) 0.0849(14) Uani 1 1 d . . . H26 H 0.0945 0.8093 0.4681 0.102 Uiso 1 1 calc R . . C48 C 0.0664(3) 0.7099(3) 0.5297(3) 0.0749(12) Uani 1 1 d . . . H27 H 0.0416 0.7384 0.5657 0.090 Uiso 1 1 calc R . . C49 C 0.0699(4) 0.6278(3) 0.5330(3) 0.1042(18) Uani 1 1 d . . . H28 H 0.0439 0.5965 0.5705 0.125 Uiso 1 1 calc R . . C50 C 0.1099(3) 0.5867(3) 0.4840(2) 0.0762(12) Uani 1 1 d . . . H29 H 0.1118 0.5285 0.4887 0.091 Uiso 1 1 calc R . . C51 C -0.0177(2) 0.5400(3) 0.2846(2) 0.0617(10) Uani 1 1 d . . . C52 C 0.0134(4) 0.6206(3) 0.2581(3) 0.1006(18) Uani 1 1 d . . . H30 H 0.0720 0.6388 0.2402 0.121 Uiso 1 1 calc R . . C53 C -0.0427(7) 0.6749(5) 0.2578(4) 0.154(4) Uani 1 1 d . . . H31 H -0.0225 0.7303 0.2393 0.185 Uiso 1 1 calc R . . C54 C -0.1261(7) 0.6491(7) 0.2839(5) 0.185(5) Uani 1 1 d . . . H32 H -0.1639 0.6864 0.2824 0.222 Uiso 1 1 calc R . . C55 C -0.1566(4) 0.5710(6) 0.3122(4) 0.150(4) Uani 1 1 d . . . H33 H -0.2132 0.5555 0.3327 0.180 Uiso 1 1 calc R . . C56 C -0.1038(3) 0.5146(4) 0.3107(3) 0.0969(18) Uani 1 1 d . . . H34 H -0.1263 0.4582 0.3274 0.116 Uiso 1 1 calc R . . C57 C -0.13352(17) 0.39874(17) 0.14459(15) 0.0318(6) Uani 1 1 d . . . C58 C -0.07397(19) 0.4567(2) 0.10564(17) 0.0423(7) Uani 1 1 d . . . H35 H -0.0089 0.4610 0.1100 0.051 Uiso 1 1 calc R . . C59 C -0.1076(2) 0.5074(2) 0.06123(19) 0.0474(7) Uani 1 1 d . . . H36 H -0.0659 0.5465 0.0352 0.057 Uiso 1 1 calc R . . C60 C -0.2022(2) 0.5018(2) 0.05430(19) 0.0475(8) Uani 1 1 d . . . H37 H -0.2255 0.5375 0.0241 0.057 Uiso 1 1 calc R . . C61 C -0.2627(2) 0.4438(2) 0.0918(2) 0.0482(8) Uani 1 1 d . . . H38 H -0.3279 0.4392 0.0868 0.058 Uiso 1 1 calc R . . C62 C -0.22885(18) 0.39265(18) 0.13641(17) 0.0388(6) Uani 1 1 d . . . H39 H -0.2710 0.3530 0.1617 0.047 Uiso 1 1 calc R . . C63 C -0.19408(17) 0.18513(17) 0.12805(15) 0.0320(6) Uani 1 1 d . . . C64 C -0.29125(18) 0.16404(18) 0.12807(17) 0.0384(6) Uani 1 1 d . . . H40 H -0.3114 0.1942 0.1662 0.046 Uiso 1 1 calc R . . C65 C -0.3590(2) 0.09938(19) 0.0728(2) 0.0470(8) Uani 1 1 d . . . H41 H -0.4253 0.0851 0.0738 0.056 Uiso 1 1 calc R . . C66 C -0.3317(2) 0.0562(2) 0.0173(2) 0.0507(8) Uani 1 1 d . . . H42 H -0.3785 0.0127 -0.0209 0.061 Uiso 1 1 calc R . . C67 C -0.2348(2) 0.0760(2) 0.0168(2) 0.0554(8) Uani 1 1 d . . . H43 H -0.2152 0.0453 -0.0214 0.066 Uiso 1 1 calc R . . C68 C -0.1666(2) 0.1404(2) 0.07165(17) 0.0446(7) Uani 1 1 d . . . H44 H -0.1004 0.1540 0.0707 0.054 Uiso 1 1 calc R . . C69 C -0.1342(2) 0.0749(2) 0.2432(2) 0.0556(10) Uani 1 1 d . . . C70 C -0.2106(2) 0.0843(3) 0.2722(3) 0.0848(16) Uani 1 1 d . . . H45 H -0.2059 0.1413 0.2977 0.102 Uiso 1 1 calc R . . C71 C -0.2964(3) 0.0082(5) 0.2636(4) 0.128(3) Uani 1 1 d . . . H46 H -0.3494 0.0135 0.2837 0.154 Uiso 1 1 calc R . . C72 C -0.3019(4) -0.0749(5) 0.2251(4) 0.131(3) Uani 1 1 d . . . H47 H -0.3593 -0.1258 0.2194 0.157 Uiso 1 1 calc R . . C73 C -0.2271(4) -0.0849(3) 0.1955(3) 0.108(2) Uani 1 1 d . . . H48 H -0.2325 -0.1415 0.1689 0.130 Uiso 1 1 calc R . . C74 C -0.1423(3) -0.0101(3) 0.2052(2) 0.0723(12) Uani 1 1 d . . . H49 H -0.0892 -0.0165 0.1859 0.087 Uiso 1 1 calc R . . C75 C 0.00451(17) 0.01682(16) 0.35563(14) 0.0296(5) Uani 1 1 d . . . C76 C -0.04364(17) 0.05316(17) 0.40165(15) 0.0335(6) Uani 1 1 d . . . H50 H -0.0342 0.1157 0.4062 0.040 Uiso 1 1 calc R . . C77 C -0.10550(18) -0.00095(18) 0.44115(16) 0.0363(6) Uani 1 1 d . . . H51 H -0.1398 0.0240 0.4712 0.044 Uiso 1 1 calc R . . C78 C -0.11667(19) -0.09128(18) 0.43625(16) 0.0374(6) Uani 1 1 d . . . H52 H -0.1582 -0.1285 0.4635 0.045 Uiso 1 1 calc R . . C79 C -0.0678(2) -0.12734(18) 0.39199(17) 0.0411(7) Uani 1 1 d . . . H53 H -0.0752 -0.1894 0.3892 0.049 Uiso 1 1 calc R . . C80 C -0.0082(2) -0.07437(17) 0.35171(16) 0.0382(6) Uani 1 1 d . . . H54 H 0.0246 -0.1003 0.3209 0.046 Uiso 1 1 calc R . . C81 C 0.22181(18) 0.04515(17) 0.35603(16) 0.0338(6) Uani 1 1 d . . . C82 C 0.2276(2) -0.0391(2) 0.3334(2) 0.0559(9) Uani 1 1 d . . . H55 H 0.1922 -0.0739 0.2867 0.067 Uiso 1 1 calc R . . C83 C 0.2848(3) -0.0722(2) 0.3787(2) 0.0676(11) Uani 1 1 d . . . H56 H 0.2906 -0.1284 0.3621 0.081 Uiso 1 1 calc R . . C84 C 0.3334(2) -0.0242(3) 0.4479(2) 0.0601(10) Uani 1 1 d . . . H57 H 0.3705 -0.0483 0.4795 0.072 Uiso 1 1 calc R . . C85 C 0.3278(2) 0.0579(3) 0.4705(2) 0.0579(9) Uani 1 1 d . . . H58 H 0.3620 0.0914 0.5177 0.069 Uiso 1 1 calc R . . C86 C 0.2725(2) 0.0931(2) 0.42494(17) 0.0433(7) Uani 1 1 d . . . H59 H 0.2695 0.1507 0.4413 0.052 Uiso 1 1 calc R . . C87 C 0.33932(18) 0.12832(17) 0.22944(14) 0.0306(5) Uani 1 1 d . . . C88 C 0.2888(2) 0.0407(2) 0.19182(18) 0.0458(7) Uani 1 1 d . . . H60 H 0.2211 0.0208 0.1769 0.055 Uiso 1 1 calc R . . C89 C 0.3366(3) -0.0174(2) 0.1762(2) 0.0576(9) Uani 1 1 d . . . H61 H 0.3016 -0.0773 0.1510 0.069 Uiso 1 1 calc R . . C90 C 0.4352(3) 0.0107(2) 0.1970(2) 0.0584(9) Uani 1 1 d . . . H62 H 0.4677 -0.0298 0.1863 0.070 Uiso 1 1 calc R . . C91 C 0.4865(2) 0.0984(2) 0.23347(19) 0.0500(8) Uani 1 1 d . . . H63 H 0.5543 0.1183 0.2476 0.060 Uiso 1 1 calc R . . C92 C 0.43810(19) 0.15682(19) 0.24917(16) 0.0374(6) Uani 1 1 d . . . H64 H 0.4732 0.2170 0.2737 0.045 Uiso 1 1 calc R . . O9 O 0.1125(11) 0.2826(11) 0.3977(9) 0.026(3) Uiso 0.10 1 d P . . O10 O 0.1948(13) 0.4214(12) 0.4721(11) 0.035(4) Uiso 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 Cl1 0.0324(3) 0.0402(4) 0.0364(4) 0.0129(3) 0.0052(3) 0.0181(3) Cl2 0.0397(4) 0.0822(6) 0.0483(5) 0.0243(4) 0.0079(3) 0.0249(4) O1 0.0621(15) 0.114(2) 0.0606(15) 0.0335(15) 0.0299(13) 0.0562(16) O2 0.102(3) 0.095(2) 0.069(2) -0.0295(18) -0.0295(19) 0.049(2) O3 0.0599(16) 0.0721(17) 0.0508(15) 0.0108(13) -0.0074(12) 0.0406(14) O4 0.0752(19) 0.089(2) 0.248(5) 0.118(3) 0.088(3) 0.0508(17) O5 0.100(2) 0.136(3) 0.107(3) 0.084(2) 0.032(2) 0.050(2) O6 0.095(2) 0.0812(19) 0.119(2) 0.0568(19) 0.0685(19) 0.0541(17) O7 0.106(3) 0.248(6) 0.089(3) -0.084(3) 0.013(2) 0.012(3) O8 0.0481(15) 0.084(2) 0.143(3) 0.024(2) -0.0166(17) 0.0232(14) N1 0.0237(10) 0.0302(11) 0.0384(12) 0.0067(9) 0.0093(9) 0.0090(9) N2 0.0244(10) 0.0311(11) 0.0393(13) -0.0047(10) -0.0007(9) 0.0094(9) N3 0.0207(10) 0.0429(13) 0.0413(13) 0.0101(10) -0.0016(9) 0.0119(9) N4 0.0226(10) 0.0312(11) 0.0450(13) 0.0192(10) 0.0037(9) 0.0074(9) C1 0.0230(11) 0.0266(12) 0.0347(14) 0.0063(10) 0.0034(10) 0.0101(10) C2 0.0221(11) 0.0284(12) 0.0353(14) 0.0082(11) 0.0035(10) 0.0095(10) C3 0.0215(11) 0.0280(12) 0.0385(14) 0.0074(11) 0.0038(10) 0.0090(10) C4 0.0196(11) 0.0280(12) 0.0395(14) 0.0071(11) 0.0030(10) 0.0075(10) C5 0.0248(12) 0.0295(13) 0.0352(14) 0.0051(11) 0.0023(10) 0.0084(10) C6 0.0264(12) 0.0262(12) 0.0373(14) 0.0047(11) 0.0011(11) 0.0091(10) C7 0.0282(12) 0.0234(12) 0.0410(15) 0.0047(11) 0.0040(11) 0.0095(10) C8 0.0296(13) 0.0252(12) 0.0458(16) 0.0044(11) 0.0029(11) 0.0111(10) C9 0.0280(13) 0.0367(14) 0.0424(16) 0.0048(12) 0.0033(11) 0.0144(11) C10 0.0292(13) 0.0434(15) 0.0436(16) -0.0016(13) -0.0020(12) 0.0181(12) C11 0.0229(12) 0.0447(15) 0.0385(15) 0.0073(12) 0.0033(11) 0.0134(11) C12 0.0193(11) 0.0396(14) 0.0357(14) 0.0051(12) 0.0028(10) 0.0108(10) C13 0.0200(11) 0.0369(14) 0.0359(14) 0.0104(11) 0.0022(10) 0.0085(10) C14 0.0207(12) 0.0446(15) 0.0407(15) 0.0157(13) 0.0054(11) 0.0122(11) C15 0.0210(12) 0.0429(15) 0.0435(16) 0.0194(13) 0.0028(11) 0.0073(11) C16 0.0236(12) 0.0339(13) 0.0354(14) 0.0134(11) 0.0023(10) 0.0044(10) C17 0.0266(12) 0.0264(12) 0.0368(14) 0.0066(11) 0.0021(11) 0.0056(10) C18 0.0257(12) 0.0260(12) 0.0381(14) 0.0091(11) 0.0038(11) 0.0072(10) C19 0.0243(12) 0.0298(12) 0.0334(14) 0.0065(11) 0.0012(10) 0.0078(10) C20 0.0237(12) 0.0276(12) 0.0315(13) 0.0064(10) 0.0023(10) 0.0077(10) C21 0.0289(12) 0.0266(12) 0.0358(14) 0.0123(11) 0.0085(11) 0.0133(10) C22 0.0298(13) 0.0334(14) 0.0414(15) 0.0083(12) 0.0058(11) 0.0125(11) C23 0.0439(16) 0.0351(14) 0.0405(16) 0.0063(12) 0.0028(13) 0.0151(12) C24 0.0551(18) 0.0419(16) 0.0416(17) 0.0080(13) 0.0135(14) 0.0253(14) C25 0.0385(15) 0.0411(15) 0.0486(17) 0.0159(14) 0.0166(13) 0.0196(13) C26 0.0296(13) 0.0348(14) 0.0404(15) 0.0109(12) 0.0078(11) 0.0123(11) C27 0.0280(12) 0.0243(12) 0.0391(14) 0.0066(11) 0.0079(11) 0.0090(10) C28 0.0295(14) 0.0398(15) 0.069(2) 0.0247(15) 0.0103(14) 0.0111(12) C29 0.0329(15) 0.0413(16) 0.081(2) 0.0233(17) 0.0175(16) 0.0078(13) C30 0.0527(19) 0.0413(17) 0.067(2) 0.0242(16) 0.0218(17) 0.0083(15) C31 0.053(2) 0.068(2) 0.067(2) 0.040(2) 0.0005(17) 0.0084(17) C32 0.0332(15) 0.0555(19) 0.056(2) 0.0241(16) 0.0004(14) 0.0048(14) C33 0.0255(12) 0.0324(13) 0.0356(14) 0.0035(11) 0.0040(11) 0.0056(10) C34 0.0309(14) 0.0504(17) 0.0511(18) 0.0125(15) 0.0031(13) 0.0129(13) C35 0.0274(15) 0.069(2) 0.053(2) 0.0108(17) -0.0016(13) 0.0051(14) C36 0.0397(17) 0.052(2) 0.063(2) 0.0069(17) 0.0030(16) -0.0075(15) C37 0.0487(19) 0.0414(18) 0.086(3) 0.0172(18) 0.0127(18) 0.0059(15) C38 0.0348(15) 0.0418(16) 0.0577(19) 0.0153(15) 0.0066(14) 0.0093(12) C39 0.0297(13) 0.0358(14) 0.0419(16) 0.0011(12) 0.0024(12) 0.0088(11) C40 0.0417(16) 0.0481(17) 0.0477(18) 0.0049(14) 0.0011(14) 0.0176(14) C41 0.0398(17) 0.072(2) 0.0455(19) -0.0021(17) -0.0064(14) 0.0185(16) C42 0.050(2) 0.090(3) 0.053(2) -0.008(2) -0.0101(17) 0.010(2) C43 0.067(2) 0.049(2) 0.077(3) -0.0186(19) -0.005(2) 0.0043(18) C44 0.0501(19) 0.0345(16) 0.073(2) -0.0061(16) -0.0044(17) 0.0105(14) C45 0.0275(13) 0.0274(13) 0.0499(17) -0.0033(12) -0.0015(12) 0.0101(10) C46 0.093(3) 0.050(2) 0.093(3) 0.015(2) 0.030(2) 0.040(2) C47 0.091(3) 0.051(2) 0.118(4) -0.016(2) 0.002(3) 0.049(2) C48 0.056(2) 0.068(3) 0.099(3) -0.010(2) 0.025(2) 0.024(2) C49 0.153(5) 0.080(3) 0.112(4) 0.017(3) 0.083(4) 0.060(3) C50 0.114(3) 0.056(2) 0.084(3) 0.018(2) 0.055(3) 0.046(2) C51 0.053(2) 0.070(2) 0.060(2) -0.0231(18) -0.0208(16) 0.0427(18) C52 0.128(4) 0.069(3) 0.110(4) -0.010(3) -0.029(3) 0.071(3) C53 0.205(8) 0.110(5) 0.148(6) -0.045(4) -0.074(6) 0.119(6) C54 0.167(7) 0.190(8) 0.185(8) -0.120(7) -0.117(6) 0.155(7) C55 0.085(4) 0.190(7) 0.163(6) -0.100(6) -0.036(4) 0.098(5) C56 0.051(2) 0.137(4) 0.094(3) -0.057(3) -0.012(2) 0.056(3) C57 0.0237(12) 0.0305(13) 0.0375(14) 0.0006(11) -0.0016(11) 0.0093(10) C58 0.0273(14) 0.0481(17) 0.0504(18) 0.0127(14) 0.0043(12) 0.0117(12) C59 0.0369(15) 0.0420(16) 0.059(2) 0.0181(15) 0.0066(14) 0.0065(13) C60 0.0415(16) 0.0381(15) 0.065(2) 0.0206(15) 0.0019(14) 0.0162(13) C61 0.0277(14) 0.0455(17) 0.075(2) 0.0204(16) 0.0035(14) 0.0171(13) C62 0.0254(13) 0.0344(14) 0.0557(18) 0.0126(13) 0.0040(12) 0.0094(11) C63 0.0252(12) 0.0288(12) 0.0416(15) 0.0136(11) -0.0002(11) 0.0091(10) C64 0.0251(13) 0.0307(13) 0.0568(18) 0.0091(13) 0.0028(12) 0.0081(11) C65 0.0271(14) 0.0326(15) 0.076(2) 0.0134(15) -0.0016(14) 0.0061(12) C66 0.0390(16) 0.0314(15) 0.065(2) 0.0034(15) -0.0134(15) 0.0021(13) C67 0.0505(19) 0.0492(19) 0.061(2) 0.0004(16) 0.0022(16) 0.0160(15) C68 0.0305(14) 0.0487(17) 0.0517(18) 0.0072(15) 0.0010(13) 0.0132(13) C69 0.0241(14) 0.065(2) 0.071(2) 0.0459(19) -0.0033(14) 0.0017(14) C70 0.0299(16) 0.118(3) 0.129(4) 0.096(3) 0.021(2) 0.0294(19) C71 0.0279(19) 0.179(6) 0.194(7) 0.153(6) 0.013(3) 0.022(3) C72 0.055(3) 0.140(5) 0.153(6) 0.118(5) -0.030(3) -0.033(3) C73 0.087(3) 0.084(3) 0.091(3) 0.051(3) -0.039(3) -0.040(3) C74 0.059(2) 0.055(2) 0.066(2) 0.0275(19) -0.0252(18) -0.0184(17) C75 0.0224(12) 0.0295(12) 0.0352(14) 0.0101(11) 0.0018(10) 0.0071(10) C76 0.0255(12) 0.0266(12) 0.0472(16) 0.0103(12) 0.0025(11) 0.0083(10) C77 0.0286(13) 0.0382(15) 0.0435(16) 0.0094(13) 0.0079(12) 0.0124(11) C78 0.0304(13) 0.0332(14) 0.0444(16) 0.0154(12) 0.0058(12) 0.0034(11) C79 0.0448(16) 0.0251(13) 0.0505(18) 0.0098(12) 0.0082(14) 0.0076(12) C80 0.0409(15) 0.0283(13) 0.0445(16) 0.0052(12) 0.0117(13) 0.0099(11) C81 0.0274(13) 0.0318(13) 0.0442(16) 0.0150(12) 0.0086(11) 0.0098(11) C82 0.061(2) 0.0346(16) 0.071(2) 0.0117(16) -0.0020(17) 0.0203(15) C83 0.074(2) 0.0460(19) 0.094(3) 0.029(2) 0.007(2) 0.0341(18) C84 0.0510(19) 0.065(2) 0.078(3) 0.040(2) 0.0093(18) 0.0309(17) C85 0.0516(19) 0.079(2) 0.052(2) 0.0194(18) 0.0024(16) 0.0350(18) C86 0.0406(16) 0.0504(17) 0.0458(17) 0.0146(14) 0.0061(13) 0.0239(14) C87 0.0309(13) 0.0281(12) 0.0339(14) 0.0070(11) 0.0046(11) 0.0120(10) C88 0.0436(16) 0.0381(15) 0.0537(19) 0.0049(14) 0.0037(14) 0.0151(13) C89 0.072(2) 0.0399(17) 0.060(2) -0.0024(16) 0.0049(18) 0.0250(17) C90 0.072(2) 0.055(2) 0.065(2) 0.0071(17) 0.0144(18) 0.0447(19) C91 0.0421(17) 0.0556(19) 0.061(2) 0.0173(16) 0.0114(15) 0.0253(15) C92 0.0334(14) 0.0389(15) 0.0427(16) 0.0085(13) 0.0065(12) 0.0161(12) _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 Cl1 O10 1.289(18) . ? Cl1 O4 1.356(2) . ? Cl1 O1 1.426(2) . ? Cl1 O2 1.428(3) . ? Cl1 O3 1.430(2) . ? Cl1 O9 1.556(16) . ? Cl2 O7 1.364(4) . ? Cl2 O8 1.382(3) . ? Cl2 O6 1.382(3) . ? Cl2 O5 1.445(3) . ? O2 O10 1.131(19) . ? O3 O10 1.32(2) . ? O3 O9 1.324(16) . ? O4 O9 1.730(16) . ? N1 C1 1.367(3) . ? N1 C4 1.377(3) . ? N2 C9 1.369(3) . ? N2 C6 1.370(3) . ? N3 C14 1.369(3) . ? N3 C11 1.381(3) . ? N4 C19 1.370(3) . ? N4 C16 1.375(3) . ? C1 C20 1.419(3) . ? C1 C2 1.448(3) . ? C2 C3 1.395(3) . ? C2 C21 1.465(4) . ? C3 C4 1.436(4) . ? C3 C27 1.487(3) . ? C4 C5 1.403(4) . ? C5 C6 1.416(4) . ? C5 C33 1.481(3) . ? C6 C7 1.429(4) . ? C7 C8 1.390(3) . ? C7 C39 1.482(4) . ? C8 C9 1.433(4) . ? C8 C45 1.488(4) . ? C9 C10 1.417(4) . ? C10 C11 1.394(4) . ? C10 C51 1.496(4) . ? C11 C12 1.444(4) . ? C12 C13 1.380(4) . ? C12 C57 1.476(3) . ? C13 C14 1.438(3) . ? C13 C63 1.481(4) . ? C14 C15 1.410(4) . ? C15 C16 1.410(3) . ? C15 C69 1.482(4) . ? C16 C17 1.449(3) . ? C17 C18 1.386(3) . ? C17 C75 1.475(3) . ? C18 C19 1.439(3) . ? C18 C81 1.489(3) . ? C19 C20 1.410(3) . ? C20 C87 1.492(3) . ? C21 C26 1.395(3) . ? C21 C22 1.397(4) . ? C22 C23 1.383(4) . ? C23 C24 1.383(4) . ? C24 C25 1.379(4) . ? C25 C26 1.390(4) . ? C27 C32 1.383(4) . ? C27 C28 1.384(4) . ? C28 C29 1.395(4) . ? C29 C30 1.365(5) . ? C30 C31 1.381(5) . ? C31 C32 1.386(4) . ? C33 C38 1.389(4) . ? C33 C34 1.398(4) . ? C34 C35 1.388(4) . ? C35 C36 1.376(5) . ? C36 C37 1.379(5) . ? C37 C38 1.387(4) . ? C39 C44 1.385(4) . ? C39 C40 1.392(4) . ? C40 C41 1.382(4) . ? C41 C42 1.365(5) . ? C42 C43 1.374(6) . ? C43 C44 1.402(5) . ? C45 C50 1.359(5) . ? C45 C46 1.373(4) . ? C46 C47 1.405(6) . ? C47 C48 1.366(6) . ? C48 C49 1.333(6) . ? C49 C50 1.377(5) . ? C51 C52 1.382(6) . ? C51 C56 1.395(6) . ? C52 C53 1.394(7) . ? C53 C54 1.360(13) . ? C54 C55 1.363(14) . ? C55 C56 1.384(7) . ? C57 C62 1.391(3) . ? C57 C58 1.396(4) . ? C58 C59 1.372(4) . ? C59 C60 1.385(4) . ? C60 C61 1.385(4) . ? C61 C62 1.381(4) . ? C63 C68 1.386(4) . ? C63 C64 1.388(4) . ? C64 C65 1.386(4) . ? C65 C66 1.359(5) . ? C66 C67 1.388(5) . ? C67 C68 1.382(4) . ? C69 C70 1.380(5) . ? C69 C74 1.412(6) . ? C70 C71 1.421(6) . ? C71 C72 1.402(10) . ? C72 C73 1.367(10) . ? C73 C74 1.399(5) . ? C75 C76 1.389(4) . ? C75 C80 1.391(4) . ? C76 C77 1.392(4) . ? C77 C78 1.381(4) . ? C78 C79 1.374(4) . ? C79 C80 1.375(4) . ? C81 C86 1.383(4) . ? C81 C82 1.395(4) . ? C82 C83 1.384(4) . ? C83 C84 1.380(6) . ? C84 C85 1.360(5) . ? C85 C86 1.390(4) . ? C87 C92 1.383(4) . ? C87 C88 1.393(4) . ? C88 C89 1.377(4) . ? C89 C90 1.383(5) . ? C90 C91 1.388(5) . ? C91 C92 1.389(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Cl1 O4 130.0(8) . . ? O10 Cl1 O1 117.1(8) . . ? O4 Cl1 O1 111.41(18) . . ? O10 Cl1 O2 48.9(9) . . ? O4 Cl1 O2 105.7(3) . . ? O1 Cl1 O2 107.5(2) . . ? O10 Cl1 O3 57.9(9) . . ? O4 Cl1 O3 115.46(19) . . ? O1 Cl1 O3 109.71(15) . . ? O2 Cl1 O3 106.51(18) . . ? O10 Cl1 O9 108.2(10) . . ? O4 Cl1 O9 72.5(6) . . ? O1 Cl1 O9 100.8(6) . . ? O2 Cl1 O9 149.7(6) . . ? O3 Cl1 O9 52.4(6) . . ? O7 Cl2 O8 109.4(3) . . ? O7 Cl2 O6 108.7(2) . . ? O8 Cl2 O6 111.9(2) . . ? O7 Cl2 O5 112.7(3) . . ? O8 Cl2 O5 106.52(19) . . ? O6 Cl2 O5 107.54(19) . . ? O10 O2 Cl1 59.1(10) . . ? O10 O3 O9 121.5(10) . . ? O10 O3 Cl1 55.7(8) . . ? O9 O3 Cl1 68.7(7) . . ? Cl1 O4 O9 59.1(5) . . ? C1 N1 C4 110.6(2) . . ? C9 N2 C6 110.1(2) . . ? C14 N3 C11 110.7(2) . . ? C19 N4 C16 110.7(2) . . ? N1 C1 C20 122.8(2) . . ? N1 C1 C2 107.3(2) . . ? C20 C1 C2 129.7(2) . . ? C3 C2 C1 106.9(2) . . ? C3 C2 C21 126.4(2) . . ? C1 C2 C21 125.6(2) . . ? C2 C3 C4 107.8(2) . . ? C2 C3 C27 126.9(2) . . ? C4 C3 C27 124.1(2) . . ? N1 C4 C5 122.6(2) . . ? N1 C4 C3 107.1(2) . . ? C5 C4 C3 130.2(2) . . ? C4 C5 C6 121.2(2) . . ? C4 C5 C33 120.8(2) . . ? C6 C5 C33 118.0(2) . . ? N2 C6 C5 122.5(2) . . ? N2 C6 C7 107.2(2) . . ? C5 C6 C7 129.9(2) . . ? C8 C7 C6 107.9(2) . . ? C8 C7 C39 127.6(2) . . ? C6 C7 C39 123.6(2) . . ? C7 C8 C9 106.8(2) . . ? C7 C8 C45 126.3(2) . . ? C9 C8 C45 125.8(2) . . ? N2 C9 C10 121.7(2) . . ? N2 C9 C8 107.7(2) . . ? C10 C9 C8 130.6(2) . . ? C11 C10 C9 121.8(2) . . ? C11 C10 C51 119.3(2) . . ? C9 C10 C51 118.9(3) . . ? N3 C11 C10 123.6(2) . . ? N3 C11 C12 106.2(2) . . ? C10 C11 C12 130.0(2) . . ? C13 C12 C11 108.1(2) . . ? C13 C12 C57 128.2(2) . . ? C11 C12 C57 122.8(2) . . ? C12 C13 C14 107.5(2) . . ? C12 C13 C63 126.7(2) . . ? C14 C13 C63 124.7(2) . . ? N3 C14 C15 123.1(2) . . ? N3 C14 C13 107.2(2) . . ? C15 C14 C13 129.6(2) . . ? C16 C15 C14 121.6(2) . . ? C16 C15 C69 119.8(2) . . ? C14 C15 C69 118.6(2) . . ? N4 C16 C15 122.4(2) . . ? N4 C16 C17 106.6(2) . . ? C15 C16 C17 130.8(2) . . ? C18 C17 C16 107.4(2) . . ? C18 C17 C75 127.4(2) . . ? C16 C17 C75 124.7(2) . . ? C17 C18 C19 107.7(2) . . ? C17 C18 C81 125.5(2) . . ? C19 C18 C81 125.1(2) . . ? N4 C19 C20 121.8(2) . . ? N4 C19 C18 107.1(2) . . ? C20 C19 C18 131.0(2) . . ? C19 C20 C1 121.0(2) . . ? C19 C20 C87 119.7(2) . . ? C1 C20 C87 119.3(2) . . ? C26 C21 C22 118.4(2) . . ? C26 C21 C2 121.3(2) . . ? C22 C21 C2 120.2(2) . . ? C23 C22 C21 120.7(2) . . ? C24 C23 C22 120.4(3) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 120.3(3) . . ? C32 C27 C28 118.5(2) . . ? C32 C27 C3 118.7(2) . . ? C28 C27 C3 122.8(2) . . ? C27 C28 C29 120.7(3) . . ? C30 C29 C28 120.0(3) . . ? C29 C30 C31 120.0(3) . . ? C30 C31 C32 120.0(3) . . ? C27 C32 C31 120.8(3) . . ? C38 C33 C34 118.2(3) . . ? C38 C33 C5 119.9(2) . . ? C34 C33 C5 121.9(2) . . ? C35 C34 C33 120.4(3) . . ? C36 C35 C34 120.5(3) . . ? C35 C36 C37 119.8(3) . . ? C36 C37 C38 120.0(3) . . ? C37 C38 C33 121.0(3) . . ? C44 C39 C40 119.2(3) . . ? C44 C39 C7 121.7(3) . . ? C40 C39 C7 119.1(2) . . ? C41 C40 C39 120.5(3) . . ? C42 C41 C40 119.8(3) . . ? C41 C42 C43 120.9(3) . . ? C42 C43 C44 119.6(3) . . ? C39 C44 C43 119.8(3) . . ? C50 C45 C46 118.2(3) . . ? C50 C45 C8 120.3(3) . . ? C46 C45 C8 121.4(3) . . ? C45 C46 C47 119.8(4) . . ? C48 C47 C46 120.6(4) . . ? C49 C48 C47 118.2(4) . . ? C48 C49 C50 122.2(5) . . ? C45 C50 C49 120.8(4) . . ? C52 C51 C56 119.7(4) . . ? C52 C51 C10 120.3(4) . . ? C56 C51 C10 119.9(4) . . ? C51 C52 C53 118.9(7) . . ? C54 C53 C52 120.4(8) . . ? C53 C54 C55 121.6(6) . . ? C54 C55 C56 119.0(8) . . ? C55 C56 C51 120.4(7) . . ? C62 C57 C58 118.2(2) . . ? C62 C57 C12 122.0(2) . . ? C58 C57 C12 119.8(2) . . ? C59 C58 C57 121.3(3) . . ? C58 C59 C60 120.1(3) . . ? C59 C60 C61 119.5(3) . . ? C62 C61 C60 120.4(3) . . ? C61 C62 C57 120.6(3) . . ? C68 C63 C64 118.6(3) . . ? C68 C63 C13 119.3(2) . . ? C64 C63 C13 122.1(3) . . ? C65 C64 C63 120.5(3) . . ? C66 C65 C64 120.7(3) . . ? C65 C66 C67 119.5(3) . . ? C68 C67 C66 120.3(3) . . ? C67 C68 C63 120.4(3) . . ? C70 C69 C74 119.7(3) . . ? C70 C69 C15 120.9(4) . . ? C74 C69 C15 119.4(3) . . ? C69 C70 C71 119.5(5) . . ? C72 C71 C70 119.2(5) . . ? C73 C72 C71 121.9(4) . . ? C72 C73 C74 118.7(6) . . ? C73 C74 C69 121.1(5) . . ? C76 C75 C80 118.4(2) . . ? C76 C75 C17 119.8(2) . . ? C80 C75 C17 121.8(2) . . ? C75 C76 C77 120.8(2) . . ? C78 C77 C76 119.5(3) . . ? C79 C78 C77 120.1(2) . . ? C78 C79 C80 120.5(2) . . ? C79 C80 C75 120.7(3) . . ? C86 C81 C82 118.5(3) . . ? C86 C81 C18 118.2(2) . . ? C82 C81 C18 123.2(3) . . ? C83 C82 C81 120.1(3) . . ? C84 C83 C82 120.6(3) . . ? C85 C84 C83 119.6(3) . . ? C84 C85 C86 120.6(3) . . ? C81 C86 C85 120.6(3) . . ? C92 C87 C88 119.1(2) . . ? C92 C87 C20 120.8(2) . . ? C88 C87 C20 120.0(2) . . ? C89 C88 C87 120.2(3) . . ? C88 C89 C90 120.6(3) . . ? C89 C90 C91 119.7(3) . . ? C90 C91 C92 119.6(3) . . ? C87 C92 C91 120.7(3) . . ? O3 O9 Cl1 58.9(7) . . ? O3 O9 O4 100.1(10) . . ? Cl1 O9 O4 48.4(5) . . ? O2 O10 Cl1 72.0(10) . . ? O2 O10 O3 137.8(16) . . ? Cl1 O10 O3 66.4(9) . . ? 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 O4 Cl1 O2 O10 -129.9(11) . . . . ? O1 Cl1 O2 O10 111.0(11) . . . . ? O3 Cl1 O2 O10 -6.5(11) . . . . ? O9 Cl1 O2 O10 -47.7(16) . . . . ? O4 Cl1 O3 O10 122.8(10) . . . . ? O1 Cl1 O3 O10 -110.3(10) . . . . ? O2 Cl1 O3 O10 5.8(10) . . . . ? O9 Cl1 O3 O10 161.1(12) . . . . ? O10 Cl1 O3 O9 -161.1(12) . . . . ? O4 Cl1 O3 O9 -38.3(8) . . . . ? O1 Cl1 O3 O9 88.6(8) . . . . ? O2 Cl1 O3 O9 -155.3(8) . . . . ? O10 Cl1 O4 O9 99.4(13) . . . . ? O1 Cl1 O4 O9 -95.0(6) . . . . ? O2 Cl1 O4 O9 148.4(6) . . . . ? O3 Cl1 O4 O9 31.0(6) . . . . ? C4 N1 C1 C20 170.2(2) . . . . ? C4 N1 C1 C2 -5.3(3) . . . . ? N1 C1 C2 C3 4.5(3) . . . . ? C20 C1 C2 C3 -170.6(2) . . . . ? N1 C1 C2 C21 -164.5(2) . . . . ? C20 C1 C2 C21 20.3(4) . . . . ? C1 C2 C3 C4 -2.1(3) . . . . ? C21 C2 C3 C4 166.9(2) . . . . ? C1 C2 C3 C27 -169.5(2) . . . . ? C21 C2 C3 C27 -0.5(4) . . . . ? C1 N1 C4 C5 -177.6(2) . . . . ? C1 N1 C4 C3 4.0(3) . . . . ? C2 C3 C4 N1 -1.0(3) . . . . ? C27 C3 C4 N1 166.8(2) . . . . ? C2 C3 C4 C5 -179.2(2) . . . . ? C27 C3 C4 C5 -11.4(4) . . . . ? N1 C4 C5 C6 -31.3(4) . . . . ? C3 C4 C5 C6 146.6(3) . . . . ? N1 C4 C5 C33 151.1(2) . . . . ? C3 C4 C5 C33 -31.0(4) . . . . ? C9 N2 C6 C5 -167.7(2) . . . . ? C9 N2 C6 C7 5.5(3) . . . . ? C4 C5 C6 N2 -31.5(4) . . . . ? C33 C5 C6 N2 146.2(2) . . . . ? C4 C5 C6 C7 157.0(3) . . . . ? C33 C5 C6 C7 -25.3(4) . . . . ? N2 C6 C7 C8 -5.1(3) . . . . ? C5 C6 C7 C8 167.4(3) . . . . ? N2 C6 C7 C39 164.9(2) . . . . ? C5 C6 C7 C39 -22.5(4) . . . . ? C6 C7 C8 C9 2.8(3) . . . . ? C39 C7 C8 C9 -166.7(2) . . . . ? C6 C7 C8 C45 171.6(2) . . . . ? C39 C7 C8 C45 2.0(4) . . . . ? C6 N2 C9 C10 176.4(2) . . . . ? C6 N2 C9 C8 -3.8(3) . . . . ? C7 C8 C9 N2 0.5(3) . . . . ? C45 C8 C9 N2 -168.3(2) . . . . ? C7 C8 C9 C10 -179.7(3) . . . . ? C45 C8 C9 C10 11.5(5) . . . . ? N2 C9 C10 C11 29.9(4) . . . . ? C8 C9 C10 C11 -149.9(3) . . . . ? N2 C9 C10 C51 -150.7(3) . . . . ? C8 C9 C10 C51 29.5(5) . . . . ? C14 N3 C11 C10 170.3(3) . . . . ? C14 N3 C11 C12 -5.4(3) . . . . ? C9 C10 C11 N3 28.6(4) . . . . ? C51 C10 C11 N3 -150.8(3) . . . . ? C9 C10 C11 C12 -156.9(3) . . . . ? C51 C10 C11 C12 23.8(5) . . . . ? N3 C11 C12 C13 4.1(3) . . . . ? C10 C11 C12 C13 -171.1(3) . . . . ? N3 C11 C12 C57 -165.3(2) . . . . ? C10 C11 C12 C57 19.4(5) . . . . ? C11 C12 C13 C14 -1.5(3) . . . . ? C57 C12 C13 C14 167.2(2) . . . . ? C11 C12 C13 C63 -170.3(2) . . . . ? C57 C12 C13 C63 -1.6(4) . . . . ? C11 N3 C14 C15 -174.1(3) . . . . ? C11 N3 C14 C13 4.5(3) . . . . ? C12 C13 C14 N3 -1.8(3) . . . . ? C63 C13 C14 N3 167.3(2) . . . . ? C12 C13 C14 C15 176.7(3) . . . . ? C63 C13 C14 C15 -14.1(5) . . . . ? N3 C14 C15 C16 -30.4(4) . . . . ? C13 C14 C15 C16 151.2(3) . . . . ? N3 C14 C15 C69 150.7(3) . . . . ? C13 C14 C15 C69 -27.6(5) . . . . ? C19 N4 C16 C15 -168.8(3) . . . . ? C19 N4 C16 C17 6.5(3) . . . . ? C14 C15 C16 N4 -26.7(4) . . . . ? C69 C15 C16 N4 152.1(3) . . . . ? C14 C15 C16 C17 159.2(3) . . . . ? C69 C15 C16 C17 -22.0(5) . . . . ? N4 C16 C17 C18 -4.2(3) . . . . ? C15 C16 C17 C18 170.5(3) . . . . ? N4 C16 C17 C75 168.3(2) . . . . ? C15 C16 C17 C75 -16.9(5) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? C75 C17 C18 C19 -171.8(3) . . . . ? C16 C17 C18 C81 166.5(3) . . . . ? C75 C17 C18 C81 -5.9(4) . . . . ? C16 N4 C19 C20 170.7(2) . . . . ? C16 N4 C19 C18 -6.2(3) . . . . ? C17 C18 C19 N4 3.3(3) . . . . ? C81 C18 C19 N4 -162.7(3) . . . . ? C17 C18 C19 C20 -173.2(3) . . . . ? C81 C18 C19 C20 20.8(5) . . . . ? N4 C19 C20 C1 30.9(4) . . . . ? C18 C19 C20 C1 -153.0(3) . . . . ? N4 C19 C20 C87 -148.6(2) . . . . ? C18 C19 C20 C87 27.6(4) . . . . ? N1 C1 C20 C19 30.8(4) . . . . ? C2 C1 C20 C19 -154.8(3) . . . . ? N1 C1 C20 C87 -149.8(2) . . . . ? C2 C1 C20 C87 24.6(4) . . . . ? C3 C2 C21 C26 55.2(3) . . . . ? C1 C2 C21 C26 -137.9(2) . . . . ? C3 C2 C21 C22 -121.5(3) . . . . ? C1 C2 C21 C22 45.4(3) . . . . ? C26 C21 C22 C23 0.5(4) . . . . ? C2 C21 C22 C23 177.3(2) . . . . ? C21 C22 C23 C24 -0.4(4) . . . . ? C22 C23 C24 C25 0.8(4) . . . . ? C23 C24 C25 C26 -1.4(4) . . . . ? C24 C25 C26 C21 1.5(4) . . . . ? C22 C21 C26 C25 -1.0(4) . . . . ? C2 C21 C26 C25 -177.8(2) . . . . ? C2 C3 C27 C32 89.5(3) . . . . ? C4 C3 C27 C32 -75.9(4) . . . . ? C2 C3 C27 C28 -90.9(4) . . . . ? C4 C3 C27 C28 103.6(3) . . . . ? C32 C27 C28 C29 0.0(5) . . . . ? C3 C27 C28 C29 -179.5(3) . . . . ? C27 C28 C29 C30 0.1(5) . . . . ? C28 C29 C30 C31 0.3(6) . . . . ? C29 C30 C31 C32 -0.7(6) . . . . ? C28 C27 C32 C31 -0.4(5) . . . . ? C3 C27 C32 C31 179.1(3) . . . . ? C30 C31 C32 C27 0.8(6) . . . . ? C4 C5 C33 C38 133.9(3) . . . . ? C6 C5 C33 C38 -43.8(4) . . . . ? C4 C5 C33 C34 -48.7(4) . . . . ? C6 C5 C33 C34 133.6(3) . . . . ? C38 C33 C34 C35 -1.0(5) . . . . ? C5 C33 C34 C35 -178.4(3) . . . . ? C33 C34 C35 C36 -0.8(5) . . . . ? C34 C35 C36 C37 1.9(6) . . . . ? C35 C36 C37 C38 -1.2(6) . . . . ? C36 C37 C38 C33 -0.7(6) . . . . ? C34 C33 C38 C37 1.7(5) . . . . ? C5 C33 C38 C37 179.2(3) . . . . ? C8 C7 C39 C44 -52.3(4) . . . . ? C6 C7 C39 C44 139.7(3) . . . . ? C8 C7 C39 C40 126.9(3) . . . . ? C6 C7 C39 C40 -41.1(4) . . . . ? C44 C39 C40 C41 -3.2(5) . . . . ? C7 C39 C40 C41 177.6(3) . . . . ? C39 C40 C41 C42 1.0(5) . . . . ? C40 C41 C42 C43 2.2(6) . . . . ? C41 C42 C43 C44 -3.0(6) . . . . ? C40 C39 C44 C43 2.4(5) . . . . ? C7 C39 C44 C43 -178.4(3) . . . . ? C42 C43 C44 C39 0.7(6) . . . . ? C7 C8 C45 C50 -89.4(4) . . . . ? C9 C8 C45 C50 77.3(4) . . . . ? C7 C8 C45 C46 92.4(4) . . . . ? C9 C8 C45 C46 -100.9(4) . . . . ? C50 C45 C46 C47 1.6(6) . . . . ? C8 C45 C46 C47 179.8(3) . . . . ? C45 C46 C47 C48 0.8(7) . . . . ? C46 C47 C48 C49 -3.3(7) . . . . ? C47 C48 C49 C50 3.4(9) . . . . ? C46 C45 C50 C49 -1.6(7) . . . . ? C8 C45 C50 C49 -179.8(4) . . . . ? C48 C49 C50 C45 -1.0(9) . . . . ? C11 C10 C51 C52 -126.5(4) . . . . ? C9 C10 C51 C52 54.1(5) . . . . ? C11 C10 C51 C56 50.6(5) . . . . ? C9 C10 C51 C56 -128.8(3) . . . . ? C56 C51 C52 C53 -0.1(7) . . . . ? C10 C51 C52 C53 177.0(4) . . . . ? C51 C52 C53 C54 0.5(9) . . . . ? C52 C53 C54 C55 1.2(11) . . . . ? C53 C54 C55 C56 -3.4(11) . . . . ? C54 C55 C56 C51 3.8(8) . . . . ? C52 C51 C56 C55 -2.1(6) . . . . ? C10 C51 C56 C55 -179.2(4) . . . . ? C13 C12 C57 C62 64.2(4) . . . . ? C11 C12 C57 C62 -128.6(3) . . . . ? C13 C12 C57 C58 -116.1(3) . . . . ? C11 C12 C57 C58 51.1(4) . . . . ? C62 C57 C58 C59 0.9(4) . . . . ? C12 C57 C58 C59 -178.8(3) . . . . ? C57 C58 C59 C60 0.0(5) . . . . ? C58 C59 C60 C61 -0.8(5) . . . . ? C59 C60 C61 C62 0.7(5) . . . . ? C60 C61 C62 C57 0.2(5) . . . . ? C58 C57 C62 C61 -1.0(4) . . . . ? C12 C57 C62 C61 178.7(3) . . . . ? C12 C13 C63 C68 105.5(3) . . . . ? C14 C13 C63 C68 -61.5(4) . . . . ? C12 C13 C63 C64 -74.2(4) . . . . ? C14 C13 C63 C64 118.8(3) . . . . ? C68 C63 C64 C65 0.2(4) . . . . ? C13 C63 C64 C65 179.9(2) . . . . ? C63 C64 C65 C66 -0.7(4) . . . . ? C64 C65 C66 C67 1.2(5) . . . . ? C65 C66 C67 C68 -1.1(5) . . . . ? C66 C67 C68 C63 0.6(5) . . . . ? C64 C63 C68 C67 -0.1(4) . . . . ? C13 C63 C68 C67 -179.8(3) . . . . ? C16 C15 C69 C70 134.0(3) . . . . ? C14 C15 C69 C70 -47.1(4) . . . . ? C16 C15 C69 C74 -45.8(4) . . . . ? C14 C15 C69 C74 133.1(3) . . . . ? C74 C69 C70 C71 0.2(5) . . . . ? C15 C69 C70 C71 -179.6(3) . . . . ? C69 C70 C71 C72 -0.6(6) . . . . ? C70 C71 C72 C73 0.0(7) . . . . ? C71 C72 C73 C74 1.1(7) . . . . ? C72 C73 C74 C69 -1.5(6) . . . . ? C70 C69 C74 C73 0.9(5) . . . . ? C15 C69 C74 C73 -179.3(3) . . . . ? C18 C17 C75 C76 128.2(3) . . . . ? C16 C17 C75 C76 -42.9(4) . . . . ? C18 C17 C75 C80 -51.4(4) . . . . ? C16 C17 C75 C80 137.5(3) . . . . ? C80 C75 C76 C77 -2.0(4) . . . . ? C17 C75 C76 C77 178.5(2) . . . . ? C75 C76 C77 C78 2.1(4) . . . . ? C76 C77 C78 C79 -0.7(4) . . . . ? C77 C78 C79 C80 -0.6(4) . . . . ? C78 C79 C80 C75 0.7(4) . . . . ? C76 C75 C80 C79 0.6(4) . . . . ? C17 C75 C80 C79 -179.9(3) . . . . ? C17 C18 C81 C86 -87.9(3) . . . . ? C19 C18 C81 C86 75.6(4) . . . . ? C17 C18 C81 C82 91.0(4) . . . . ? C19 C18 C81 C82 -105.5(3) . . . . ? C86 C81 C82 C83 -1.4(5) . . . . ? C18 C81 C82 C83 179.6(3) . . . . ? C81 C82 C83 C84 2.7(6) . . . . ? C82 C83 C84 C85 -2.4(6) . . . . ? C83 C84 C85 C86 0.9(5) . . . . ? C82 C81 C86 C85 -0.1(4) . . . . ? C18 C81 C86 C85 178.9(3) . . . . ? C84 C85 C86 C81 0.3(5) . . . . ? C19 C20 C87 C92 -140.2(3) . . . . ? C1 C20 C87 C92 40.3(4) . . . . ? C19 C20 C87 C88 41.6(4) . . . . ? C1 C20 C87 C88 -137.9(3) . . . . ? C92 C87 C88 C89 1.6(4) . . . . ? C20 C87 C88 C89 179.9(3) . . . . ? C87 C88 C89 C90 -0.6(5) . . . . ? C88 C89 C90 C91 -0.4(6) . . . . ? C89 C90 C91 C92 0.4(5) . . . . ? C88 C87 C92 C91 -1.6(4) . . . . ? C20 C87 C92 C91 -179.8(3) . . . . ? C90 C91 C92 C87 0.6(5) . . . . ? O10 O3 O9 Cl1 -18.3(11) . . . . ? O10 O3 O9 O4 8.1(14) . . . . ? Cl1 O3 O9 O4 26.4(4) . . . . ? O10 Cl1 O9 O3 16.8(11) . . . . ? O4 Cl1 O9 O3 144.1(6) . . . . ? O1 Cl1 O9 O3 -106.6(5) . . . . ? O2 Cl1 O9 O3 52.7(13) . . . . ? O10 Cl1 O9 O4 -127.3(9) . . . . ? O1 Cl1 O9 O4 109.2(3) . . . . ? O2 Cl1 O9 O4 -91.4(11) . . . . ? O3 Cl1 O9 O4 -144.1(6) . . . . ? Cl1 O4 O9 O3 -30.6(6) . . . . ? Cl1 O2 O10 O3 10.1(17) . . . . ? O4 Cl1 O10 O2 74.7(12) . . . . ? O1 Cl1 O10 O2 -90.2(9) . . . . ? O3 Cl1 O10 O2 172.6(12) . . . . ? O9 Cl1 O10 O2 156.9(8) . . . . ? O4 Cl1 O10 O3 -97.8(9) . . . . ? O1 Cl1 O10 O3 97.3(6) . . . . ? O2 Cl1 O10 O3 -172.6(12) . . . . ? O9 Cl1 O10 O3 -15.7(10) . . . . ? O9 O3 O10 O2 10(3) . . . . ? Cl1 O3 O10 O2 -10.5(17) . . . . ? O9 O3 O10 Cl1 20.7(13) . . . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.801 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.058 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 0.000 919 151 ' ' _platon_squeeze_details 'A THF, an EtOH and a water molecules per asymmetric unit were deleted with the squeeze program' data_ishi7 _database_code_depnum_ccdc_archive 'CCDC 866777' #TrackingRef 'H4DCDPP2(ClO4)-rev2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H103 Cl2 N4 O18.50' _chemical_formula_weight 1811.83 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 20.917(4) _cell_length_b 21.983(4) _cell_length_c 22.099(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.546(2) _cell_angle_gamma 90.00 _cell_volume 9168(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3820 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9442 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker APEXII' _diffrn_measurement_method '2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32702 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 21.97 _reflns_number_total 11141 _reflns_number_gt 6604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2009, 11, 0, 0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009' _computing_publication_material 'Mercury CSD 3.0.1' _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^)+(0.1188P)^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 11141 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2090 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 N1 N 0.25624(18) 0.45776(14) 0.46501(15) 0.0310(9) Uani 1 1 d . . . H1 H 0.2755 0.4302 0.4966 0.037 Uiso 1 1 calc R . . N2 N 0.20583(19) 0.32739(14) 0.44682(16) 0.0325(9) Uani 1 1 d . . . H2 H 0.1820 0.3559 0.4562 0.039 Uiso 1 1 calc R . . N3 N 0.21015(19) 0.33479(14) 0.58469(15) 0.0334(9) Uani 1 1 d . . . H3 H 0.2407 0.3517 0.5721 0.040 Uiso 1 1 calc R . . N4 N 0.25464(19) 0.46517(14) 0.59961(16) 0.0344(9) Uani 1 1 d . . . H4 H 0.2213 0.4488 0.5634 0.041 Uiso 1 1 calc R . . C1 C 0.2515(2) 0.51855(18) 0.4762(2) 0.0323(11) Uani 1 1 d . . . C2 C 0.2108(2) 0.54591(17) 0.41292(19) 0.0311(11) Uani 1 1 d . . . C3 C 0.1953(2) 0.50245(17) 0.36474(19) 0.0307(10) Uani 1 1 d . . . C4 C 0.2264(2) 0.44622(18) 0.39709(19) 0.0304(10) Uani 1 1 d . . . C5 C 0.2342(2) 0.39004(18) 0.3708(2) 0.0340(11) Uani 1 1 d . . . C6 C 0.2390(2) 0.33478(18) 0.4060(2) 0.0337(11) Uani 1 1 d . . . C7 C 0.2755(2) 0.27993(17) 0.4070(2) 0.0316(11) Uani 1 1 d . . . C8 C 0.2605(2) 0.23885(17) 0.4467(2) 0.0336(11) Uani 1 1 d . . . C9 C 0.2150(2) 0.26922(17) 0.4710(2) 0.0317(11) Uani 1 1 d . . . C10 C 0.1833(2) 0.24634(17) 0.5111(2) 0.0318(10) Uani 1 1 d . . . C11 C 0.1702(2) 0.28344(17) 0.5558(2) 0.0332(11) Uani 1 1 d . . . C12 C 0.1234(2) 0.27514(17) 0.58640(19) 0.0300(10) Uani 1 1 d . . . C13 C 0.1384(2) 0.31903(17) 0.63551(19) 0.0310(10) Uani 1 1 d . . . C14 C 0.1953(2) 0.35526(18) 0.6353(2) 0.0339(11) Uani 1 1 d . . . C15 C 0.2350(2) 0.40187(18) 0.68082(19) 0.0322(11) Uani 1 1 d . . . C16 C 0.2714(2) 0.44632(18) 0.66390(19) 0.0315(11) Uani 1 1 d . . . C17 C 0.3314(2) 0.48174(17) 0.70672(19) 0.0320(11) Uani 1 1 d . . . C18 C 0.3467(2) 0.52271(17) 0.66724(19) 0.0316(11) Uani 1 1 d . . . C19 C 0.2967(2) 0.51302(17) 0.5991(2) 0.0307(10) Uani 1 1 d . . . C20 C 0.2856(2) 0.54465(17) 0.5410(2) 0.0327(11) Uani 1 1 d . . . C21 C 0.1818(2) 0.60904(19) 0.4054(2) 0.0378(11) Uani 1 1 d . . . C22 C 0.1390(3) 0.6246(2) 0.4353(3) 0.0555(14) Uani 1 1 d . . . H5 H 0.1279 0.5954 0.4609 0.067 Uiso 1 1 calc R . . C23 C 0.1115(3) 0.6837(3) 0.4281(3) 0.0732(17) Uani 1 1 d . . . H6 H 0.0807 0.6943 0.4479 0.088 Uiso 1 1 calc R . . C24 C 0.1293(4) 0.7264(2) 0.3921(3) 0.0720(18) Uani 1 1 d . . . H7 H 0.1122 0.7669 0.3884 0.086 Uiso 1 1 calc R . . C25 C 0.1701(4) 0.7110(2) 0.3627(3) 0.0772(19) Uani 1 1 d . . . H8 H 0.1811 0.7403 0.3370 0.093 Uiso 1 1 calc R . . C26 C 0.1968(3) 0.65297(19) 0.3686(3) 0.0568(15) Uani 1 1 d . . . H9 H 0.2260 0.6429 0.3471 0.068 Uiso 1 1 calc R . . C27 C 0.1435(2) 0.50697(18) 0.2924(2) 0.0366(11) Uani 1 1 d . . . C28 C 0.1536(3) 0.5472(2) 0.2489(2) 0.0517(14) Uani 1 1 d . . . H10 H 0.1949 0.5717 0.2641 0.062 Uiso 1 1 calc R . . C29 C 0.1029(3) 0.5512(2) 0.1833(2) 0.0662(16) Uani 1 1 d . . . H11 H 0.1100 0.5787 0.1536 0.079 Uiso 1 1 calc R . . C30 C 0.0426(4) 0.5163(3) 0.1602(3) 0.0807(19) Uani 1 1 d . . . H12 H 0.0082 0.5196 0.1149 0.097 Uiso 1 1 calc R . . C31 C 0.0325(3) 0.4764(3) 0.2034(3) 0.0746(17) Uani 1 1 d . . . H13 H -0.0091 0.4521 0.1881 0.090 Uiso 1 1 calc R . . C32 C 0.0828(3) 0.4718(2) 0.2691(2) 0.0532(14) Uani 1 1 d . . . H14 H 0.0756 0.4441 0.2986 0.064 Uiso 1 1 calc R . . C33 C 0.2389(2) 0.38854(18) 0.3066(2) 0.0323(11) Uani 1 1 d . . . C34 C 0.2723(2) 0.43563(19) 0.2886(2) 0.0389(12) Uani 1 1 d . . . H15 H 0.2935 0.4680 0.3193 0.047 Uiso 1 1 calc R . . C35 C 0.2753(3) 0.4363(2) 0.2278(2) 0.0438(12) Uani 1 1 d . . . H16 H 0.2964 0.4697 0.2158 0.053 Uiso 1 1 calc R . . C36 C 0.2472(3) 0.3878(2) 0.1839(2) 0.0416(12) Uani 1 1 d . . . C37 C 0.2164(3) 0.34088(19) 0.2013(2) 0.0449(13) Uani 1 1 d . . . H17 H 0.1981 0.3074 0.1716 0.054 Uiso 1 1 calc R . . C38 C 0.2111(2) 0.34110(18) 0.2616(2) 0.0382(11) Uani 1 1 d . . . H18 H 0.1882 0.3083 0.2722 0.046 Uiso 1 1 calc R . . C39 C 0.2504(3) 0.3896(2) 0.1175(2) 0.0477(13) Uani 1 1 d . . . C40 C 0.3310(3) 0.27359(19) 0.3827(2) 0.0376(11) Uani 1 1 d . . . C41 C 0.3891(3) 0.3105(2) 0.4081(3) 0.0578(14) Uani 1 1 d . . . H19 H 0.3929 0.3401 0.4409 0.069 Uiso 1 1 calc R . . C42 C 0.4422(3) 0.3060(3) 0.3874(4) 0.0793(19) Uani 1 1 d . . . H20 H 0.4814 0.3332 0.4043 0.095 Uiso 1 1 calc R . . C43 C 0.4378(4) 0.2628(3) 0.3430(4) 0.087(2) Uani 1 1 d . . . H21 H 0.4752 0.2588 0.3296 0.105 Uiso 1 1 calc R . . C44 C 0.3806(4) 0.2238(2) 0.3161(3) 0.0729(18) Uani 1 1 d . . . H22 H 0.3780 0.1940 0.2840 0.087 Uiso 1 1 calc R . . C45 C 0.3275(3) 0.2291(2) 0.3367(2) 0.0523(14) Uani 1 1 d . . . H23 H 0.2882 0.2021 0.3194 0.063 Uiso 1 1 calc R . . C46 C 0.2957(2) 0.17973(18) 0.4719(2) 0.0397(12) Uani 1 1 d . . . C47 C 0.2865(3) 0.1309(2) 0.4288(3) 0.0535(14) Uani 1 1 d . . . H24 H 0.2583 0.1354 0.3820 0.064 Uiso 1 1 calc R . . C48 C 0.3189(4) 0.0755(2) 0.4546(5) 0.086(2) Uani 1 1 d . . . H25 H 0.3145 0.0426 0.4251 0.103 Uiso 1 1 calc R . . C49 C 0.3570(4) 0.0681(3) 0.5223(5) 0.100(3) Uani 1 1 d . . . H26 H 0.3780 0.0298 0.5397 0.120 Uiso 1 1 calc R . . C50 C 0.3654(3) 0.1160(3) 0.5657(4) 0.090(2) Uani 1 1 d . . . H27 H 0.3917 0.1109 0.6127 0.108 Uiso 1 1 calc R . . C51 C 0.3349(3) 0.1708(2) 0.5397(3) 0.0610(15) Uani 1 1 d . . . H28 H 0.3411 0.2039 0.5694 0.073 Uiso 1 1 calc R . . C52 C 0.1694(3) 0.18098(19) 0.5091(3) 0.0489(13) Uani 1 1 d . . . C53 C 0.1406(3) 0.1502(2) 0.4488(3) 0.0687(17) Uani 1 1 d . . . H29 H 0.1260 0.1716 0.4077 0.082 Uiso 1 1 calc R . . C54 C 0.1332(4) 0.0866(3) 0.4493(5) 0.106(3) Uani 1 1 d . . . H30 H 0.1127 0.0654 0.4078 0.127 Uiso 1 1 calc R . . C55 C 0.1539(6) 0.0553(4) 0.5059(8) 0.148(6) Uani 1 1 d . . . H31 H 0.1495 0.0123 0.5050 0.177 Uiso 1 1 calc R . . C56 C 0.1813(5) 0.0853(4) 0.5647(6) 0.131(4) Uani 1 1 d . . . H32 H 0.1956 0.0626 0.6050 0.158 Uiso 1 1 calc R . . C57 C 0.1898(3) 0.1491(2) 0.5689(3) 0.0721(18) Uani 1 1 d . . . H33 H 0.2087 0.1694 0.6109 0.086 Uiso 1 1 calc R . . C58 C 0.0599(2) 0.23437(18) 0.5597(2) 0.0375(11) Uani 1 1 d . . . C59 C 0.0086(3) 0.2438(2) 0.4955(2) 0.0458(12) Uani 1 1 d . . . H34 H 0.0154 0.2741 0.4682 0.055 Uiso 1 1 calc R . . C60 C -0.0520(3) 0.2099(2) 0.4708(3) 0.0620(15) Uani 1 1 d . . . H35 H -0.0875 0.2171 0.4267 0.074 Uiso 1 1 calc R . . C61 C -0.0620(3) 0.1651(2) 0.5096(3) 0.0669(16) Uani 1 1 d . . . H36 H -0.1042 0.1414 0.4921 0.080 Uiso 1 1 calc R . . C62 C -0.0118(3) 0.1549(2) 0.5725(3) 0.0661(16) Uani 1 1 d . . . H37 H -0.0184 0.1242 0.5995 0.079 Uiso 1 1 calc R . . C63 C 0.0497(3) 0.1900(2) 0.5974(2) 0.0535(14) Uani 1 1 d . . . H38 H 0.0851 0.1827 0.6416 0.064 Uiso 1 1 calc R . . C64 C 0.0974(2) 0.33313(19) 0.6737(2) 0.0354(11) Uani 1 1 d . . . C65 C 0.0614(3) 0.3876(2) 0.6624(2) 0.0499(13) Uani 1 1 d . . . H39 H 0.0630 0.4148 0.6296 0.060 Uiso 1 1 calc R . . C66 C 0.0232(3) 0.4036(3) 0.6974(3) 0.0728(17) Uani 1 1 d . . . H40 H -0.0013 0.4413 0.6888 0.087 Uiso 1 1 calc R . . C67 C 0.0209(3) 0.3648(3) 0.7447(3) 0.0758(19) Uani 1 1 d . . . H41 H -0.0048 0.3756 0.7696 0.091 Uiso 1 1 calc R . . C68 C 0.0557(3) 0.3100(3) 0.7561(3) 0.0726(17) Uani 1 1 d . . . H42 H 0.0532 0.2827 0.7883 0.087 Uiso 1 1 calc R . . C69 C 0.0944(3) 0.2945(2) 0.7212(2) 0.0520(13) Uani 1 1 d . . . H43 H 0.1191 0.2568 0.7301 0.062 Uiso 1 1 calc R . . C70 C 0.2374(2) 0.40141(19) 0.7480(2) 0.0360(11) Uani 1 1 d . . . C71 C 0.2202(3) 0.4517(2) 0.7745(2) 0.0529(14) Uani 1 1 d . . . H44 H 0.2077 0.4885 0.7495 0.063 Uiso 1 1 calc R . . C72 C 0.2207(3) 0.4496(2) 0.8379(2) 0.0585(15) Uani 1 1 d . . . H45 H 0.2071 0.4843 0.8550 0.070 Uiso 1 1 calc R . . C73 C 0.2410(3) 0.3976(2) 0.8751(2) 0.0456(13) Uani 1 1 d . . . C74 C 0.2597(3) 0.3468(2) 0.8503(2) 0.0451(12) Uani 1 1 d . . . H46 H 0.2733 0.3106 0.8761 0.054 Uiso 1 1 calc R . . C75 C 0.2584(3) 0.3491(2) 0.7876(2) 0.0429(12) Uani 1 1 d . . . H47 H 0.2722 0.3142 0.7708 0.051 Uiso 1 1 calc R . . C76 C 0.2426(3) 0.3936(2) 0.9431(3) 0.0540(14) Uani 1 1 d . . . C77 C 0.3771(2) 0.46891(19) 0.7779(2) 0.0386(12) Uani 1 1 d . . . C78 C 0.4103(3) 0.4133(2) 0.7963(2) 0.0534(14) Uani 1 1 d . . . H48 H 0.4030 0.3831 0.7631 0.064 Uiso 1 1 calc R . . C79 C 0.4538(3) 0.4014(2) 0.8621(3) 0.0664(16) Uani 1 1 d . . . H49 H 0.4766 0.3630 0.8742 0.080 Uiso 1 1 calc R . . C80 C 0.4649(3) 0.4434(3) 0.9102(3) 0.0636(15) Uani 1 1 d . . . H50 H 0.4948 0.4341 0.9557 0.076 Uiso 1 1 calc R . . C81 C 0.4337(3) 0.4986(3) 0.8937(2) 0.0667(16) Uani 1 1 d . . . H51 H 0.4425 0.5284 0.9276 0.080 Uiso 1 1 calc R . . C82 C 0.3883(3) 0.5121(2) 0.8264(2) 0.0596(15) Uani 1 1 d . . . H52 H 0.3656 0.5507 0.8147 0.071 Uiso 1 1 calc R . . C83 C 0.4125(2) 0.55907(18) 0.6906(2) 0.0337(11) Uani 1 1 d . . . C84 C 0.4237(3) 0.6094(2) 0.7302(2) 0.0515(14) Uani 1 1 d . . . H53 H 0.3865 0.6245 0.7399 0.062 Uiso 1 1 calc R . . C85 C 0.4897(3) 0.6392(2) 0.7567(3) 0.0615(15) Uani 1 1 d . . . H54 H 0.4971 0.6742 0.7842 0.074 Uiso 1 1 calc R . . C86 C 0.5420(3) 0.6182(3) 0.7430(3) 0.0645(15) Uani 1 1 d . . . H55 H 0.5868 0.6378 0.7615 0.077 Uiso 1 1 calc R . . C87 C 0.5312(3) 0.5690(3) 0.7025(3) 0.085(2) Uani 1 1 d . . . H56 H 0.5683 0.5548 0.6923 0.102 Uiso 1 1 calc R . . C88 C 0.4664(3) 0.5395(2) 0.6763(3) 0.0658(16) Uani 1 1 d . . . H57 H 0.4594 0.5052 0.6480 0.079 Uiso 1 1 calc R . . C89 C 0.3103(3) 0.60796(18) 0.5462(2) 0.0384(12) Uani 1 1 d . . . C90 C 0.2982(3) 0.6495(2) 0.5861(2) 0.0634(16) Uani 1 1 d . . . H58 H 0.2738 0.6375 0.6118 0.076 Uiso 1 1 calc R . . C91 C 0.3217(4) 0.7098(2) 0.5895(3) 0.087(2) Uani 1 1 d . . . H59 H 0.3140 0.7383 0.6179 0.105 Uiso 1 1 calc R . . C92 C 0.3554(4) 0.7273(3) 0.5519(4) 0.098(3) Uani 1 1 d . . . H60 H 0.3694 0.7685 0.5530 0.118 Uiso 1 1 calc R . . C93 C 0.3693(4) 0.6876(3) 0.5137(3) 0.082(2) Uani 1 1 d . . . H61 H 0.3951 0.7001 0.4895 0.098 Uiso 1 1 calc R . . C94 C 0.3458(3) 0.6280(2) 0.5093(2) 0.0574(15) Uani 1 1 d . . . H62 H 0.3541 0.6003 0.4805 0.069 Uiso 1 1 calc R . . O1 O 0.2640(2) 0.43883(15) 0.09747(17) 0.0686(11) Uani 1 1 d . . . O2 O 0.2383(2) 0.34056(14) 0.08577(16) 0.0699(12) Uani 1 1 d . . . H63 H 0.2413 0.3459 0.0494 0.105 Uiso 1 1 calc R . . O3 O 0.2517(2) 0.34478(17) 0.97266(16) 0.0692(11) Uani 1 1 d . . . O4 O 0.2367(3) 0.44360(18) 0.96911(18) 0.0928(15) Uani 1 1 d . . . H64 H 0.2382 0.4369 1.0072 0.139 Uiso 1 1 calc R . . O5 O 0.4365(3) 0.3845(3) 0.6565(3) 0.172(3) Uani 1 1 d . . . O6 O 0.3985(7) 0.4074(5) 0.5579(6) 0.136(4) Uani 0.50 1 d P . . O7 O 0.4450(3) 0.3146(2) 0.5860(3) 0.1233(18) Uani 1 1 d . . . O8 O 0.3384(7) 0.3370(12) 0.5714(11) 0.193(11) Uani 0.50 1 d P . . O9 O 0.3358(9) 0.3685(6) 0.5589(7) 0.121(7) Uani 0.50 1 d P . . O10 O 0.0059(3) 0.4700(2) 0.4055(3) 0.149(2) Uani 1 1 d . . . O11 O 0.1157(4) 0.4690(4) 0.4953(4) 0.243(5) Uani 1 1 d . . . O12 O 0.0244(5) 0.4026(3) 0.4924(4) 0.220(4) Uani 1 1 d . . . O13 O 0.0723(3) 0.3843(2) 0.4187(3) 0.129(2) Uani 1 1 d . . . Cl1 Cl 0.40259(9) 0.35270(7) 0.60309(8) 0.0711(5) Uani 1 1 d . . . Cl2 Cl 0.05755(11) 0.43378(10) 0.45649(11) 0.1107(7) Uani 1 1 d . . . O14 O 0.3729(8) 0.3114(6) 0.6456(8) 0.140(4) Uani 0.50 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 N1 0.050(2) 0.026(2) 0.0209(19) 0.0061(15) 0.0193(18) 0.0015(17) N2 0.051(3) 0.028(2) 0.0261(19) -0.0049(16) 0.0239(19) 0.0017(17) N3 0.051(3) 0.035(2) 0.0218(19) -0.0005(17) 0.0231(19) -0.0072(18) N4 0.046(2) 0.039(2) 0.021(2) -0.0087(17) 0.0174(18) -0.0118(18) C1 0.047(3) 0.032(3) 0.027(3) 0.000(2) 0.025(2) -0.006(2) C2 0.049(3) 0.030(2) 0.021(2) 0.003(2) 0.021(2) 0.001(2) C3 0.044(3) 0.036(2) 0.017(2) 0.002(2) 0.017(2) -0.004(2) C4 0.038(3) 0.035(3) 0.017(2) 0.004(2) 0.012(2) -0.002(2) C5 0.045(3) 0.034(2) 0.027(2) -0.002(2) 0.020(2) -0.005(2) C6 0.044(3) 0.040(3) 0.023(2) -0.005(2) 0.021(2) -0.002(2) C7 0.039(3) 0.033(2) 0.031(2) -0.006(2) 0.023(2) -0.002(2) C8 0.045(3) 0.033(2) 0.030(2) -0.010(2) 0.022(2) -0.004(2) C9 0.044(3) 0.030(2) 0.025(2) -0.001(2) 0.019(2) -0.001(2) C10 0.036(3) 0.035(2) 0.028(2) -0.002(2) 0.018(2) -0.004(2) C11 0.047(3) 0.029(2) 0.031(2) 0.002(2) 0.024(2) -0.001(2) C12 0.036(3) 0.034(2) 0.021(2) 0.007(2) 0.013(2) -0.001(2) C13 0.041(3) 0.034(2) 0.021(2) 0.006(2) 0.016(2) 0.000(2) C14 0.046(3) 0.038(2) 0.022(2) 0.006(2) 0.018(2) 0.003(2) C15 0.046(3) 0.032(2) 0.023(2) 0.004(2) 0.019(2) -0.001(2) C16 0.043(3) 0.039(2) 0.016(2) -0.002(2) 0.016(2) 0.004(2) C17 0.046(3) 0.032(2) 0.019(2) -0.003(2) 0.015(2) 0.001(2) C18 0.045(3) 0.030(2) 0.019(2) 0.000(2) 0.013(2) 0.000(2) C19 0.039(3) 0.029(2) 0.028(3) -0.006(2) 0.018(2) 0.000(2) C20 0.047(3) 0.029(2) 0.025(2) 0.000(2) 0.017(2) 0.001(2) C21 0.043(3) 0.039(3) 0.024(2) 0.001(2) 0.008(2) 0.009(2) C22 0.060(4) 0.052(3) 0.059(3) -0.007(3) 0.031(3) 0.003(3) C23 0.060(4) 0.075(4) 0.083(4) -0.034(4) 0.029(4) 0.007(3) C24 0.102(5) 0.032(3) 0.066(4) 0.000(3) 0.022(4) 0.020(3) C25 0.117(6) 0.045(3) 0.065(4) 0.003(3) 0.035(4) 0.017(3) C26 0.086(4) 0.031(3) 0.056(3) 0.004(3) 0.032(3) 0.009(3) C27 0.048(3) 0.034(2) 0.027(3) -0.004(2) 0.016(2) 0.007(2) C28 0.076(4) 0.047(3) 0.031(3) 0.006(2) 0.022(3) -0.009(3) C29 0.094(5) 0.059(3) 0.032(3) 0.011(3) 0.013(3) -0.005(3) C30 0.102(6) 0.069(4) 0.041(3) 0.006(3) 0.003(4) -0.003(4) C31 0.074(4) 0.069(4) 0.053(4) -0.009(3) 0.000(3) -0.020(3) C32 0.061(4) 0.051(3) 0.040(3) 0.003(3) 0.015(3) -0.012(3) C33 0.048(3) 0.032(2) 0.024(2) 0.000(2) 0.022(2) 0.006(2) C34 0.055(3) 0.037(3) 0.036(3) -0.004(2) 0.030(3) -0.002(2) C35 0.067(4) 0.043(3) 0.033(3) 0.004(2) 0.031(3) -0.008(2) C36 0.065(4) 0.044(3) 0.024(3) 0.003(2) 0.028(3) 0.004(2) C37 0.070(4) 0.035(3) 0.029(3) -0.007(2) 0.021(3) 0.001(2) C38 0.051(3) 0.034(2) 0.032(3) 0.000(2) 0.020(2) -0.005(2) C39 0.073(4) 0.039(3) 0.034(3) 0.001(3) 0.026(3) 0.008(3) C40 0.050(3) 0.035(2) 0.036(3) 0.000(2) 0.027(3) 0.000(2) C41 0.068(4) 0.051(3) 0.073(4) -0.008(3) 0.047(3) -0.004(3) C42 0.066(4) 0.069(4) 0.133(6) -0.011(4) 0.071(5) -0.008(3) C43 0.113(6) 0.063(4) 0.139(6) 0.009(4) 0.105(6) 0.015(4) C44 0.123(6) 0.049(3) 0.085(4) -0.009(3) 0.080(5) 0.005(4) C45 0.073(4) 0.049(3) 0.058(3) -0.015(3) 0.051(3) -0.005(3) C46 0.042(3) 0.030(2) 0.052(3) -0.002(2) 0.026(3) 0.004(2) C47 0.064(4) 0.040(3) 0.067(4) -0.008(3) 0.038(3) -0.004(3) C48 0.088(6) 0.034(3) 0.159(7) -0.009(4) 0.076(6) 0.003(3) C49 0.078(6) 0.053(4) 0.170(9) 0.041(6) 0.055(6) 0.024(4) C50 0.075(5) 0.070(4) 0.100(5) 0.040(4) 0.017(4) 0.028(4) C51 0.062(4) 0.056(3) 0.057(4) 0.007(3) 0.019(3) 0.004(3) C52 0.061(4) 0.031(3) 0.077(4) -0.006(3) 0.050(3) -0.005(2) C53 0.076(4) 0.049(3) 0.115(5) -0.025(3) 0.072(4) -0.023(3) C54 0.130(7) 0.057(5) 0.187(9) -0.059(5) 0.122(7) -0.038(5) C55 0.149(9) 0.045(5) 0.327(18) -0.027(7) 0.176(12) -0.013(5) C56 0.148(9) 0.062(5) 0.241(12) 0.078(6) 0.138(9) 0.034(5) C57 0.097(5) 0.046(3) 0.104(5) 0.033(3) 0.072(4) 0.016(3) C58 0.047(3) 0.039(3) 0.035(3) -0.006(2) 0.026(3) -0.006(2) C59 0.057(4) 0.050(3) 0.030(3) -0.009(2) 0.018(3) -0.009(3) C60 0.056(4) 0.075(4) 0.046(3) -0.014(3) 0.013(3) -0.019(3) C61 0.067(4) 0.068(4) 0.069(4) -0.029(3) 0.032(4) -0.032(3) C62 0.090(5) 0.058(3) 0.057(4) -0.004(3) 0.039(4) -0.023(3) C63 0.055(4) 0.066(3) 0.037(3) 0.004(3) 0.017(3) -0.028(3) C64 0.041(3) 0.044(3) 0.027(2) -0.003(2) 0.020(2) -0.009(2) C65 0.059(4) 0.058(3) 0.042(3) -0.005(3) 0.031(3) -0.003(3) C66 0.067(4) 0.090(4) 0.081(4) -0.027(4) 0.049(4) -0.005(3) C67 0.056(4) 0.120(5) 0.074(4) -0.046(4) 0.049(4) -0.022(4) C68 0.078(5) 0.103(5) 0.062(4) 0.001(4) 0.055(4) -0.016(4) C69 0.058(4) 0.066(3) 0.044(3) 0.000(3) 0.033(3) -0.004(3) C70 0.046(3) 0.037(3) 0.026(2) -0.006(2) 0.016(2) -0.012(2) C71 0.084(4) 0.046(3) 0.042(3) -0.004(2) 0.040(3) -0.007(3) C72 0.106(5) 0.039(3) 0.051(3) -0.008(3) 0.053(3) -0.008(3) C73 0.063(4) 0.049(3) 0.033(3) -0.008(3) 0.028(3) -0.017(3) C74 0.057(3) 0.052(3) 0.029(3) 0.001(2) 0.022(3) -0.008(2) C75 0.057(3) 0.046(3) 0.025(3) -0.003(2) 0.018(2) -0.003(2) C76 0.081(4) 0.048(3) 0.045(3) -0.015(3) 0.040(3) -0.013(3) C77 0.050(3) 0.040(3) 0.028(3) -0.011(2) 0.019(2) -0.017(2) C78 0.074(4) 0.040(3) 0.030(3) 0.000(2) 0.008(3) -0.005(3) C79 0.075(4) 0.058(3) 0.039(3) 0.011(3) -0.002(3) 0.012(3) C80 0.081(4) 0.075(4) 0.028(3) 0.011(3) 0.016(3) 0.002(3) C81 0.083(4) 0.080(4) 0.024(3) -0.012(3) 0.011(3) 0.007(3) C82 0.094(5) 0.054(3) 0.029(3) -0.005(3) 0.024(3) -0.002(3) C83 0.040(3) 0.033(2) 0.026(2) 0.001(2) 0.013(2) -0.001(2) C84 0.058(4) 0.055(3) 0.045(3) -0.027(3) 0.026(3) -0.025(3) C85 0.071(4) 0.068(3) 0.049(3) -0.022(3) 0.029(3) -0.022(3) C86 0.047(4) 0.076(4) 0.061(4) -0.013(3) 0.015(3) -0.023(3) C87 0.066(5) 0.089(4) 0.118(5) -0.048(4) 0.056(4) -0.024(4) C88 0.042(4) 0.065(3) 0.088(4) -0.032(3) 0.026(3) -0.009(3) C89 0.053(3) 0.032(3) 0.024(2) -0.002(2) 0.011(2) -0.003(2) C90 0.092(5) 0.043(3) 0.043(3) -0.005(3) 0.018(3) 0.005(3) C91 0.125(6) 0.030(3) 0.068(4) -0.013(3) 0.005(4) 0.006(3) C92 0.127(7) 0.047(4) 0.078(5) 0.026(4) 0.003(5) -0.016(4) C93 0.096(5) 0.065(4) 0.072(4) 0.009(4) 0.024(4) -0.034(4) C94 0.065(4) 0.061(3) 0.039(3) 0.001(3) 0.015(3) -0.027(3) O1 0.123(4) 0.056(2) 0.048(2) 0.0009(18) 0.057(2) -0.009(2) O2 0.138(4) 0.047(2) 0.044(2) -0.0015(18) 0.057(2) 0.000(2) O3 0.112(3) 0.070(3) 0.040(2) 0.0102(19) 0.047(2) 0.004(2) O4 0.173(5) 0.080(3) 0.059(2) -0.014(2) 0.082(3) -0.020(3) O5 0.162(6) 0.175(5) 0.135(5) -0.110(5) 0.023(4) -0.033(4) O6 0.173(12) 0.099(7) 0.175(11) 0.067(8) 0.112(10) 0.066(8) O7 0.143(5) 0.107(3) 0.154(5) -0.019(3) 0.097(4) 0.040(3) O8 0.026(8) 0.32(3) 0.23(2) -0.19(2) 0.056(11) -0.064(11) O9 0.115(13) 0.120(10) 0.112(10) 0.102(10) 0.034(9) 0.071(9) O10 0.121(5) 0.136(4) 0.131(4) 0.047(4) -0.001(4) 0.046(4) O11 0.101(5) 0.272(9) 0.215(7) 0.030(7) -0.066(5) -0.105(6) O12 0.387(12) 0.150(5) 0.247(8) 0.042(5) 0.255(9) -0.022(6) O13 0.153(5) 0.118(4) 0.134(4) 0.000(3) 0.078(4) 0.067(4) Cl1 0.0599(11) 0.0733(10) 0.0662(10) -0.0246(9) 0.0140(9) 0.0085(9) Cl2 0.0923(16) 0.1237(16) 0.1213(16) 0.0511(14) 0.0510(14) 0.0221(13) O14 0.149(12) 0.154(10) 0.170(12) -0.019(10) 0.118(11) -0.039(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 N1 C1 1.370(5) . ? N1 C4 1.378(5) . ? N2 C6 1.365(5) . ? N2 C9 1.367(5) . ? N3 C14 1.361(5) . ? N3 C11 1.386(5) . ? N4 C16 1.372(5) . ? N4 C19 1.374(5) . ? C1 C20 1.417(6) . ? C1 C2 1.419(5) . ? C2 C3 1.361(5) . ? C2 C21 1.495(6) . ? C3 C4 1.435(5) . ? C3 C27 1.498(6) . ? C4 C5 1.404(5) . ? C5 C6 1.422(5) . ? C5 C33 1.465(5) . ? C6 C7 1.422(5) . ? C7 C8 1.385(5) . ? C7 C40 1.483(6) . ? C8 C9 1.442(6) . ? C8 C46 1.479(6) . ? C9 C10 1.411(5) . ? C10 C11 1.395(5) . ? C10 C52 1.463(6) . ? C11 C12 1.419(6) . ? C12 C13 1.383(5) . ? C12 C58 1.498(6) . ? C13 C14 1.433(6) . ? C13 C64 1.471(6) . ? C14 C15 1.425(6) . ? C15 C16 1.386(5) . ? C15 C70 1.464(5) . ? C16 C17 1.432(6) . ? C17 C18 1.384(5) . ? C17 C77 1.473(6) . ? C18 C19 1.432(6) . ? C18 C83 1.478(6) . ? C19 C20 1.388(5) . ? C20 C89 1.472(6) . ? C21 C22 1.366(6) . ? C21 C26 1.381(6) . ? C22 C23 1.402(7) . ? C23 C24 1.383(8) . ? C24 C25 1.320(8) . ? C25 C26 1.375(7) . ? C27 C32 1.383(6) . ? C27 C28 1.388(6) . ? C28 C29 1.380(7) . ? C29 C30 1.373(8) . ? C30 C31 1.380(7) . ? C31 C32 1.380(7) . ? C33 C38 1.384(5) . ? C33 C34 1.399(6) . ? C34 C35 1.372(6) . ? C35 C36 1.390(6) . ? C36 C37 1.358(6) . ? C36 C39 1.498(6) . ? C37 C38 1.383(6) . ? C39 O1 1.247(5) . ? C39 O2 1.251(5) . ? C40 C41 1.365(6) . ? C40 C45 1.390(6) . ? C41 C42 1.377(7) . ? C42 C43 1.341(8) . ? C43 C44 1.380(8) . ? C44 C45 1.375(7) . ? C46 C51 1.377(7) . ? C46 C47 1.393(6) . ? C47 C48 1.390(8) . ? C48 C49 1.368(10) . ? C49 C50 1.383(9) . ? C50 C51 1.368(7) . ? C52 C53 1.380(7) . ? C52 C57 1.389(7) . ? C53 C54 1.407(8) . ? C54 C55 1.326(13) . ? C55 C56 1.344(14) . ? C56 C57 1.411(9) . ? C58 C63 1.358(6) . ? C58 C59 1.377(6) . ? C59 C60 1.366(7) . ? C60 C61 1.379(7) . ? C61 C62 1.351(8) . ? C62 C63 1.394(7) . ? C64 C69 1.373(6) . ? C64 C65 1.380(6) . ? C65 C66 1.375(7) . ? C66 C67 1.367(8) . ? C67 C68 1.373(8) . ? C68 C69 1.381(7) . ? C70 C71 1.371(6) . ? C70 C75 1.396(6) . ? C71 C72 1.396(6) . ? C72 C73 1.365(6) . ? C73 C74 1.372(6) . ? C73 C76 1.489(6) . ? C74 C75 1.375(6) . ? C76 O3 1.229(5) . ? C76 O4 1.271(5) . ? C77 C82 1.376(6) . ? C77 C78 1.379(6) . ? C78 C79 1.368(6) . ? C79 C80 1.350(7) . ? C80 C81 1.352(7) . ? C81 C82 1.409(7) . ? C83 C84 1.367(6) . ? C83 C88 1.367(6) . ? C84 C85 1.409(7) . ? C85 C86 1.336(7) . ? C86 C87 1.359(7) . ? C87 C88 1.385(7) . ? C89 C90 1.367(6) . ? C89 C94 1.389(6) . ? C90 C91 1.405(8) . ? C91 C92 1.355(9) . ? C92 C93 1.330(9) . ? C93 C94 1.389(7) . ? O5 Cl1 1.289(5) . ? O6 Cl1 1.542(10) . ? O6 O9 1.57(2) . ? O7 Cl1 1.386(4) . ? O8 O9 0.74(3) . ? O8 Cl1 1.265(12) . ? O8 O14 1.58(2) . ? O9 Cl1 1.359(14) . ? O10 Cl2 1.421(5) . ? O11 Cl2 1.385(6) . ? O12 Cl2 1.434(5) . ? O13 Cl2 1.482(5) . ? Cl1 O14 1.611(11) . ? 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 C1 N1 C4 110.0(3) . . ? C6 N2 C9 110.1(3) . . ? C14 N3 C11 110.0(3) . . ? C16 N4 C19 111.2(3) . . ? N1 C1 C20 122.2(4) . . ? N1 C1 C2 107.1(3) . . ? C20 C1 C2 130.6(4) . . ? C3 C2 C1 108.2(3) . . ? C3 C2 C21 128.0(4) . . ? C1 C2 C21 123.0(3) . . ? C2 C3 C4 108.1(3) . . ? C2 C3 C27 127.4(4) . . ? C4 C3 C27 123.5(3) . . ? N1 C4 C5 122.2(4) . . ? N1 C4 C3 106.2(3) . . ? C5 C4 C3 131.3(4) . . ? C4 C5 C6 121.3(3) . . ? C4 C5 C33 119.3(3) . . ? C6 C5 C33 119.4(3) . . ? N2 C6 C7 108.1(3) . . ? N2 C6 C5 121.8(4) . . ? C7 C6 C5 130.2(4) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 C40 126.5(4) . . ? C6 C7 C40 124.9(4) . . ? C7 C8 C9 107.4(3) . . ? C7 C8 C46 126.8(4) . . ? C9 C8 C46 124.7(4) . . ? N2 C9 C10 123.7(4) . . ? N2 C9 C8 107.0(3) . . ? C10 C9 C8 129.4(4) . . ? C11 C10 C9 121.7(4) . . ? C11 C10 C52 119.9(4) . . ? C9 C10 C52 118.2(4) . . ? N3 C11 C10 122.6(4) . . ? N3 C11 C12 106.7(3) . . ? C10 C11 C12 130.3(4) . . ? C13 C12 C11 108.4(4) . . ? C13 C12 C58 126.0(4) . . ? C11 C12 C58 124.5(4) . . ? C12 C13 C14 107.0(3) . . ? C12 C13 C64 127.3(4) . . ? C14 C13 C64 125.0(4) . . ? N3 C14 C15 123.2(4) . . ? N3 C14 C13 107.7(4) . . ? C15 C14 C13 129.0(4) . . ? C16 C15 C14 122.5(3) . . ? C16 C15 C70 119.7(4) . . ? C14 C15 C70 117.7(3) . . ? N4 C16 C15 124.5(4) . . ? N4 C16 C17 106.3(3) . . ? C15 C16 C17 129.2(4) . . ? C18 C17 C16 108.2(3) . . ? C18 C17 C77 125.3(4) . . ? C16 C17 C77 125.5(4) . . ? C17 C18 C19 107.7(4) . . ? C17 C18 C83 124.4(4) . . ? C19 C18 C83 126.6(4) . . ? N4 C19 C20 122.6(4) . . ? N4 C19 C18 106.5(3) . . ? C20 C19 C18 130.8(4) . . ? C19 C20 C1 122.8(4) . . ? C19 C20 C89 119.3(4) . . ? C1 C20 C89 117.9(3) . . ? C22 C21 C26 118.0(4) . . ? C22 C21 C2 119.9(4) . . ? C26 C21 C2 122.1(4) . . ? C21 C22 C23 120.1(5) . . ? C24 C23 C22 119.6(5) . . ? C25 C24 C23 120.1(5) . . ? C24 C25 C26 120.8(6) . . ? C25 C26 C21 121.3(5) . . ? C32 C27 C28 119.1(4) . . ? C32 C27 C3 119.1(4) . . ? C28 C27 C3 121.7(4) . . ? C29 C28 C27 119.5(5) . . ? C30 C29 C28 121.4(5) . . ? C29 C30 C31 119.2(5) . . ? C30 C31 C32 120.0(5) . . ? C31 C32 C27 120.8(5) . . ? C38 C33 C34 117.4(4) . . ? C38 C33 C5 122.0(4) . . ? C34 C33 C5 120.6(4) . . ? C35 C34 C33 121.7(4) . . ? C34 C35 C36 119.4(4) . . ? C37 C36 C35 119.6(4) . . ? C37 C36 C39 121.6(4) . . ? C35 C36 C39 118.7(4) . . ? C36 C37 C38 121.0(4) . . ? C37 C38 C33 120.8(4) . . ? O1 C39 O2 124.9(4) . . ? O1 C39 C36 118.9(4) . . ? O2 C39 C36 116.3(4) . . ? C41 C40 C45 118.5(4) . . ? C41 C40 C7 119.5(4) . . ? C45 C40 C7 122.0(4) . . ? C40 C41 C42 121.6(5) . . ? C43 C42 C41 118.9(6) . . ? C42 C43 C44 121.9(5) . . ? C45 C44 C43 118.7(5) . . ? C44 C45 C40 120.4(5) . . ? C51 C46 C47 118.4(4) . . ? C51 C46 C8 120.0(4) . . ? C47 C46 C8 121.5(4) . . ? C48 C47 C46 119.7(6) . . ? C49 C48 C47 120.2(6) . . ? C48 C49 C50 120.5(6) . . ? C51 C50 C49 118.9(6) . . ? C50 C51 C46 122.2(6) . . ? C53 C52 C57 119.8(5) . . ? C53 C52 C10 120.6(5) . . ? C57 C52 C10 119.4(5) . . ? C52 C53 C54 118.9(7) . . ? C55 C54 C53 122.0(9) . . ? C54 C55 C56 119.2(8) . . ? C55 C56 C57 122.7(9) . . ? C52 C57 C56 117.4(7) . . ? C63 C58 C59 118.9(4) . . ? C63 C58 C12 122.4(4) . . ? C59 C58 C12 118.7(4) . . ? C60 C59 C58 120.3(5) . . ? C59 C60 C61 120.4(5) . . ? C62 C61 C60 119.9(5) . . ? C61 C62 C63 119.4(5) . . ? C58 C63 C62 121.1(5) . . ? C69 C64 C65 118.3(4) . . ? C69 C64 C13 122.5(4) . . ? C65 C64 C13 119.2(4) . . ? C66 C65 C64 121.7(5) . . ? C67 C66 C65 119.4(6) . . ? C66 C67 C68 119.9(5) . . ? C67 C68 C69 120.4(5) . . ? C64 C69 C68 120.4(5) . . ? C71 C70 C75 117.8(4) . . ? C71 C70 C15 121.8(4) . . ? C75 C70 C15 120.3(4) . . ? C70 C71 C72 120.7(4) . . ? C73 C72 C71 120.0(4) . . ? C72 C73 C74 120.5(4) . . ? C72 C73 C76 121.6(4) . . ? C74 C73 C76 118.0(4) . . ? C73 C74 C75 119.3(4) . . ? C74 C75 C70 121.6(4) . . ? O3 C76 O4 122.5(4) . . ? O3 C76 C73 121.3(4) . . ? O4 C76 C73 116.2(5) . . ? C82 C77 C78 119.3(4) . . ? C82 C77 C17 121.0(4) . . ? C78 C77 C17 119.8(4) . . ? C79 C78 C77 120.1(5) . . ? C80 C79 C78 121.1(5) . . ? C79 C80 C81 120.2(5) . . ? C80 C81 C82 120.1(5) . . ? C77 C82 C81 119.2(5) . . ? C84 C83 C88 118.2(4) . . ? C84 C83 C18 122.6(4) . . ? C88 C83 C18 119.0(4) . . ? C83 C84 C85 120.6(5) . . ? C86 C85 C84 119.8(5) . . ? C85 C86 C87 120.3(5) . . ? C86 C87 C88 120.2(5) . . ? C83 C88 C87 120.8(5) . . ? C90 C89 C94 117.5(4) . . ? C90 C89 C20 121.6(4) . . ? C94 C89 C20 120.9(4) . . ? C89 C90 C91 120.4(6) . . ? C92 C91 C90 119.8(6) . . ? C93 C92 C91 121.1(6) . . ? C92 C93 C94 119.7(6) . . ? C89 C94 C93 121.4(5) . . ? Cl1 O6 O9 51.7(5) . . ? O9 O8 Cl1 81(2) . . ? O9 O8 O14 130(3) . . ? Cl1 O8 O14 67.8(10) . . ? O8 O9 Cl1 66.8(17) . . ? O8 O9 O6 126(2) . . ? Cl1 O9 O6 62.9(9) . . ? O8 Cl1 O5 133.4(7) . . ? O8 Cl1 O9 32.4(15) . . ? O5 Cl1 O9 120.5(8) . . ? O8 Cl1 O7 109.7(8) . . ? O5 Cl1 O7 114.4(4) . . ? O9 Cl1 O7 122.7(8) . . ? O8 Cl1 O6 96.0(15) . . ? O5 Cl1 O6 91.4(6) . . ? O9 Cl1 O6 65.4(7) . . ? O7 Cl1 O6 99.1(4) . . ? O8 Cl1 O14 65.5(12) . . ? O5 Cl1 O14 88.3(6) . . ? O9 Cl1 O14 91.6(8) . . ? O7 Cl1 O14 105.8(5) . . ? O6 Cl1 O14 152.8(7) . . ? O11 Cl2 O10 110.1(4) . . ? O11 Cl2 O12 115.4(6) . . ? O10 Cl2 O12 108.9(5) . . ? O11 Cl2 O13 114.8(5) . . ? O10 Cl2 O13 103.6(4) . . ? O12 Cl2 O13 103.2(4) . . ? O8 O14 Cl1 46.7(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 N1 C1 C20 -172.0(4) . . . . ? C4 N1 C1 C2 5.7(5) . . . . ? N1 C1 C2 C3 -3.3(5) . . . . ? C20 C1 C2 C3 174.1(4) . . . . ? N1 C1 C2 C21 167.5(4) . . . . ? C20 C1 C2 C21 -15.1(7) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C21 C2 C3 C4 -170.4(4) . . . . ? C1 C2 C3 C27 168.5(4) . . . . ? C21 C2 C3 C27 -1.8(7) . . . . ? C1 N1 C4 C5 169.1(4) . . . . ? C1 N1 C4 C3 -5.8(4) . . . . ? C2 C3 C4 N1 3.6(5) . . . . ? C27 C3 C4 N1 -165.6(4) . . . . ? C2 C3 C4 C5 -170.6(4) . . . . ? C27 C3 C4 C5 20.2(7) . . . . ? N1 C4 C5 C6 32.9(6) . . . . ? C3 C4 C5 C6 -153.6(4) . . . . ? N1 C4 C5 C33 -145.8(4) . . . . ? C3 C4 C5 C33 27.6(7) . . . . ? C9 N2 C6 C7 -3.9(5) . . . . ? C9 N2 C6 C5 176.1(4) . . . . ? C4 C5 C6 N2 30.6(6) . . . . ? C33 C5 C6 N2 -150.6(4) . . . . ? C4 C5 C6 C7 -149.3(5) . . . . ? C33 C5 C6 C7 29.4(7) . . . . ? N2 C6 C7 C8 2.8(5) . . . . ? C5 C6 C7 C8 -177.2(4) . . . . ? N2 C6 C7 C40 -165.0(4) . . . . ? C5 C6 C7 C40 15.0(7) . . . . ? C6 C7 C8 C9 -0.7(5) . . . . ? C40 C7 C8 C9 166.8(4) . . . . ? C6 C7 C8 C46 -168.9(4) . . . . ? C40 C7 C8 C46 -1.3(7) . . . . ? C6 N2 C9 C10 -175.8(4) . . . . ? C6 N2 C9 C8 3.5(5) . . . . ? C7 C8 C9 N2 -1.6(5) . . . . ? C46 C8 C9 N2 166.9(4) . . . . ? C7 C8 C9 C10 177.6(4) . . . . ? C46 C8 C9 C10 -14.0(7) . . . . ? N2 C9 C10 C11 -32.2(6) . . . . ? C8 C9 C10 C11 148.8(4) . . . . ? N2 C9 C10 C52 152.8(4) . . . . ? C8 C9 C10 C52 -26.2(7) . . . . ? C14 N3 C11 C10 -168.2(4) . . . . ? C14 N3 C11 C12 5.5(5) . . . . ? C9 C10 C11 N3 -27.1(6) . . . . ? C52 C10 C11 N3 147.8(4) . . . . ? C9 C10 C11 C12 160.9(4) . . . . ? C52 C10 C11 C12 -24.2(7) . . . . ? N3 C11 C12 C13 -3.3(4) . . . . ? C10 C11 C12 C13 169.6(4) . . . . ? N3 C11 C12 C58 165.1(4) . . . . ? C10 C11 C12 C58 -22.0(7) . . . . ? C11 C12 C13 C14 0.1(4) . . . . ? C58 C12 C13 C14 -168.1(4) . . . . ? C11 C12 C13 C64 171.1(4) . . . . ? C58 C12 C13 C64 2.9(7) . . . . ? C11 N3 C14 C15 170.7(4) . . . . ? C11 N3 C14 C13 -5.4(5) . . . . ? C12 C13 C14 N3 3.2(4) . . . . ? C64 C13 C14 N3 -168.0(4) . . . . ? C12 C13 C14 C15 -172.5(4) . . . . ? C64 C13 C14 C15 16.2(7) . . . . ? N3 C14 C15 C16 26.7(6) . . . . ? C13 C14 C15 C16 -158.1(4) . . . . ? N3 C14 C15 C70 -152.5(4) . . . . ? C13 C14 C15 C70 22.7(7) . . . . ? C19 N4 C16 C15 175.2(4) . . . . ? C19 N4 C16 C17 -4.2(4) . . . . ? C14 C15 C16 N4 25.0(6) . . . . ? C70 C15 C16 N4 -155.8(4) . . . . ? C14 C15 C16 C17 -155.7(4) . . . . ? C70 C15 C16 C17 23.5(7) . . . . ? N4 C16 C17 C18 2.8(4) . . . . ? C15 C16 C17 C18 -176.6(4) . . . . ? N4 C16 C17 C77 -166.3(4) . . . . ? C15 C16 C17 C77 14.2(7) . . . . ? C16 C17 C18 C19 -0.5(5) . . . . ? C77 C17 C18 C19 168.7(4) . . . . ? C16 C17 C18 C83 -167.9(4) . . . . ? C77 C17 C18 C83 1.3(6) . . . . ? C16 N4 C19 C20 -173.1(4) . . . . ? C16 N4 C19 C18 4.0(4) . . . . ? C17 C18 C19 N4 -2.1(4) . . . . ? C83 C18 C19 N4 165.0(4) . . . . ? C17 C18 C19 C20 174.7(4) . . . . ? C83 C18 C19 C20 -18.3(7) . . . . ? N4 C19 C20 C1 -25.6(6) . . . . ? C18 C19 C20 C1 158.1(4) . . . . ? N4 C19 C20 C89 154.7(4) . . . . ? C18 C19 C20 C89 -21.6(7) . . . . ? N1 C1 C20 C19 -31.4(6) . . . . ? C2 C1 C20 C19 151.5(4) . . . . ? N1 C1 C20 C89 148.3(4) . . . . ? C2 C1 C20 C89 -28.8(7) . . . . ? C3 C2 C21 C22 112.6(5) . . . . ? C1 C2 C21 C22 -56.4(6) . . . . ? C3 C2 C21 C26 -67.3(7) . . . . ? C1 C2 C21 C26 123.7(5) . . . . ? C26 C21 C22 C23 0.2(7) . . . . ? C2 C21 C22 C23 -179.7(5) . . . . ? C21 C22 C23 C24 -1.6(8) . . . . ? C22 C23 C24 C25 2.3(9) . . . . ? C23 C24 C25 C26 -1.6(10) . . . . ? C24 C25 C26 C21 0.1(9) . . . . ? C22 C21 C26 C25 0.6(7) . . . . ? C2 C21 C26 C25 -179.5(5) . . . . ? C2 C3 C27 C32 -112.0(5) . . . . ? C4 C3 C27 C32 55.0(6) . . . . ? C2 C3 C27 C28 65.5(6) . . . . ? C4 C3 C27 C28 -127.5(4) . . . . ? C32 C27 C28 C29 0.0(7) . . . . ? C3 C27 C28 C29 -177.6(4) . . . . ? C27 C28 C29 C30 0.1(8) . . . . ? C28 C29 C30 C31 0.0(9) . . . . ? C29 C30 C31 C32 -0.2(9) . . . . ? C30 C31 C32 C27 0.3(9) . . . . ? C28 C27 C32 C31 -0.2(7) . . . . ? C3 C27 C32 C31 177.4(5) . . . . ? C4 C5 C33 C38 -146.0(4) . . . . ? C6 C5 C33 C38 35.3(6) . . . . ? C4 C5 C33 C34 34.2(6) . . . . ? C6 C5 C33 C34 -144.5(4) . . . . ? C38 C33 C34 C35 2.5(6) . . . . ? C5 C33 C34 C35 -177.7(4) . . . . ? C33 C34 C35 C36 -2.9(7) . . . . ? C34 C35 C36 C37 0.9(7) . . . . ? C34 C35 C36 C39 179.5(4) . . . . ? C35 C36 C37 C38 1.3(7) . . . . ? C39 C36 C37 C38 -177.2(4) . . . . ? C36 C37 C38 C33 -1.7(7) . . . . ? C34 C33 C38 C37 -0.2(6) . . . . ? C5 C33 C38 C37 -180.0(4) . . . . ? C37 C36 C39 O1 163.7(5) . . . . ? C35 C36 C39 O1 -14.8(7) . . . . ? C37 C36 C39 O2 -15.8(7) . . . . ? C35 C36 C39 O2 165.7(5) . . . . ? C8 C7 C40 C41 -109.9(5) . . . . ? C6 C7 C40 C41 55.6(6) . . . . ? C8 C7 C40 C45 67.0(6) . . . . ? C6 C7 C40 C45 -127.5(5) . . . . ? C45 C40 C41 C42 2.5(8) . . . . ? C7 C40 C41 C42 179.5(5) . . . . ? C40 C41 C42 C43 -2.5(9) . . . . ? C41 C42 C43 C44 1.9(10) . . . . ? C42 C43 C44 C45 -1.3(10) . . . . ? C43 C44 C45 C40 1.2(8) . . . . ? C41 C40 C45 C44 -1.8(7) . . . . ? C7 C40 C45 C44 -178.8(5) . . . . ? C7 C8 C46 C51 114.8(5) . . . . ? C9 C8 C46 C51 -51.4(7) . . . . ? C7 C8 C46 C47 -69.4(6) . . . . ? C9 C8 C46 C47 124.4(5) . . . . ? C51 C46 C47 C48 -2.3(7) . . . . ? C8 C46 C47 C48 -178.1(5) . . . . ? C46 C47 C48 C49 2.8(9) . . . . ? C47 C48 C49 C50 -1.6(10) . . . . ? C48 C49 C50 C51 -0.1(10) . . . . ? C49 C50 C51 C46 0.7(9) . . . . ? C47 C46 C51 C50 0.5(8) . . . . ? C8 C46 C51 C50 176.5(5) . . . . ? C11 C10 C52 C53 140.9(5) . . . . ? C9 C10 C52 C53 -44.0(6) . . . . ? C11 C10 C52 C57 -43.4(6) . . . . ? C9 C10 C52 C57 131.7(5) . . . . ? C57 C52 C53 C54 -0.7(8) . . . . ? C10 C52 C53 C54 175.0(5) . . . . ? C52 C53 C54 C55 -0.9(11) . . . . ? C53 C54 C55 C56 1.6(14) . . . . ? C54 C55 C56 C57 -0.7(15) . . . . ? C53 C52 C57 C56 1.5(8) . . . . ? C10 C52 C57 C56 -174.2(5) . . . . ? C55 C56 C57 C52 -0.9(11) . . . . ? C13 C12 C58 C63 -68.2(6) . . . . ? C11 C12 C58 C63 125.4(5) . . . . ? C13 C12 C58 C59 109.2(5) . . . . ? C11 C12 C58 C59 -57.1(6) . . . . ? C63 C58 C59 C60 1.3(7) . . . . ? C12 C58 C59 C60 -176.2(4) . . . . ? C58 C59 C60 C61 -1.0(7) . . . . ? C59 C60 C61 C62 0.3(8) . . . . ? C60 C61 C62 C63 0.0(8) . . . . ? C59 C58 C63 C62 -1.0(7) . . . . ? C12 C58 C63 C62 176.4(4) . . . . ? C61 C62 C63 C58 0.4(8) . . . . ? C12 C13 C64 C69 70.2(6) . . . . ? C14 C13 C64 C69 -120.4(5) . . . . ? C12 C13 C64 C65 -110.9(5) . . . . ? C14 C13 C64 C65 58.5(6) . . . . ? C69 C64 C65 C66 0.0(7) . . . . ? C13 C64 C65 C66 -178.9(5) . . . . ? C64 C65 C66 C67 0.2(8) . . . . ? C65 C66 C67 C68 -0.9(9) . . . . ? C66 C67 C68 C69 1.4(9) . . . . ? C65 C64 C69 C68 0.5(7) . . . . ? C13 C64 C69 C68 179.4(5) . . . . ? C67 C68 C69 C64 -1.2(8) . . . . ? C16 C15 C70 C71 53.5(6) . . . . ? C14 C15 C70 C71 -127.3(5) . . . . ? C16 C15 C70 C75 -125.7(5) . . . . ? C14 C15 C70 C75 53.5(6) . . . . ? C75 C70 C71 C72 -2.8(7) . . . . ? C15 C70 C71 C72 178.0(5) . . . . ? C70 C71 C72 C73 2.3(8) . . . . ? C71 C72 C73 C74 -1.1(8) . . . . ? C71 C72 C73 C76 179.7(5) . . . . ? C72 C73 C74 C75 0.6(7) . . . . ? C76 C73 C74 C75 179.8(4) . . . . ? C73 C74 C75 C70 -1.2(7) . . . . ? C71 C70 C75 C74 2.2(7) . . . . ? C15 C70 C75 C74 -178.5(4) . . . . ? C72 C73 C76 O3 170.2(5) . . . . ? C74 C73 C76 O3 -9.0(8) . . . . ? C72 C73 C76 O4 -12.1(8) . . . . ? C74 C73 C76 O4 168.7(5) . . . . ? C18 C17 C77 C82 67.9(6) . . . . ? C16 C17 C77 C82 -124.8(5) . . . . ? C18 C17 C77 C78 -110.8(5) . . . . ? C16 C17 C77 C78 56.5(6) . . . . ? C82 C77 C78 C79 0.1(8) . . . . ? C17 C77 C78 C79 178.8(5) . . . . ? C77 C78 C79 C80 0.2(9) . . . . ? C78 C79 C80 C81 -0.9(9) . . . . ? C79 C80 C81 C82 1.3(9) . . . . ? C78 C77 C82 C81 0.3(7) . . . . ? C17 C77 C82 C81 -178.4(5) . . . . ? C80 C81 C82 C77 -1.0(9) . . . . ? C17 C18 C83 C84 -76.9(6) . . . . ? C19 C18 C83 C84 118.1(5) . . . . ? C17 C18 C83 C88 98.4(5) . . . . ? C19 C18 C83 C88 -66.6(6) . . . . ? C88 C83 C84 C85 -1.5(7) . . . . ? C18 C83 C84 C85 173.8(4) . . . . ? C83 C84 C85 C86 0.1(8) . . . . ? C84 C85 C86 C87 1.3(9) . . . . ? C85 C86 C87 C88 -1.2(10) . . . . ? C84 C83 C88 C87 1.6(8) . . . . ? C18 C83 C88 C87 -173.9(5) . . . . ? C86 C87 C88 C83 -0.2(10) . . . . ? C19 C20 C89 C90 -46.0(6) . . . . ? C1 C20 C89 C90 134.2(5) . . . . ? C19 C20 C89 C94 135.2(5) . . . . ? C1 C20 C89 C94 -44.5(6) . . . . ? C94 C89 C90 C91 -0.5(7) . . . . ? C20 C89 C90 C91 -179.3(5) . . . . ? C89 C90 C91 C92 1.2(9) . . . . ? C90 C91 C92 C93 -2.6(10) . . . . ? C91 C92 C93 C94 3.3(10) . . . . ? C90 C89 C94 C93 1.1(7) . . . . ? C20 C89 C94 C93 179.9(5) . . . . ? C92 C93 C94 C89 -2.6(9) . . . . ? O14 O8 O9 Cl1 50(2) . . . . ? Cl1 O8 O9 O6 22(3) . . . . ? O14 O8 O9 O6 73(4) . . . . ? Cl1 O6 O9 O8 -23(3) . . . . ? O9 O8 Cl1 O5 79(3) . . . . ? O14 O8 Cl1 O5 -61.6(19) . . . . ? O14 O8 Cl1 O9 -141(2) . . . . ? O9 O8 Cl1 O7 -120(2) . . . . ? O14 O8 Cl1 O7 98.8(7) . . . . ? O9 O8 Cl1 O6 -18(2) . . . . ? O14 O8 Cl1 O6 -159.2(8) . . . . ? O9 O8 Cl1 O14 141(2) . . . . ? O6 O9 Cl1 O8 -160(3) . . . . ? O8 O9 Cl1 O5 -124(2) . . . . ? O6 O9 Cl1 O5 76.1(8) . . . . ? O8 O9 Cl1 O7 75(2) . . . . ? O6 O9 Cl1 O7 -85.0(8) . . . . ? O8 O9 Cl1 O6 160(3) . . . . ? O8 O9 Cl1 O14 -35(2) . . . . ? O6 O9 Cl1 O14 165.1(7) . . . . ? O9 O6 Cl1 O8 10.7(13) . . . . ? O9 O6 Cl1 O5 -123.2(9) . . . . ? O9 O6 Cl1 O7 121.9(9) . . . . ? O9 O6 Cl1 O14 -34.2(18) . . . . ? O9 O8 O14 Cl1 -55(3) . . . . ? O5 Cl1 O14 O8 140.3(10) . . . . ? O9 Cl1 O14 O8 19.8(14) . . . . ? O7 Cl1 O14 O8 -104.9(10) . . . . ? O6 Cl1 O14 O8 51(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.683 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.053 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 -0.001 0.000 1385 339 ' ' 2 0.500 0.154 0.500 1385 339 ' ' _platon_squeeze_details ; Six and a half of EtOH molecules per the asymmetric unit were deleted with the squeeze program ; # Attachment 'H4TCDPP2Cl-rev2.CIF' data_sankar47 _database_code_depnum_ccdc_archive 'CCDC 866778' #TrackingRef 'H4TCDPP2Cl-rev2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C105 H112 Cl2 N4 O23' _chemical_formula_weight 1868.89 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.306(5) _cell_length_b 15.402(5) _cell_length_c 19.612(7) _cell_angle_alpha 81.772(5) _cell_angle_beta 74.657(5) _cell_angle_gamma 89.895(5) _cell_volume 4410(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9693 _exptl_absorpt_correction_T_max 0.9768 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker APEXII' _diffrn_measurement_method '2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18643 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 23.74 _reflns_number_total 13197 _reflns_number_gt 7838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2009, 11, 0, 0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009' _computing_publication_material 'Mercury CSD 3.0.1' _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^)+(0.1061P)^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 13197 _refine_ls_number_parameters 993 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _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 Cl1 Cl 0.91399(8) 0.08897(7) 0.38253(6) 0.0362(3) Uani 1 1 d . . . Cl2 Cl 0.99893(10) 0.10728(9) 0.12019(7) 0.0570(4) Uani 1 1 d . . . O1 O 1.4821(2) 0.49723(19) 0.17802(17) 0.0416(8) Uani 1 1 d . . . H61 H 1.5228 0.5330 0.1519 0.062 Uiso 1 1 calc R . . O2 O 1.3857(2) 0.59665(18) 0.14957(16) 0.0434(9) Uani 1 1 d . . . O3 O 0.5423(2) 0.58081(18) 0.33262(17) 0.0376(8) Uani 1 1 d . . . H62 H 0.4953 0.6098 0.3429 0.056 Uiso 1 1 calc R . . O4 O 0.4396(2) 0.47065(19) 0.35279(17) 0.0457(9) Uani 1 1 d . . . O5 O 0.4811(2) -0.28864(17) 0.19009(15) 0.0330(8) Uani 1 1 d . . . H63 H 0.4555 -0.3294 0.1774 0.050 Uiso 1 1 calc R . . O6 O 0.6002(2) -0.37464(19) 0.16408(15) 0.0309(7) Uani 1 1 d . . . O7 O 1.41022(19) -0.30969(18) 0.35639(15) 0.0317(7) Uani 1 1 d . . . O8 O 1.33046(19) -0.40893(17) 0.32138(15) 0.0344(8) Uani 1 1 d . . . H64 H 1.3701 -0.4419 0.3320 0.052 Uiso 1 1 calc R . . N1 N 1.0933(2) 0.08868(19) 0.25252(17) 0.0209(8) Uani 1 1 d . . . H1 H 1.0394 0.0933 0.2817 0.025 Uiso 1 1 calc R . . N2 N 0.9683(2) 0.23812(19) 0.23654(17) 0.0209(8) Uani 1 1 d . . . H2 H 0.9698 0.1990 0.2077 0.025 Uiso 1 1 calc R . . N3 N 0.8151(2) 0.10512(19) 0.25571(16) 0.0211(8) Uani 1 1 d . . . H3 H 0.8493 0.0952 0.2854 0.025 Uiso 1 1 calc R . . N4 N 0.9449(2) -0.04105(19) 0.25742(16) 0.0212(8) Uani 1 1 d . . . H4 H 0.9616 0.0078 0.2272 0.025 Uiso 1 1 calc R . . C1 C 1.1321(3) 0.0118(2) 0.2383(2) 0.0216(10) Uani 1 1 d . . . C2 C 1.2164(3) 0.0316(2) 0.1853(2) 0.0218(10) Uani 1 1 d . . . C3 C 1.2273(3) 0.1223(2) 0.1709(2) 0.0220(10) Uani 1 1 d . . . C4 C 1.1498(3) 0.1581(2) 0.2150(2) 0.0222(10) Uani 1 1 d . . . C5 C 1.1306(3) 0.2444(2) 0.2254(2) 0.0205(10) Uani 1 1 d . . . C6 C 1.0423(3) 0.2684(2) 0.2537(2) 0.0214(10) Uani 1 1 d . . . C7 C 1.0103(3) 0.3274(2) 0.3052(2) 0.0210(10) Uani 1 1 d . . . C8 C 0.9167(3) 0.3327(2) 0.3170(2) 0.0203(10) Uani 1 1 d . . . C9 C 0.8903(3) 0.2771(2) 0.2706(2) 0.0205(10) Uani 1 1 d . . . C10 C 0.8065(3) 0.2648(2) 0.2577(2) 0.0197(10) Uani 1 1 d . . . C11 C 0.7891(3) 0.1852(3) 0.2317(2) 0.0257(10) Uani 1 1 d . . . C12 C 0.7388(3) 0.1750(2) 0.1811(2) 0.0229(10) Uani 1 1 d . . . C13 C 0.7345(3) 0.0860(2) 0.1772(2) 0.0217(10) Uani 1 1 d . . . C14 C 0.7802(3) 0.0419(2) 0.2270(2) 0.0218(9) Uani 1 1 d . . . C15 C 0.7889(3) -0.0477(2) 0.2486(2) 0.0258(10) Uani 1 1 d . . . C16 C 0.8604(3) -0.0782(2) 0.2781(2) 0.0212(9) Uani 1 1 d . . . C17 C 0.8590(3) -0.1522(2) 0.3316(2) 0.0224(10) Uani 1 1 d . . . C18 C 0.9451(3) -0.1603(2) 0.3395(2) 0.0237(10) Uani 1 1 d . . . C19 C 1.0007(3) -0.0907(2) 0.2904(2) 0.0222(10) Uani 1 1 d . . . C20 C 1.0937(3) -0.0728(2) 0.2718(2) 0.0217(10) Uani 1 1 d . . . C21 C 1.2643(3) -0.0371(3) 0.1454(2) 0.0250(11) Uani 1 1 d . . . C22 C 1.2156(3) -0.0807(3) 0.1089(2) 0.0332(11) Uani 1 1 d . . . H5 H 1.1568 -0.0626 0.1072 0.040 Uiso 1 1 calc R . . C23 C 1.2525(4) -0.1496(3) 0.0756(2) 0.0391(13) Uani 1 1 d . . . H6 H 1.2192 -0.1790 0.0506 0.047 Uiso 1 1 calc R . . C24 C 1.3370(4) -0.1763(3) 0.0782(2) 0.0415(13) Uani 1 1 d . . . H7 H 1.3618 -0.2251 0.0560 0.050 Uiso 1 1 calc R . . C25 C 1.3860(3) -0.1320(3) 0.1131(2) 0.0371(12) Uani 1 1 d . . . H8 H 1.4454 -0.1494 0.1136 0.045 Uiso 1 1 calc R . . C26 C 1.3498(3) -0.0634(3) 0.1468(2) 0.0318(11) Uani 1 1 d . . . H9 H 1.3837 -0.0339 0.1713 0.038 Uiso 1 1 calc R . . C27 C 1.2982(3) 0.1737(2) 0.1136(2) 0.0221(10) Uani 1 1 d . . . C28 C 1.3894(3) 0.1649(3) 0.1097(2) 0.0251(10) Uani 1 1 d . . . H10 H 1.4072 0.1236 0.1439 0.030 Uiso 1 1 calc R . . C29 C 1.4543(3) 0.2152(3) 0.0570(2) 0.0292(11) Uani 1 1 d . . . H11 H 1.5167 0.2079 0.0546 0.035 Uiso 1 1 calc R . . C30 C 1.4294(3) 0.2761(3) 0.0078(2) 0.0379(12) Uani 1 1 d . . . H12 H 1.4745 0.3119 -0.0278 0.045 Uiso 1 1 calc R . . C31 C 1.3401(3) 0.2853(3) 0.0099(2) 0.0320(11) Uani 1 1 d . . . H13 H 1.3232 0.3263 -0.0250 0.038 Uiso 1 1 calc R . . C32 C 1.2740(3) 0.2350(3) 0.0628(2) 0.0279(10) Uani 1 1 d . . . H14 H 1.2119 0.2423 0.0645 0.033 Uiso 1 1 calc R . . C33 C 1.2030(3) 0.3138(2) 0.2100(2) 0.0211(10) Uani 1 1 d . . . C34 C 1.2841(3) 0.2989(2) 0.2282(2) 0.0226(10) Uani 1 1 d . . . H15 H 1.2938 0.2425 0.2512 0.027 Uiso 1 1 calc R . . C35 C 1.3503(3) 0.3638(3) 0.2139(2) 0.0274(11) Uani 1 1 d . . . H16 H 1.4061 0.3521 0.2255 0.033 Uiso 1 1 calc R . . C36 C 1.3348(3) 0.4477(3) 0.1817(2) 0.0267(10) Uani 1 1 d . . . C37 C 1.2548(3) 0.4647(3) 0.1638(2) 0.0280(11) Uani 1 1 d . . . H17 H 1.2445 0.5216 0.1421 0.034 Uiso 1 1 calc R . . C38 C 1.1888(3) 0.3971(2) 0.1779(2) 0.0253(10) Uani 1 1 d . . . H18 H 1.1336 0.4082 0.1654 0.030 Uiso 1 1 calc R . . C39 C 1.4054(3) 0.5194(3) 0.1682(2) 0.0282(11) Uani 1 1 d . . . C40 C 1.0701(3) 0.3541(2) 0.34772(19) 0.0189(9) Uani 1 1 d . . . C41 C 1.1092(3) 0.2879(3) 0.3840(2) 0.0276(10) Uani 1 1 d . . . H19 H 1.0918 0.2284 0.3852 0.033 Uiso 1 1 calc R . . C42 C 1.1728(3) 0.3067(3) 0.4185(2) 0.0347(12) Uani 1 1 d . . . H20 H 1.1998 0.2607 0.4425 0.042 Uiso 1 1 calc R . . C43 C 1.1965(3) 0.3925(3) 0.4176(2) 0.0361(12) Uani 1 1 d . . . H21 H 1.2413 0.4061 0.4404 0.043 Uiso 1 1 calc R . . C44 C 1.1561(3) 0.4596(3) 0.3839(2) 0.0340(11) Uani 1 1 d . . . H22 H 1.1706 0.5192 0.3854 0.041 Uiso 1 1 calc R . . C45 C 1.0950(3) 0.4393(3) 0.3483(2) 0.0274(10) Uani 1 1 d . . . H23 H 1.0693 0.4854 0.3233 0.033 Uiso 1 1 calc R . . C46 C 0.8529(3) 0.3710(2) 0.3725(2) 0.0204(10) Uani 1 1 d . . . C47 C 0.8598(3) 0.4595(3) 0.3790(2) 0.0237(10) Uani 1 1 d . . . H24 H 0.9075 0.4959 0.3469 0.028 Uiso 1 1 calc R . . C48 C 0.7972(3) 0.4946(3) 0.4325(2) 0.0292(11) Uani 1 1 d . . . H25 H 0.8027 0.5546 0.4376 0.035 Uiso 1 1 calc R . . C49 C 0.7266(3) 0.4411(3) 0.4784(2) 0.0328(11) Uani 1 1 d . . . H26 H 0.6825 0.4650 0.5140 0.039 Uiso 1 1 calc R . . C50 C 0.7205(3) 0.3526(3) 0.4722(2) 0.0353(12) Uani 1 1 d . . . H27 H 0.6732 0.3157 0.5044 0.042 Uiso 1 1 calc R . . C51 C 0.7827(3) 0.3188(3) 0.4197(2) 0.0259(10) Uani 1 1 d . . . H28 H 0.7778 0.2584 0.4155 0.031 Uiso 1 1 calc R . . C52 C 0.7345(3) 0.3259(2) 0.2715(2) 0.0221(10) Uani 1 1 d . . . C53 C 0.7511(3) 0.4170(3) 0.2582(2) 0.0269(11) Uani 1 1 d . . . H29 H 0.8106 0.4403 0.2346 0.032 Uiso 1 1 calc R . . C54 C 0.6819(3) 0.4733(3) 0.2790(2) 0.0274(11) Uani 1 1 d . . . H30 H 0.6945 0.5348 0.2709 0.033 Uiso 1 1 calc R . . C55 C 0.5953(3) 0.4409(3) 0.3111(2) 0.0250(10) Uani 1 1 d . . . C56 C 0.5764(3) 0.3506(3) 0.3222(2) 0.0280(11) Uani 1 1 d . . . H31 H 0.5159 0.3281 0.3428 0.034 Uiso 1 1 calc R . . C57 C 0.6460(3) 0.2939(3) 0.3034(2) 0.0247(10) Uani 1 1 d . . . H32 H 0.6332 0.2324 0.3123 0.030 Uiso 1 1 calc R . . C58 C 0.5199(3) 0.5003(3) 0.3339(2) 0.0296(11) Uani 1 1 d . . . C59 C 0.7174(3) 0.2498(2) 0.1311(2) 0.0238(10) Uani 1 1 d . . . C60 C 0.7879(4) 0.2888(3) 0.0767(3) 0.0467(13) Uani 1 1 d . . . H33 H 0.8477 0.2691 0.0726 0.056 Uiso 1 1 calc R . . C61 C 0.7722(5) 0.3569(4) 0.0275(3) 0.075(2) Uani 1 1 d . . . H34 H 0.8209 0.3818 -0.0116 0.090 Uiso 1 1 calc R . . C62 C 0.6865(5) 0.3888(4) 0.0349(3) 0.0636(18) Uani 1 1 d . . . H35 H 0.6764 0.4368 0.0020 0.076 Uiso 1 1 calc R . . C63 C 0.6160(4) 0.3511(3) 0.0897(3) 0.0444(13) Uani 1 1 d . . . H36 H 0.5567 0.3727 0.0952 0.053 Uiso 1 1 calc R . . C64 C 0.6321(3) 0.2801(3) 0.1378(2) 0.0366(12) Uani 1 1 d . . . H37 H 0.5830 0.2529 0.1753 0.044 Uiso 1 1 calc R . . C65 C 0.7031(3) 0.0435(2) 0.1250(2) 0.0232(10) Uani 1 1 d . . . C66 C 0.6170(3) 0.0560(2) 0.1162(2) 0.0249(10) Uani 1 1 d . . . H38 H 0.5792 0.0962 0.1417 0.030 Uiso 1 1 calc R . . C67 C 0.5852(3) 0.0110(3) 0.0711(2) 0.0304(12) Uani 1 1 d . . . H39 H 0.5260 0.0204 0.0653 0.037 Uiso 1 1 calc R . . C68 C 0.6401(3) -0.0476(3) 0.0345(2) 0.0305(12) Uani 1 1 d . . . H40 H 0.6177 -0.0804 0.0048 0.037 Uiso 1 1 calc R . . C69 C 0.7273(3) -0.0591(3) 0.0408(2) 0.0304(11) Uani 1 1 d . . . H41 H 0.7652 -0.0986 0.0145 0.037 Uiso 1 1 calc R . . C70 C 0.7594(3) -0.0130(3) 0.0854(2) 0.0268(11) Uani 1 1 d . . . H42 H 0.8198 -0.0199 0.0889 0.032 Uiso 1 1 calc R . . C71 C 0.7274(3) -0.1157(2) 0.2378(2) 0.0239(10) Uani 1 1 d . . . C72 C 0.6341(3) -0.1063(3) 0.2512(2) 0.0258(10) Uani 1 1 d . . . H43 H 0.6070 -0.0573 0.2717 0.031 Uiso 1 1 calc R . . C73 C 0.5811(3) -0.1681(3) 0.2348(2) 0.0283(11) Uani 1 1 d . . . H44 H 0.5176 -0.1610 0.2435 0.034 Uiso 1 1 calc R . . C74 C 0.6196(3) -0.2410(3) 0.2054(2) 0.0256(11) Uani 1 1 d . . . C75 C 0.7133(3) -0.2518(2) 0.1926(2) 0.0283(11) Uani 1 1 d . . . H45 H 0.7403 -0.3014 0.1729 0.034 Uiso 1 1 calc R . . C76 C 0.7662(3) -0.1891(2) 0.2093(2) 0.0255(10) Uani 1 1 d . . . H46 H 0.8296 -0.1962 0.2012 0.031 Uiso 1 1 calc R . . C77 C 0.5659(3) -0.3066(3) 0.1848(2) 0.0258(11) Uani 1 1 d . . . C78 C 0.7735(3) -0.1961(3) 0.3807(2) 0.0257(10) Uani 1 1 d . . . C79 C 0.7240(3) -0.1503(3) 0.4320(3) 0.0448(13) Uani 1 1 d . . . H47 H 0.7443 -0.0930 0.4348 0.054 Uiso 1 1 calc R . . C80 C 0.6449(4) -0.1867(4) 0.4795(3) 0.0652(17) Uani 1 1 d . . . H48 H 0.6118 -0.1550 0.5155 0.078 Uiso 1 1 calc R . . C81 C 0.6135(4) -0.2699(4) 0.4747(3) 0.0615(17) Uani 1 1 d . . . H49 H 0.5587 -0.2950 0.5068 0.074 Uiso 1 1 calc R . . C82 C 0.6625(3) -0.3147(3) 0.4235(3) 0.0457(14) Uani 1 1 d . . . H50 H 0.6416 -0.3714 0.4197 0.055 Uiso 1 1 calc R . . C83 C 0.7418(3) -0.2786(3) 0.3772(2) 0.0364(12) Uani 1 1 d . . . H51 H 0.7755 -0.3112 0.3420 0.044 Uiso 1 1 calc R . . C84 C 0.9771(3) -0.2231(2) 0.39075(19) 0.0190(9) Uani 1 1 d . . . C85 C 0.9634(3) -0.3130(2) 0.3938(2) 0.0234(10) Uani 1 1 d . . . H52 H 0.9283 -0.3341 0.3659 0.028 Uiso 1 1 calc R . . C86 C 1.0006(3) -0.3714(3) 0.4372(2) 0.0292(11) Uani 1 1 d . . . H53 H 0.9905 -0.4327 0.4395 0.035 Uiso 1 1 calc R . . C87 C 1.0528(3) -0.3410(3) 0.4776(2) 0.0300(11) Uani 1 1 d . . . H54 H 1.0811 -0.3812 0.5057 0.036 Uiso 1 1 calc R . . C88 C 1.0633(3) -0.2523(3) 0.4764(2) 0.0263(10) Uani 1 1 d . . . H55 H 1.0964 -0.2314 0.5058 0.032 Uiso 1 1 calc R . . C89 C 1.0269(3) -0.1939(3) 0.4338(2) 0.0272(11) Uani 1 1 d . . . H56 H 1.0355 -0.1327 0.4333 0.033 Uiso 1 1 calc R . . C90 C 1.1586(3) -0.1399(2) 0.2867(2) 0.0237(10) Uani 1 1 d . . . C91 C 1.1548(3) -0.2249(2) 0.2697(2) 0.0231(10) Uani 1 1 d . . . H57 H 1.1098 -0.2402 0.2477 0.028 Uiso 1 1 calc R . . C92 C 1.2142(3) -0.2857(3) 0.2839(2) 0.0268(10) Uani 1 1 d . . . H58 H 1.2105 -0.3428 0.2716 0.032 Uiso 1 1 calc R . . C93 C 1.2808(3) -0.2653(2) 0.3164(2) 0.0232(10) Uani 1 1 d . . . C94 C 1.2870(3) -0.1799(3) 0.3321(2) 0.0277(11) Uani 1 1 d . . . H59 H 1.3332 -0.1642 0.3529 0.033 Uiso 1 1 calc R . . C95 C 1.2263(3) -0.1189(3) 0.3175(2) 0.0263(10) Uani 1 1 d . . . H60 H 1.2307 -0.0613 0.3287 0.032 Uiso 1 1 calc R . . C96 C 1.3452(3) -0.3299(3) 0.3328(2) 0.0281(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0357(7) 0.0393(6) 0.0366(6) -0.0109(5) -0.0124(5) -0.0007(5) Cl2 0.0681(10) 0.0532(8) 0.0508(8) -0.0073(6) -0.0181(7) -0.0062(7) O1 0.029(2) 0.0373(18) 0.058(2) -0.0078(15) -0.0098(17) -0.0160(16) O2 0.062(2) 0.0274(17) 0.0472(19) 0.0000(15) -0.0289(18) -0.0175(16) O3 0.035(2) 0.0273(17) 0.052(2) -0.0085(15) -0.0131(18) 0.0109(15) O4 0.021(2) 0.0360(18) 0.068(2) 0.0081(16) 0.0002(17) 0.0067(16) O5 0.037(2) 0.0200(15) 0.0442(18) -0.0069(13) -0.0125(15) -0.0124(14) O6 0.0326(19) 0.0225(16) 0.0375(17) -0.0092(14) -0.0064(15) -0.0057(15) O7 0.0240(18) 0.0391(17) 0.0350(17) -0.0100(14) -0.0108(14) 0.0065(14) O8 0.0274(18) 0.0230(16) 0.0514(19) -0.0011(14) -0.0107(15) 0.0075(14) N1 0.015(2) 0.0167(18) 0.034(2) -0.0086(15) -0.0088(16) 0.0055(16) N2 0.024(2) 0.0149(17) 0.0278(19) -0.0152(14) -0.0076(17) 0.0019(16) N3 0.024(2) 0.0197(17) 0.0283(18) -0.0114(14) -0.0185(16) 0.0036(15) N4 0.023(2) 0.0101(15) 0.0307(19) -0.0040(14) -0.0072(16) -0.0020(15) C1 0.023(3) 0.017(2) 0.029(2) -0.0072(17) -0.012(2) 0.0033(19) C2 0.023(3) 0.019(2) 0.027(2) -0.0072(18) -0.011(2) 0.001(2) C3 0.018(2) 0.023(2) 0.026(2) -0.0082(18) -0.005(2) -0.0002(19) C4 0.018(3) 0.020(2) 0.029(2) -0.0059(18) -0.006(2) -0.0050(19) C5 0.016(3) 0.021(2) 0.024(2) -0.0030(17) -0.0046(19) -0.0034(19) C6 0.024(3) 0.018(2) 0.024(2) -0.0045(17) -0.009(2) -0.007(2) C7 0.021(3) 0.019(2) 0.025(2) -0.0046(18) -0.0090(19) -0.0007(19) C8 0.024(3) 0.017(2) 0.023(2) -0.0061(17) -0.009(2) 0.0005(19) C9 0.023(3) 0.016(2) 0.026(2) -0.0084(17) -0.012(2) 0.0027(19) C10 0.021(2) 0.019(2) 0.023(2) -0.0091(17) -0.0099(19) 0.0031(19) C11 0.023(3) 0.025(2) 0.029(2) -0.0074(18) -0.006(2) 0.000(2) C12 0.026(3) 0.022(2) 0.027(2) -0.0128(17) -0.013(2) 0.0006(19) C13 0.021(2) 0.021(2) 0.025(2) -0.0094(17) -0.0071(19) 0.0009(18) C14 0.017(2) 0.019(2) 0.028(2) -0.0059(17) -0.0036(19) 0.0011(18) C15 0.031(3) 0.025(2) 0.025(2) -0.0084(18) -0.010(2) -0.006(2) C16 0.022(3) 0.0142(19) 0.032(2) -0.0141(17) -0.009(2) 0.0045(18) C17 0.025(3) 0.021(2) 0.024(2) -0.0084(17) -0.0098(19) -0.0031(19) C18 0.026(3) 0.024(2) 0.023(2) -0.0042(17) -0.0081(19) -0.0023(19) C19 0.029(3) 0.0135(19) 0.030(2) -0.0084(17) -0.015(2) 0.0051(19) C20 0.020(2) 0.023(2) 0.023(2) -0.0048(17) -0.0064(19) -0.0021(19) C21 0.026(3) 0.022(2) 0.024(2) -0.0025(18) -0.003(2) -0.008(2) C22 0.039(3) 0.024(2) 0.036(3) -0.009(2) -0.006(2) -0.001(2) C23 0.047(4) 0.024(3) 0.043(3) -0.010(2) -0.002(3) -0.007(2) C24 0.052(4) 0.024(2) 0.037(3) -0.010(2) 0.009(3) 0.005(3) C25 0.036(3) 0.025(2) 0.042(3) -0.007(2) 0.005(2) 0.000(2) C26 0.034(3) 0.027(3) 0.032(2) -0.001(2) -0.006(2) 0.002(2) C27 0.020(3) 0.020(2) 0.029(2) -0.0105(17) -0.0065(19) -0.0013(18) C28 0.028(3) 0.025(2) 0.023(2) -0.0069(18) -0.006(2) 0.005(2) C29 0.019(3) 0.035(2) 0.033(2) -0.009(2) -0.004(2) -0.004(2) C30 0.038(3) 0.035(3) 0.033(3) -0.003(2) 0.004(2) -0.008(2) C31 0.045(3) 0.026(2) 0.022(2) -0.0040(18) -0.003(2) 0.007(2) C32 0.027(3) 0.030(2) 0.028(2) -0.0103(19) -0.008(2) 0.005(2) C33 0.021(2) 0.020(2) 0.023(2) -0.0082(17) -0.0048(19) -0.0002(18) C34 0.024(3) 0.0145(19) 0.031(2) -0.0097(17) -0.009(2) -0.0010(19) C35 0.022(3) 0.028(2) 0.036(2) -0.0062(19) -0.014(2) -0.002(2) C36 0.029(3) 0.025(2) 0.027(2) -0.0127(18) -0.004(2) -0.003(2) C37 0.035(3) 0.019(2) 0.030(2) -0.0032(18) -0.008(2) -0.005(2) C38 0.023(3) 0.023(2) 0.031(2) -0.0082(18) -0.006(2) 0.0006(19) C39 0.031(3) 0.025(2) 0.028(2) -0.0044(19) -0.007(2) -0.001(2) C40 0.015(2) 0.023(2) 0.018(2) -0.0109(17) 0.0006(18) 0.0011(18) C41 0.030(3) 0.025(2) 0.030(2) -0.0077(18) -0.011(2) -0.004(2) C42 0.035(3) 0.043(3) 0.028(2) -0.002(2) -0.014(2) 0.000(2) C43 0.030(3) 0.051(3) 0.034(3) -0.017(2) -0.014(2) -0.006(2) C44 0.031(3) 0.034(2) 0.041(3) -0.012(2) -0.013(2) -0.007(2) C45 0.032(3) 0.023(2) 0.028(2) -0.0099(18) -0.006(2) 0.002(2) C46 0.022(2) 0.020(2) 0.023(2) -0.0084(17) -0.011(2) 0.0036(19) C47 0.020(3) 0.026(2) 0.029(2) -0.0080(19) -0.009(2) 0.002(2) C48 0.034(3) 0.027(2) 0.031(2) -0.013(2) -0.012(2) 0.001(2) C49 0.032(3) 0.039(3) 0.030(2) -0.016(2) -0.007(2) 0.007(2) C50 0.039(3) 0.037(3) 0.028(3) -0.004(2) -0.006(2) -0.013(2) C51 0.025(3) 0.028(2) 0.026(2) -0.0081(19) -0.008(2) 0.000(2) C52 0.026(3) 0.020(2) 0.025(2) -0.0084(17) -0.012(2) 0.001(2) C53 0.029(3) 0.027(2) 0.028(2) -0.0060(19) -0.013(2) -0.003(2) C54 0.029(3) 0.018(2) 0.038(3) -0.0011(19) -0.015(2) 0.006(2) C55 0.026(3) 0.027(2) 0.022(2) -0.0042(18) -0.007(2) 0.005(2) C56 0.022(3) 0.033(2) 0.030(2) -0.0045(19) -0.009(2) 0.002(2) C57 0.023(3) 0.024(2) 0.031(2) -0.0092(18) -0.011(2) 0.003(2) C58 0.035(3) 0.023(2) 0.033(2) -0.0045(19) -0.012(2) 0.007(2) C59 0.030(3) 0.015(2) 0.033(2) -0.0120(18) -0.015(2) 0.000(2) C60 0.041(3) 0.045(3) 0.049(3) 0.006(2) -0.009(3) 0.003(3) C61 0.076(5) 0.073(4) 0.058(4) 0.027(3) -0.008(4) -0.002(4) C62 0.086(5) 0.047(3) 0.058(4) 0.017(3) -0.032(4) 0.004(3) C63 0.055(4) 0.036(3) 0.056(3) -0.011(2) -0.036(3) 0.009(3) C64 0.043(3) 0.031(2) 0.040(3) -0.007(2) -0.019(2) 0.002(2) C65 0.025(3) 0.019(2) 0.026(2) -0.0041(18) -0.008(2) -0.003(2) C66 0.029(3) 0.022(2) 0.026(2) -0.0079(18) -0.010(2) 0.008(2) C67 0.032(3) 0.029(2) 0.036(3) -0.005(2) -0.019(2) 0.000(2) C68 0.042(3) 0.026(2) 0.030(2) -0.009(2) -0.018(2) -0.003(2) C69 0.037(3) 0.030(2) 0.027(2) -0.0132(19) -0.008(2) 0.000(2) C70 0.026(3) 0.029(2) 0.027(2) -0.0084(19) -0.007(2) 0.003(2) C71 0.031(3) 0.018(2) 0.025(2) -0.0031(18) -0.012(2) -0.003(2) C72 0.025(3) 0.027(2) 0.028(2) -0.0062(18) -0.010(2) -0.001(2) C73 0.025(3) 0.027(2) 0.035(2) -0.003(2) -0.012(2) -0.002(2) C74 0.026(3) 0.024(2) 0.026(2) -0.0001(19) -0.009(2) -0.005(2) C75 0.034(3) 0.012(2) 0.043(3) -0.0057(18) -0.017(2) -0.002(2) C76 0.016(2) 0.020(2) 0.044(3) -0.0090(19) -0.011(2) -0.0011(19) C77 0.024(3) 0.020(2) 0.032(2) 0.0016(19) -0.008(2) -0.006(2) C78 0.022(3) 0.027(2) 0.029(2) -0.0020(19) -0.011(2) 0.004(2) C79 0.040(3) 0.047(3) 0.044(3) -0.009(3) -0.004(3) -0.006(3) C80 0.048(4) 0.090(5) 0.050(3) -0.011(3) 0.002(3) 0.006(4) C81 0.036(4) 0.077(4) 0.057(4) 0.013(3) 0.002(3) -0.018(3) C82 0.030(3) 0.038(3) 0.065(4) 0.006(3) -0.013(3) -0.011(3) C83 0.033(3) 0.034(3) 0.038(3) 0.000(2) -0.007(2) -0.003(2) C84 0.014(2) 0.017(2) 0.024(2) -0.0042(16) -0.0018(18) 0.0010(18) C85 0.020(2) 0.021(2) 0.029(2) -0.0042(18) -0.0060(19) -0.0040(19) C86 0.032(3) 0.024(2) 0.032(2) -0.0013(19) -0.009(2) -0.002(2) C87 0.034(3) 0.033(2) 0.025(2) 0.0006(19) -0.014(2) 0.004(2) C88 0.031(3) 0.028(2) 0.023(2) -0.0085(18) -0.011(2) -0.005(2) C89 0.033(3) 0.024(2) 0.027(2) -0.0043(18) -0.013(2) -0.005(2) C90 0.022(3) 0.019(2) 0.029(2) -0.0021(17) -0.007(2) -0.0011(19) C91 0.020(2) 0.022(2) 0.027(2) -0.0059(18) -0.0059(19) 0.0021(19) C92 0.028(3) 0.020(2) 0.029(2) -0.0067(18) -0.002(2) 0.003(2) C93 0.014(2) 0.024(2) 0.030(2) -0.0029(18) -0.0039(19) 0.0031(19) C94 0.026(3) 0.028(2) 0.031(2) -0.0035(19) -0.012(2) 0.000(2) C95 0.025(3) 0.020(2) 0.039(3) -0.0095(19) -0.015(2) 0.002(2) C96 0.029(3) 0.024(2) 0.026(2) -0.0049(18) 0.002(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C39 1.278(5) . ? O2 C39 1.254(5) . ? O3 C58 1.282(5) . ? O4 C58 1.254(5) . ? O5 C77 1.307(5) . ? O6 C77 1.244(5) . ? O7 C96 1.259(5) . ? O8 C96 1.300(5) . ? N1 C1 1.355(5) . ? N1 C4 1.369(5) . ? N2 C6 1.365(5) . ? N2 C9 1.386(5) . ? N3 C11 1.353(5) . ? N3 C14 1.367(5) . ? N4 C16 1.350(5) . ? N4 C19 1.372(5) . ? C1 C20 1.424(5) . ? C1 C2 1.429(6) . ? C2 C3 1.386(5) . ? C2 C21 1.483(6) . ? C3 C4 1.432(6) . ? C3 C27 1.474(5) . ? C4 C5 1.392(6) . ? C5 C6 1.390(6) . ? C5 C33 1.482(5) . ? C6 C7 1.443(6) . ? C7 C8 1.394(5) . ? C7 C40 1.485(5) . ? C8 C46 1.452(6) . ? C8 C9 1.464(5) . ? C9 C10 1.389(5) . ? C10 C52 1.444(6) . ? C10 C11 1.444(5) . ? C11 C12 1.434(5) . ? C12 C13 1.387(5) . ? C12 C59 1.496(5) . ? C13 C14 1.439(5) . ? C13 C65 1.470(5) . ? C14 C15 1.401(5) . ? C15 C16 1.418(5) . ? C15 C71 1.483(5) . ? C16 C17 1.431(5) . ? C17 C18 1.370(5) . ? C17 C78 1.498(5) . ? C18 C19 1.441(5) . ? C18 C84 1.473(5) . ? C19 C20 1.389(5) . ? C20 C90 1.486(5) . ? C21 C26 1.375(6) . ? C21 C22 1.393(6) . ? C22 C23 1.368(6) . ? C23 C24 1.368(7) . ? C24 C25 1.379(6) . ? C25 C26 1.366(6) . ? C27 C28 1.385(5) . ? C27 C32 1.395(5) . ? C28 C29 1.374(5) . ? C29 C30 1.375(6) . ? C30 C31 1.366(6) . ? C31 C32 1.384(6) . ? C33 C38 1.389(5) . ? C33 C34 1.390(5) . ? C34 C35 1.370(5) . ? C35 C36 1.404(5) . ? C36 C37 1.375(6) . ? C36 C39 1.492(5) . ? C37 C38 1.398(5) . ? C40 C45 1.370(5) . ? C40 C41 1.387(5) . ? C41 C42 1.374(5) . ? C42 C43 1.368(6) . ? C43 C44 1.380(6) . ? C44 C45 1.367(5) . ? C46 C51 1.386(5) . ? C46 C47 1.393(5) . ? C47 C48 1.393(6) . ? C48 C49 1.390(6) . ? C49 C50 1.392(6) . ? C50 C51 1.368(6) . ? C52 C57 1.391(6) . ? C52 C53 1.400(5) . ? C53 C54 1.382(6) . ? C54 C55 1.368(6) . ? C55 C56 1.395(6) . ? C55 C58 1.486(6) . ? C56 C57 1.384(6) . ? C59 C64 1.366(6) . ? C59 C60 1.369(6) . ? C60 C61 1.387(7) . ? C61 C62 1.379(8) . ? C62 C63 1.366(7) . ? C63 C64 1.404(6) . ? C65 C66 1.383(6) . ? C65 C70 1.393(6) . ? C66 C67 1.381(5) . ? C67 C68 1.378(6) . ? C68 C69 1.381(6) . ? C69 C70 1.385(6) . ? C71 C72 1.393(6) . ? C71 C76 1.394(6) . ? C72 C73 1.377(5) . ? C73 C74 1.394(6) . ? C74 C75 1.404(6) . ? C74 C77 1.468(5) . ? C75 C76 1.389(5) . ? C78 C79 1.373(6) . ? C78 C83 1.379(6) . ? C79 C80 1.380(7) . ? C80 C81 1.394(8) . ? C81 C82 1.358(8) . ? C82 C83 1.372(6) . ? C84 C85 1.390(5) . ? C84 C89 1.395(5) . ? C85 C86 1.375(5) . ? C86 C87 1.389(5) . ? C87 C88 1.372(5) . ? C88 C89 1.359(5) . ? C90 C95 1.390(5) . ? C90 C91 1.401(5) . ? C91 C92 1.356(5) . ? C92 C93 1.394(5) . ? C93 C94 1.403(6) . ? C93 C96 1.463(6) . ? C94 C95 1.375(6) . ? 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 C1 N1 C4 110.4(4) . . ? C6 N2 C9 111.1(3) . . ? C11 N3 C14 110.0(3) . . ? C16 N4 C19 110.0(3) . . ? N1 C1 C20 124.6(4) . . ? N1 C1 C2 108.0(3) . . ? C20 C1 C2 127.4(4) . . ? C3 C2 C1 106.9(4) . . ? C3 C2 C21 130.6(4) . . ? C1 C2 C21 120.9(3) . . ? C2 C3 C4 107.7(3) . . ? C2 C3 C27 126.6(4) . . ? C4 C3 C27 125.2(3) . . ? N1 C4 C5 122.2(4) . . ? N1 C4 C3 107.0(3) . . ? C5 C4 C3 130.8(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 C33 116.9(3) . . ? C4 C5 C33 122.0(4) . . ? N2 C6 C5 124.4(4) . . ? N2 C6 C7 107.1(4) . . ? C5 C6 C7 128.5(3) . . ? C8 C7 C6 108.5(3) . . ? C8 C7 C40 129.7(4) . . ? C6 C7 C40 120.0(4) . . ? C7 C8 C46 128.5(3) . . ? C7 C8 C9 106.5(4) . . ? C46 C8 C9 124.1(4) . . ? N2 C9 C10 123.4(3) . . ? N2 C9 C8 106.6(3) . . ? C10 C9 C8 129.9(4) . . ? C9 C10 C52 123.5(3) . . ? C9 C10 C11 118.4(4) . . ? C52 C10 C11 118.1(3) . . ? N3 C11 C12 108.4(3) . . ? N3 C11 C10 123.8(3) . . ? C12 C11 C10 127.6(4) . . ? C13 C12 C11 106.7(3) . . ? C13 C12 C59 128.1(3) . . ? C11 C12 C59 123.6(3) . . ? C12 C13 C14 107.3(3) . . ? C12 C13 C65 127.6(3) . . ? C14 C13 C65 124.4(3) . . ? N3 C14 C15 121.8(3) . . ? N3 C14 C13 107.3(3) . . ? C15 C14 C13 130.9(3) . . ? C14 C15 C16 121.4(3) . . ? C14 C15 C71 121.9(3) . . ? C16 C15 C71 116.6(3) . . ? N4 C16 C15 123.9(3) . . ? N4 C16 C17 107.9(3) . . ? C15 C16 C17 128.2(3) . . ? C18 C17 C16 107.6(3) . . ? C18 C17 C78 127.3(3) . . ? C16 C17 C78 123.5(3) . . ? C17 C18 C19 107.2(3) . . ? C17 C18 C84 128.3(3) . . ? C19 C18 C84 124.4(3) . . ? N4 C19 C20 121.5(3) . . ? N4 C19 C18 107.1(3) . . ? C20 C19 C18 131.4(3) . . ? C19 C20 C1 121.7(4) . . ? C19 C20 C90 122.2(3) . . ? C1 C20 C90 116.0(3) . . ? C26 C21 C22 119.3(4) . . ? C26 C21 C2 124.0(4) . . ? C22 C21 C2 116.5(4) . . ? C23 C22 C21 120.0(5) . . ? C22 C23 C24 120.4(5) . . ? C23 C24 C25 119.6(5) . . ? C26 C25 C24 120.6(5) . . ? C25 C26 C21 120.1(4) . . ? C28 C27 C32 118.4(4) . . ? C28 C27 C3 121.6(3) . . ? C32 C27 C3 120.0(4) . . ? C29 C28 C27 120.7(4) . . ? C28 C29 C30 120.3(4) . . ? C31 C30 C29 120.1(4) . . ? C30 C31 C32 120.1(4) . . ? C31 C32 C27 120.4(4) . . ? C38 C33 C34 118.7(3) . . ? C38 C33 C5 119.2(3) . . ? C34 C33 C5 122.1(3) . . ? C35 C34 C33 121.5(4) . . ? C34 C35 C36 119.2(4) . . ? C37 C36 C35 120.7(3) . . ? C37 C36 C39 119.9(4) . . ? C35 C36 C39 119.4(4) . . ? C36 C37 C38 119.1(4) . . ? C33 C38 C37 120.9(4) . . ? O2 C39 O1 124.4(4) . . ? O2 C39 C36 118.8(4) . . ? O1 C39 C36 116.8(4) . . ? C45 C40 C41 118.1(3) . . ? C45 C40 C7 124.3(3) . . ? C41 C40 C7 117.4(3) . . ? C42 C41 C40 121.3(4) . . ? C43 C42 C41 119.1(4) . . ? C42 C43 C44 120.7(4) . . ? C45 C44 C43 119.1(4) . . ? C44 C45 C40 121.7(4) . . ? C51 C46 C47 119.1(4) . . ? C51 C46 C8 119.4(3) . . ? C47 C46 C8 121.5(4) . . ? C48 C47 C46 120.3(4) . . ? C49 C48 C47 119.4(4) . . ? C48 C49 C50 120.1(4) . . ? C51 C50 C49 119.9(4) . . ? C50 C51 C46 121.2(4) . . ? C57 C52 C53 118.3(4) . . ? C57 C52 C10 119.3(3) . . ? C53 C52 C10 122.3(4) . . ? C54 C53 C52 120.7(4) . . ? C55 C54 C53 120.4(4) . . ? C54 C55 C56 119.9(4) . . ? C54 C55 C58 121.2(4) . . ? C56 C55 C58 118.8(4) . . ? C57 C56 C55 119.8(4) . . ? C56 C57 C52 120.8(4) . . ? O4 C58 O3 123.7(4) . . ? O4 C58 C55 119.8(4) . . ? O3 C58 C55 116.5(4) . . ? C64 C59 C60 119.6(4) . . ? C64 C59 C12 123.2(4) . . ? C60 C59 C12 117.3(4) . . ? C59 C60 C61 120.1(5) . . ? C62 C61 C60 120.3(5) . . ? C63 C62 C61 119.8(5) . . ? C62 C63 C64 119.3(5) . . ? C59 C64 C63 120.8(4) . . ? C66 C65 C70 119.1(4) . . ? C66 C65 C13 121.1(4) . . ? C70 C65 C13 119.7(4) . . ? C67 C66 C65 121.1(4) . . ? C68 C67 C66 119.3(4) . . ? C67 C68 C69 120.5(4) . . ? C68 C69 C70 120.0(4) . . ? C69 C70 C65 119.9(4) . . ? C72 C71 C76 119.5(4) . . ? C72 C71 C15 122.5(4) . . ? C76 C71 C15 117.9(4) . . ? C73 C72 C71 120.1(4) . . ? C72 C73 C74 120.7(4) . . ? C73 C74 C75 119.7(4) . . ? C73 C74 C77 122.3(4) . . ? C75 C74 C77 118.0(4) . . ? C76 C75 C74 119.1(4) . . ? C75 C76 C71 120.9(4) . . ? O6 C77 O5 123.1(4) . . ? O6 C77 C74 121.1(4) . . ? O5 C77 C74 115.8(4) . . ? C79 C78 C83 118.4(4) . . ? C79 C78 C17 117.2(4) . . ? C83 C78 C17 124.3(4) . . ? C78 C79 C80 120.6(5) . . ? C79 C80 C81 120.1(6) . . ? C82 C81 C80 119.1(5) . . ? C81 C82 C83 120.5(5) . . ? C82 C83 C78 121.3(5) . . ? C85 C84 C89 118.7(3) . . ? C85 C84 C18 120.6(3) . . ? C89 C84 C18 120.6(3) . . ? C86 C85 C84 120.2(4) . . ? C85 C86 C87 120.2(4) . . ? C88 C87 C86 119.3(4) . . ? C89 C88 C87 121.0(4) . . ? C88 C89 C84 120.5(4) . . ? C95 C90 C91 118.2(4) . . ? C95 C90 C20 120.0(3) . . ? C91 C90 C20 121.8(3) . . ? C92 C91 C90 121.2(4) . . ? C91 C92 C93 120.7(4) . . ? C92 C93 C94 118.8(4) . . ? C92 C93 C96 121.8(4) . . ? C94 C93 C96 119.4(3) . . ? C95 C94 C93 119.9(4) . . ? C94 C95 C90 121.2(4) . . ? O7 C96 O8 122.8(4) . . ? O7 C96 C93 121.9(4) . . ? O8 C96 C93 115.2(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 C4 N1 C1 C20 176.0(3) . . . . ? C4 N1 C1 C2 -3.7(4) . . . . ? N1 C1 C2 C3 2.3(4) . . . . ? C20 C1 C2 C3 -177.4(3) . . . . ? N1 C1 C2 C21 -164.8(3) . . . . ? C20 C1 C2 C21 15.5(6) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C21 C2 C3 C4 165.3(4) . . . . ? C1 C2 C3 C27 -171.7(3) . . . . ? C21 C2 C3 C27 -6.3(6) . . . . ? C1 N1 C4 C5 -173.2(3) . . . . ? C1 N1 C4 C3 3.6(4) . . . . ? C2 C3 C4 N1 -2.1(4) . . . . ? C27 C3 C4 N1 169.7(3) . . . . ? C2 C3 C4 C5 174.3(4) . . . . ? C27 C3 C4 C5 -13.9(6) . . . . ? N1 C4 C5 C6 -23.1(5) . . . . ? C3 C4 C5 C6 161.0(4) . . . . ? N1 C4 C5 C33 154.2(3) . . . . ? C3 C4 C5 C33 -21.6(6) . . . . ? C9 N2 C6 C5 -177.0(3) . . . . ? C9 N2 C6 C7 3.2(4) . . . . ? C4 C5 C6 N2 -40.3(5) . . . . ? C33 C5 C6 N2 142.3(3) . . . . ? C4 C5 C6 C7 139.4(4) . . . . ? C33 C5 C6 C7 -38.0(5) . . . . ? N2 C6 C7 C8 -1.2(4) . . . . ? C5 C6 C7 C8 179.1(3) . . . . ? N2 C6 C7 C40 164.9(3) . . . . ? C5 C6 C7 C40 -14.8(5) . . . . ? C6 C7 C8 C46 168.2(3) . . . . ? C40 C7 C8 C46 3.9(6) . . . . ? C6 C7 C8 C9 -1.2(4) . . . . ? C40 C7 C8 C9 -165.5(3) . . . . ? C6 N2 C9 C10 173.7(3) . . . . ? C6 N2 C9 C8 -3.9(4) . . . . ? C7 C8 C9 N2 3.0(4) . . . . ? C46 C8 C9 N2 -166.9(3) . . . . ? C7 C8 C9 C10 -174.4(4) . . . . ? C46 C8 C9 C10 15.6(6) . . . . ? N2 C9 C10 C52 -157.1(3) . . . . ? C8 C9 C10 C52 20.0(6) . . . . ? N2 C9 C10 C11 25.5(5) . . . . ? C8 C9 C10 C11 -157.4(4) . . . . ? C14 N3 C11 C12 -3.6(5) . . . . ? C14 N3 C11 C10 173.3(4) . . . . ? C9 C10 C11 N3 40.5(6) . . . . ? C52 C10 C11 N3 -137.1(4) . . . . ? C9 C10 C11 C12 -143.3(4) . . . . ? C52 C10 C11 C12 39.1(6) . . . . ? N3 C11 C12 C13 1.2(5) . . . . ? C10 C11 C12 C13 -175.5(4) . . . . ? N3 C11 C12 C59 -165.5(4) . . . . ? C10 C11 C12 C59 17.8(7) . . . . ? C11 C12 C13 C14 1.5(5) . . . . ? C59 C12 C13 C14 167.4(4) . . . . ? C11 C12 C13 C65 -169.4(4) . . . . ? C59 C12 C13 C65 -3.5(7) . . . . ? C11 N3 C14 C15 -173.3(4) . . . . ? C11 N3 C14 C13 4.5(4) . . . . ? C12 C13 C14 N3 -3.6(5) . . . . ? C65 C13 C14 N3 167.6(4) . . . . ? C12 C13 C14 C15 173.9(4) . . . . ? C65 C13 C14 C15 -14.9(7) . . . . ? N3 C14 C15 C16 -25.0(6) . . . . ? C13 C14 C15 C16 157.8(4) . . . . ? N3 C14 C15 C71 158.7(4) . . . . ? C13 C14 C15 C71 -18.4(7) . . . . ? C19 N4 C16 C15 -173.7(4) . . . . ? C19 N4 C16 C17 4.7(4) . . . . ? C14 C15 C16 N4 -35.0(6) . . . . ? C71 C15 C16 N4 141.4(4) . . . . ? C14 C15 C16 C17 146.9(4) . . . . ? C71 C15 C16 C17 -36.6(6) . . . . ? N4 C16 C17 C18 -2.9(4) . . . . ? C15 C16 C17 C18 175.5(4) . . . . ? N4 C16 C17 C78 163.7(4) . . . . ? C15 C16 C17 C78 -17.9(6) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C78 C17 C18 C19 -165.9(4) . . . . ? C16 C17 C18 C84 176.2(4) . . . . ? C78 C17 C18 C84 10.3(7) . . . . ? C16 N4 C19 C20 172.1(4) . . . . ? C16 N4 C19 C18 -4.6(4) . . . . ? C17 C18 C19 N4 2.7(4) . . . . ? C84 C18 C19 N4 -173.6(4) . . . . ? C17 C18 C19 C20 -173.6(4) . . . . ? C84 C18 C19 C20 10.1(7) . . . . ? N4 C19 C20 C1 22.6(6) . . . . ? C18 C19 C20 C1 -161.5(4) . . . . ? N4 C19 C20 C90 -158.4(4) . . . . ? C18 C19 C20 C90 17.4(7) . . . . ? N1 C1 C20 C19 35.8(6) . . . . ? C2 C1 C20 C19 -144.6(4) . . . . ? N1 C1 C20 C90 -143.3(4) . . . . ? C2 C1 C20 C90 36.4(5) . . . . ? C3 C2 C21 C26 77.1(5) . . . . ? C1 C2 C21 C26 -119.2(4) . . . . ? C3 C2 C21 C22 -107.5(5) . . . . ? C1 C2 C21 C22 56.2(5) . . . . ? C26 C21 C22 C23 0.7(6) . . . . ? C2 C21 C22 C23 -174.9(3) . . . . ? C21 C22 C23 C24 0.3(6) . . . . ? C22 C23 C24 C25 -1.6(6) . . . . ? C23 C24 C25 C26 1.9(6) . . . . ? C24 C25 C26 C21 -0.9(6) . . . . ? C22 C21 C26 C25 -0.4(6) . . . . ? C2 C21 C26 C25 174.8(4) . . . . ? C2 C3 C27 C28 -60.4(5) . . . . ? C4 C3 C27 C28 129.4(4) . . . . ? C2 C3 C27 C32 121.7(4) . . . . ? C4 C3 C27 C32 -48.5(5) . . . . ? C32 C27 C28 C29 -0.2(6) . . . . ? C3 C27 C28 C29 -178.1(4) . . . . ? C27 C28 C29 C30 0.9(6) . . . . ? C28 C29 C30 C31 -1.7(7) . . . . ? C29 C30 C31 C32 1.7(7) . . . . ? C30 C31 C32 C27 -1.0(6) . . . . ? C28 C27 C32 C31 0.2(6) . . . . ? C3 C27 C32 C31 178.2(4) . . . . ? C6 C5 C33 C38 -42.7(5) . . . . ? C4 C5 C33 C38 139.8(4) . . . . ? C6 C5 C33 C34 135.7(4) . . . . ? C4 C5 C33 C34 -41.8(6) . . . . ? C38 C33 C34 C35 -1.4(6) . . . . ? C5 C33 C34 C35 -179.8(4) . . . . ? C33 C34 C35 C36 1.8(6) . . . . ? C34 C35 C36 C37 -1.0(6) . . . . ? C34 C35 C36 C39 177.9(4) . . . . ? C35 C36 C37 C38 -0.1(6) . . . . ? C39 C36 C37 C38 -179.0(4) . . . . ? C34 C33 C38 C37 0.3(6) . . . . ? C5 C33 C38 C37 178.8(4) . . . . ? C36 C37 C38 C33 0.4(6) . . . . ? C37 C36 C39 O2 9.4(6) . . . . ? C35 C36 C39 O2 -169.5(4) . . . . ? C37 C36 C39 O1 -171.9(4) . . . . ? C35 C36 C39 O1 9.2(6) . . . . ? C8 C7 C40 C45 -75.3(5) . . . . ? C6 C7 C40 C45 122.0(4) . . . . ? C8 C7 C40 C41 110.7(5) . . . . ? C6 C7 C40 C41 -52.0(5) . . . . ? C45 C40 C41 C42 -1.3(6) . . . . ? C7 C40 C41 C42 173.0(4) . . . . ? C40 C41 C42 C43 1.0(7) . . . . ? C41 C42 C43 C44 1.3(7) . . . . ? C42 C43 C44 C45 -3.1(7) . . . . ? C43 C44 C45 C40 2.8(7) . . . . ? C41 C40 C45 C44 -0.6(6) . . . . ? C7 C40 C45 C44 -174.5(4) . . . . ? C7 C8 C46 C51 -120.3(4) . . . . ? C9 C8 C46 C51 47.4(5) . . . . ? C7 C8 C46 C47 60.4(5) . . . . ? C9 C8 C46 C47 -131.9(4) . . . . ? C51 C46 C47 C48 0.2(5) . . . . ? C8 C46 C47 C48 179.5(3) . . . . ? C46 C47 C48 C49 -1.3(6) . . . . ? C47 C48 C49 C50 2.0(6) . . . . ? C48 C49 C50 C51 -1.6(6) . . . . ? C49 C50 C51 C46 0.5(6) . . . . ? C47 C46 C51 C50 0.2(6) . . . . ? C8 C46 C51 C50 -179.2(4) . . . . ? C9 C10 C52 C57 -137.2(4) . . . . ? C11 C10 C52 C57 40.3(5) . . . . ? C9 C10 C52 C53 38.6(5) . . . . ? C11 C10 C52 C53 -144.0(4) . . . . ? C57 C52 C53 C54 2.7(5) . . . . ? C10 C52 C53 C54 -173.1(3) . . . . ? C52 C53 C54 C55 -2.0(6) . . . . ? C53 C54 C55 C56 -0.7(6) . . . . ? C53 C54 C55 C58 -180.0(3) . . . . ? C54 C55 C56 C57 2.6(6) . . . . ? C58 C55 C56 C57 -178.1(3) . . . . ? C55 C56 C57 C52 -1.8(6) . . . . ? C53 C52 C57 C56 -0.8(5) . . . . ? C10 C52 C57 C56 175.1(3) . . . . ? C54 C55 C58 O4 168.9(4) . . . . ? C56 C55 C58 O4 -10.4(5) . . . . ? C54 C55 C58 O3 -11.0(5) . . . . ? C56 C55 C58 O3 169.7(4) . . . . ? C13 C12 C59 C64 86.7(6) . . . . ? C11 C12 C59 C64 -109.6(5) . . . . ? C13 C12 C59 C60 -93.4(5) . . . . ? C11 C12 C59 C60 70.3(6) . . . . ? C64 C59 C60 C61 -1.8(7) . . . . ? C12 C59 C60 C61 178.3(5) . . . . ? C59 C60 C61 C62 3.1(9) . . . . ? C60 C61 C62 C63 -2.1(9) . . . . ? C61 C62 C63 C64 -0.1(8) . . . . ? C60 C59 C64 C63 -0.4(6) . . . . ? C12 C59 C64 C63 179.5(4) . . . . ? C62 C63 C64 C59 1.4(7) . . . . ? C12 C13 C65 C66 -57.2(6) . . . . ? C14 C13 C65 C66 133.3(4) . . . . ? C12 C13 C65 C70 125.3(5) . . . . ? C14 C13 C65 C70 -44.2(5) . . . . ? C70 C65 C66 C67 2.5(5) . . . . ? C13 C65 C66 C67 -175.1(3) . . . . ? C65 C66 C67 C68 0.4(6) . . . . ? C66 C67 C68 C69 -2.4(6) . . . . ? C67 C68 C69 C70 1.5(6) . . . . ? C68 C69 C70 C65 1.3(6) . . . . ? C66 C65 C70 C69 -3.3(5) . . . . ? C13 C65 C70 C69 174.3(3) . . . . ? C14 C15 C71 C72 -43.0(6) . . . . ? C16 C15 C71 C72 140.6(4) . . . . ? C14 C15 C71 C76 133.3(4) . . . . ? C16 C15 C71 C76 -43.1(5) . . . . ? C76 C71 C72 C73 -1.6(5) . . . . ? C15 C71 C72 C73 174.7(3) . . . . ? C71 C72 C73 C74 0.8(6) . . . . ? C72 C73 C74 C75 0.2(6) . . . . ? C72 C73 C74 C77 -177.8(3) . . . . ? C73 C74 C75 C76 -0.3(5) . . . . ? C77 C74 C75 C76 177.8(3) . . . . ? C74 C75 C76 C71 -0.5(6) . . . . ? C72 C71 C76 C75 1.5(6) . . . . ? C15 C71 C76 C75 -174.9(3) . . . . ? C73 C74 C77 O6 -174.2(4) . . . . ? C75 C74 C77 O6 7.7(5) . . . . ? C73 C74 C77 O5 5.6(5) . . . . ? C75 C74 C77 O5 -172.5(3) . . . . ? C18 C17 C78 C79 94.0(5) . . . . ? C16 C17 C78 C79 -69.9(5) . . . . ? C18 C17 C78 C83 -86.3(5) . . . . ? C16 C17 C78 C83 109.8(5) . . . . ? C83 C78 C79 C80 0.8(7) . . . . ? C17 C78 C79 C80 -179.4(4) . . . . ? C78 C79 C80 C81 -1.4(8) . . . . ? C79 C80 C81 C82 0.9(8) . . . . ? C80 C81 C82 C83 0.1(8) . . . . ? C81 C82 C83 C78 -0.7(7) . . . . ? C79 C78 C83 C82 0.2(6) . . . . ? C17 C78 C83 C82 -179.5(4) . . . . ? C17 C18 C84 C85 56.2(6) . . . . ? C19 C18 C84 C85 -128.3(4) . . . . ? C17 C18 C84 C89 -128.0(5) . . . . ? C19 C18 C84 C89 47.5(6) . . . . ? C89 C84 C85 C86 -1.7(6) . . . . ? C18 C84 C85 C86 174.1(4) . . . . ? C84 C85 C86 C87 -0.7(6) . . . . ? C85 C86 C87 C88 3.1(6) . . . . ? C86 C87 C88 C89 -3.2(7) . . . . ? C87 C88 C89 C84 0.7(7) . . . . ? C85 C84 C89 C88 1.7(6) . . . . ? C18 C84 C89 C88 -174.1(4) . . . . ? C19 C20 C90 C95 -132.9(4) . . . . ? C1 C20 C90 C95 46.1(5) . . . . ? C19 C20 C90 C91 47.9(6) . . . . ? C1 C20 C90 C91 -133.0(4) . . . . ? C95 C90 C91 C92 1.2(6) . . . . ? C20 C90 C91 C92 -179.6(4) . . . . ? C90 C91 C92 C93 0.3(6) . . . . ? C91 C92 C93 C94 -1.9(6) . . . . ? C91 C92 C93 C96 179.5(4) . . . . ? C92 C93 C94 C95 2.0(6) . . . . ? C96 C93 C94 C95 -179.4(4) . . . . ? C93 C94 C95 C90 -0.5(6) . . . . ? C91 C90 C95 C94 -1.1(6) . . . . ? C20 C90 C95 C94 179.7(4) . . . . ? C92 C93 C96 O7 173.7(4) . . . . ? C94 C93 C96 O7 -4.9(6) . . . . ? C92 C93 C96 O8 -6.3(6) . . . . ? C94 C93 C96 O8 175.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.74 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.445 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.069 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 0.000 619 143 ' ' 2 -0.016 0.000 0.500 583 121 ' ' 3 0.500 0.500 0.000 33 2 ' ' 4 0.500 0.500 0.500 36 3 ' ' _platon_squeeze_details 'Five MeOH and four water molecules per asymmetric unit were deleted with the squeeze program' # Attachment 'H4OCDPP2Cl-rev2.CIF' data_sankar77 _database_code_depnum_ccdc_archive 'CCDC 866779' #TrackingRef 'H4OCDPP2Cl-rev2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H172 Cl2 N4 O24' _chemical_formula_weight 2437.78 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 36.043(11) _cell_length_b 18.849(6) _cell_length_c 20.929(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.756(4) _cell_angle_gamma 90.00 _cell_volume 12806(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5208 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9635 _exptl_absorpt_correction_T_max 0.9938 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker APEXII' _diffrn_measurement_method '2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19439 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 20.48 _reflns_number_total 6576 _reflns_number_gt 3865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2009, 11, 0, 0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009' _computing_publication_material 'Mercury CSD 3.0.1' _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^)+(0.1310P)^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 6576 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2215 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Cl1 Cl 0.78593(6) 0.0000 0.47952(9) 0.0493(6) Uani 1 2 d S . . Cl2 Cl 0.90726(7) 0.0000 0.43374(12) 0.0757(7) Uani 1 2 d S . . O1 O 0.76453(16) 0.18532(18) 0.07191(19) 0.0860(14) Uani 1 1 d . . . H30 H 0.7498 0.1819 0.0280 0.129 Uiso 1 1 calc R . . O2 O 0.74346(18) 0.2980(2) 0.0568(2) 0.1118(19) Uani 1 1 d . . . O3 O 0.76405(15) 0.38224(17) 0.3611(2) 0.0864(14) Uani 1 1 d . . . O4 O 0.74592(14) 0.43255(18) 0.2551(2) 0.0861(14) Uani 1 1 d . . . O5 O 0.85840(18) 0.38473(19) 0.6125(3) 0.0933(14) Uani 1 1 d . . . O6 O 0.91442(16) 0.43085(19) 0.7003(2) 0.0990(16) Uani 1 1 d . . . O7 O 1.02554(16) 0.1551(3) 0.8123(3) 0.1162(17) Uani 1 1 d . . . H31 H 1.0485 0.1537 0.8480 0.174 Uiso 1 1 calc R . . N1 N 0.80907(17) 0.0000 0.3441(3) 0.0370(14) Uani 1 2 d S . . H1 H 0.8343 0.0000 0.3785 0.044 Uiso 1 2 calc SR . . N2 N 0.84624(12) 0.11214(17) 0.4604(2) 0.0407(10) Uani 1 1 d . . . H2 H 0.8329 0.0758 0.4668 0.049 Uiso 1 1 calc R . . N3 N 0.88994(17) 0.0000 0.5709(3) 0.0380(14) Uani 1 2 d S . . H3 H 0.8883 0.0000 0.5277 0.046 Uiso 1 2 calc SR . . C1 C 0.74684(16) 0.0370(2) 0.2608(2) 0.0365(13) Uani 1 1 d . . . C2 C 0.78652(17) 0.0594(2) 0.3133(2) 0.0391(13) Uani 1 1 d . . . C3 C 0.80280(16) 0.1281(2) 0.3320(2) 0.0384(13) Uani 1 1 d . . . C4 C 0.83712(16) 0.1439(2) 0.3960(3) 0.0377(12) Uani 1 1 d . . . C5 C 0.86814(17) 0.1969(2) 0.4093(3) 0.0485(14) Uani 1 1 d . . . C6 C 0.89319(18) 0.1983(3) 0.4804(3) 0.0523(14) Uani 1 1 d . . . C7 C 0.87926(17) 0.1455(2) 0.5134(3) 0.0450(13) Uani 1 1 d . . . C8 C 0.89354(15) 0.1287(2) 0.5855(2) 0.0399(13) Uani 1 1 d . . . C9 C 0.89142(16) 0.0595(2) 0.6101(3) 0.0442(13) Uani 1 1 d . . . C10 C 0.89270(15) 0.0358(2) 0.6759(2) 0.0419(13) Uani 1 1 d . . . C11 C 0.71051(16) 0.0810(2) 0.2209(3) 0.0420(13) Uani 1 1 d . . . C12 C 0.69119(18) 0.1135(3) 0.2581(3) 0.0614(16) Uani 1 1 d . . . H4 H 0.7024 0.1106 0.3083 0.074 Uiso 1 1 calc R . . C13 C 0.6540(2) 0.1513(3) 0.2178(5) 0.088(2) Uani 1 1 d . . . H5 H 0.6397 0.1732 0.2416 0.106 Uiso 1 1 calc R . . C14 C 0.6388(2) 0.1565(3) 0.1470(5) 0.099(2) Uani 1 1 d . . . H6 H 0.6143 0.1829 0.1215 0.119 Uiso 1 1 calc R . . C15 C 0.6582(2) 0.1239(3) 0.1106(4) 0.084(2) Uani 1 1 d . . . H7 H 0.6471 0.1268 0.0604 0.101 Uiso 1 1 calc R . . C16 C 0.6941(2) 0.0873(3) 0.1493(3) 0.0664(17) Uani 1 1 d . . . H8 H 0.7080 0.0656 0.1248 0.080 Uiso 1 1 calc R . . C17 C 0.78477(15) 0.1885(2) 0.2835(2) 0.0384(13) Uani 1 1 d . . . C18 C 0.77760(16) 0.2519(2) 0.3099(3) 0.0491(14) Uani 1 1 d . . . H9 H 0.7827 0.2546 0.3583 0.059 Uiso 1 1 calc R . . C19 C 0.76295(17) 0.3121(2) 0.2666(3) 0.0498(14) Uani 1 1 d . . . C20 C 0.75607(18) 0.3082(2) 0.1973(3) 0.0620(17) Uani 1 1 d . . . H10 H 0.7470 0.3492 0.1681 0.074 Uiso 1 1 calc R . . C21 C 0.76208(18) 0.2457(2) 0.1689(3) 0.0567(16) Uani 1 1 d . . . C22 C 0.77724(16) 0.1852(2) 0.2127(3) 0.0456(14) Uani 1 1 d . . . H11 H 0.7822 0.1424 0.1937 0.055 Uiso 1 1 calc R . . C23 C 0.7560(2) 0.2453(3) 0.0952(3) 0.086(2) Uani 1 1 d . . . C24 C 0.7570(2) 0.3802(3) 0.2971(3) 0.0674(18) Uani 1 1 d . . . C25 C 0.87507(19) 0.2288(3) 0.3511(3) 0.0624(17) Uani 1 1 d . . . C26 C 0.88426(17) 0.1862(3) 0.3067(3) 0.0663(17) Uani 1 1 d . . . H12 H 0.8855 0.1364 0.3142 0.080 Uiso 1 1 calc R . . C27 C 0.8917(2) 0.2118(4) 0.2523(3) 0.090(2) Uani 1 1 d . . . H13 H 0.8985 0.1805 0.2235 0.108 Uiso 1 1 calc R . . C28 C 0.8892(3) 0.2831(5) 0.2402(4) 0.112(3) Uani 1 1 d . . . H14 H 0.8936 0.3016 0.2018 0.135 Uiso 1 1 calc R . . C29 C 0.8804(3) 0.3282(4) 0.2828(4) 0.114(3) Uani 1 1 d . . . H15 H 0.8793 0.3778 0.2743 0.137 Uiso 1 1 calc R . . C30 C 0.8730(2) 0.3022(3) 0.3390(3) 0.084(2) Uani 1 1 d . . . H16 H 0.8667 0.3337 0.3683 0.101 Uiso 1 1 calc R . . C31 C 0.93266(17) 0.2363(3) 0.5169(2) 0.084(2) Uani 1 1 d G . . C32 C 0.9686(2) 0.1966(3) 0.5495(3) 0.141(4) Uani 1 1 d G . . H17 H 0.9674 0.1463 0.5466 0.169 Uiso 1 1 calc R . . C33 C 1.00615(18) 0.2305(5) 0.5865(3) 0.308(13) Uani 1 1 d G . . H18 H 1.0307 0.2034 0.6088 0.370 Uiso 1 1 calc R . . C34 C 1.00784(19) 0.3042(5) 0.5908(3) 0.275(12) Uani 1 1 d G . . H19 H 1.0335 0.3273 0.6160 0.330 Uiso 1 1 calc R . . C35 C 0.9719(3) 0.3438(3) 0.5581(3) 0.221(8) Uani 1 1 d G . . H20 H 0.9731 0.3941 0.5611 0.266 Uiso 1 1 calc R . . C36 C 0.9344(2) 0.3099(3) 0.5212(3) 0.124(3) Uani 1 1 d G . . H21 H 0.9098 0.3370 0.4989 0.149 Uiso 1 1 calc R . . C37 C 0.91369(17) 0.1860(2) 0.6379(3) 0.0451(14) Uani 1 1 d . . . C38 C 0.95041(19) 0.1755(2) 0.6969(3) 0.0564(15) Uani 1 1 d . . . H22 H 0.9623 0.1295 0.7058 0.068 Uiso 1 1 calc R . . C39 C 0.9706(2) 0.2298(3) 0.7438(3) 0.0700(18) Uani 1 1 d . . . C40 C 0.9512(2) 0.2962(3) 0.7310(3) 0.0759(19) Uani 1 1 d . . . H23 H 0.9642 0.3342 0.7627 0.091 Uiso 1 1 calc R . . C41 C 0.9138(2) 0.3080(3) 0.6740(3) 0.0583(15) Uani 1 1 d . . . C42 C 0.89476(17) 0.2528(2) 0.6270(3) 0.0518(14) Uani 1 1 d . . . H24 H 0.8689 0.2604 0.5875 0.062 Uiso 1 1 calc R . . C43 C 0.8947(2) 0.3791(3) 0.6613(4) 0.0652(17) Uani 1 1 d . . . C44 C 1.0106(3) 0.2191(5) 0.8045(4) 0.114(3) Uani 1 1 d . . . O8 O 1.0299(2) 0.2671(3) 0.8438(3) 0.192(4) Uani 1 1 d . . . C45 C 0.8884(2) 0.0827(2) 0.7294(3) 0.0514(15) Uani 1 1 d . . . C46 C 0.9182(2) 0.0878(3) 0.7975(3) 0.0749(19) Uani 1 1 d . . . H25 H 0.9432 0.0624 0.8106 0.090 Uiso 1 1 calc R . . C47 C 0.9132(3) 0.1287(4) 0.8480(3) 0.113(3) Uani 1 1 d . . . H26 H 0.9341 0.1323 0.8952 0.136 Uiso 1 1 calc R . . C48 C 0.8755(4) 0.1646(4) 0.8257(5) 0.116(3) Uani 1 1 d . . . H27 H 0.8708 0.1918 0.8597 0.139 Uiso 1 1 calc R . . C49 C 0.8457(3) 0.1626(3) 0.7590(5) 0.090(2) Uani 1 1 d . . . H28 H 0.8211 0.1892 0.7459 0.108 Uiso 1 1 calc R . . C50 C 0.8516(2) 0.1205(3) 0.7092(3) 0.0645(17) Uani 1 1 d . . . H29 H 0.8307 0.1176 0.6619 0.077 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 Cl1 0.0712(14) 0.0220(9) 0.0647(13) 0.000 0.0388(11) 0.000 Cl2 0.0886(18) 0.0628(13) 0.0802(16) 0.000 0.0409(14) 0.000 O1 0.176(5) 0.031(2) 0.056(3) 0.0071(19) 0.055(3) 0.018(2) O2 0.242(6) 0.036(2) 0.066(3) 0.022(2) 0.074(3) 0.039(3) O3 0.153(4) 0.029(2) 0.073(3) -0.008(2) 0.046(3) 0.015(2) O4 0.139(4) 0.0208(19) 0.090(3) 0.011(2) 0.041(3) 0.008(2) O5 0.133(4) 0.035(2) 0.105(4) -0.002(2) 0.046(4) 0.020(3) O6 0.161(5) 0.027(2) 0.122(4) -0.030(2) 0.072(3) -0.033(3) O7 0.100(4) 0.091(4) 0.097(4) 0.005(3) -0.013(3) 0.001(3) N1 0.056(4) 0.024(3) 0.026(3) 0.000 0.014(3) 0.000 N2 0.062(3) 0.014(2) 0.045(3) 0.005(2) 0.023(2) -0.004(2) N3 0.067(4) 0.022(3) 0.025(3) 0.000 0.020(3) 0.000 C1 0.067(4) 0.015(2) 0.037(3) -0.002(2) 0.031(3) 0.001(3) C2 0.072(4) 0.019(3) 0.031(3) 0.008(2) 0.026(3) 0.009(3) C3 0.061(4) 0.020(3) 0.038(3) -0.002(2) 0.025(3) 0.002(3) C4 0.056(4) 0.021(3) 0.037(3) 0.003(3) 0.020(3) 0.001(3) C5 0.064(4) 0.032(3) 0.048(4) 0.004(3) 0.023(3) -0.018(3) C6 0.070(4) 0.040(3) 0.042(4) 0.000(3) 0.020(3) -0.023(3) C7 0.067(4) 0.027(3) 0.038(4) -0.003(3) 0.021(3) -0.001(3) C8 0.057(4) 0.023(3) 0.037(3) -0.009(2) 0.018(3) -0.005(2) C9 0.061(4) 0.025(3) 0.040(3) -0.003(3) 0.015(3) 0.000(2) C10 0.069(4) 0.022(2) 0.035(3) -0.002(2) 0.024(3) -0.003(2) C11 0.062(4) 0.021(3) 0.036(4) -0.001(2) 0.015(3) 0.001(3) C12 0.072(4) 0.041(3) 0.075(4) 0.014(3) 0.035(4) 0.011(3) C13 0.097(6) 0.065(4) 0.113(6) 0.023(4) 0.056(5) 0.030(4) C14 0.098(6) 0.052(4) 0.104(7) 0.014(5) 0.003(5) 0.023(4) C15 0.115(6) 0.037(3) 0.075(5) 0.004(4) 0.016(5) 0.014(4) C16 0.089(5) 0.030(3) 0.060(5) 0.000(3) 0.014(4) 0.021(3) C17 0.057(4) 0.013(3) 0.041(3) 0.003(2) 0.017(3) -0.002(2) C18 0.085(4) 0.022(3) 0.033(3) -0.002(2) 0.019(3) -0.011(3) C19 0.087(4) 0.016(3) 0.046(4) -0.004(3) 0.029(3) 0.000(3) C20 0.109(5) 0.019(3) 0.056(4) 0.012(3) 0.033(4) 0.003(3) C21 0.102(5) 0.026(3) 0.039(4) 0.002(3) 0.028(3) -0.009(3) C22 0.080(4) 0.011(3) 0.048(4) -0.009(2) 0.030(3) -0.003(3) C23 0.171(7) 0.025(4) 0.059(5) 0.006(3) 0.047(4) 0.005(4) C24 0.125(6) 0.018(3) 0.057(4) 0.002(3) 0.037(4) 0.000(3) C25 0.092(5) 0.049(4) 0.044(4) -0.002(3) 0.027(3) -0.036(3) C26 0.083(5) 0.067(4) 0.055(4) 0.001(3) 0.035(4) -0.030(3) C27 0.141(7) 0.071(5) 0.077(5) -0.011(4) 0.065(5) -0.046(5) C28 0.176(8) 0.130(7) 0.053(5) -0.014(5) 0.070(5) -0.075(6) C29 0.204(9) 0.078(5) 0.075(5) 0.004(4) 0.075(6) -0.065(5) C30 0.134(6) 0.056(4) 0.066(4) -0.006(3) 0.046(4) -0.044(4) C31 0.082(6) 0.114(6) 0.052(4) 0.002(4) 0.025(4) -0.038(5) C32 0.106(7) 0.236(11) 0.070(5) 0.016(6) 0.029(5) -0.077(8) C33 0.130(10) 0.69(4) 0.082(8) 0.045(13) 0.021(7) -0.217(16) C34 0.207(14) 0.56(3) 0.076(8) -0.112(12) 0.082(9) -0.297(18) C35 0.269(16) 0.304(15) 0.095(8) -0.059(9) 0.082(10) -0.242(15) C36 0.177(9) 0.123(7) 0.078(5) -0.030(5) 0.059(6) -0.098(7) C37 0.071(4) 0.030(3) 0.037(3) 0.007(3) 0.026(3) -0.004(3) C38 0.086(5) 0.018(3) 0.050(4) 0.000(3) 0.015(4) -0.006(3) C39 0.095(5) 0.042(4) 0.053(4) -0.005(3) 0.014(4) -0.015(4) C40 0.123(6) 0.027(4) 0.068(5) -0.008(3) 0.032(5) -0.023(4) C41 0.082(5) 0.024(3) 0.059(4) -0.002(3) 0.021(4) -0.012(3) C42 0.074(4) 0.021(3) 0.056(4) -0.001(3) 0.024(3) -0.008(3) C43 0.083(5) 0.041(4) 0.062(4) 0.005(3) 0.023(4) 0.001(4) C44 0.132(8) 0.077(6) 0.076(6) -0.012(5) -0.007(5) 0.002(6) O8 0.191(7) 0.098(4) 0.140(5) -0.049(4) -0.065(5) -0.019(4) C45 0.088(5) 0.026(3) 0.048(4) -0.001(3) 0.037(4) -0.003(3) C46 0.125(6) 0.038(3) 0.045(4) 0.003(3) 0.021(4) 0.008(4) C47 0.228(10) 0.054(4) 0.045(4) -0.009(4) 0.048(5) 0.016(6) C48 0.235(11) 0.047(4) 0.096(7) -0.019(5) 0.101(8) 0.011(6) C49 0.139(7) 0.057(4) 0.095(6) -0.015(4) 0.070(6) -0.001(4) C50 0.094(5) 0.034(3) 0.072(4) -0.017(3) 0.042(4) -0.007(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 O1 C23 1.320(6) . ? O2 C23 1.234(6) . ? O3 C24 1.250(6) . ? O4 C24 1.265(6) . ? O5 C43 1.266(7) . ? O6 C43 1.272(7) . ? O7 C44 1.303(8) . ? N1 C2 1.369(5) 6 ? N1 C2 1.369(5) . ? N2 C7 1.377(6) . ? N2 C4 1.378(5) . ? N3 C9 1.376(5) . ? N3 C9 1.376(5) 6 ? C1 C1 1.393(8) 6 ? C1 C2 1.438(7) . ? C1 C11 1.466(7) . ? C2 C3 1.406(6) . ? C3 C4 1.405(6) . ? C3 C17 1.474(6) . ? C4 C5 1.434(6) . ? C5 C6 1.364(7) . ? C5 C25 1.474(7) . ? C6 C7 1.422(6) . ? C6 C31 1.475(7) . ? C7 C8 1.402(6) . ? C8 C9 1.417(6) . ? C8 C37 1.484(6) . ? C9 C10 1.430(6) . ? C10 C10 1.348(8) 6 ? C10 C45 1.488(7) . ? C11 C16 1.356(7) . ? C11 C12 1.392(7) . ? C12 C13 1.426(8) . ? C13 C14 1.343(9) . ? C14 C15 1.382(9) . ? C15 C16 1.377(8) . ? C17 C22 1.386(6) . ? C17 C18 1.387(6) . ? C18 C19 1.405(6) . ? C19 C20 1.364(6) . ? C19 C24 1.489(7) . ? C20 C21 1.379(7) . ? C21 C22 1.416(7) . ? C21 C23 1.461(7) . ? C25 C26 1.374(7) . ? C25 C30 1.402(8) . ? C26 C27 1.364(7) . ? C27 C28 1.364(10) . ? C28 C29 1.364(10) . ? C29 C30 1.402(8) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C37 C38 1.377(7) . ? C37 C42 1.404(6) . ? C38 C39 1.386(7) . ? C39 C40 1.402(8) . ? C39 C44 1.463(10) . ? C40 C41 1.375(8) . ? C41 C42 1.389(7) . ? C41 C43 1.478(8) . ? C44 O8 1.218(8) . ? C45 C46 1.365(7) . ? C45 C50 1.399(7) . ? C46 C47 1.382(8) . ? C47 C48 1.404(11) . ? C48 C49 1.342(10) . ? C49 C50 1.397(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 C2 N1 C2 109.7(6) 6 . ? C7 N2 C4 110.2(4) . . ? C9 N3 C9 109.2(5) . 6 ? C1 C1 C2 107.1(2) 6 . ? C1 C1 C11 124.5(2) 6 . ? C2 C1 C11 127.9(4) . . ? N1 C2 C3 122.2(5) . . ? N1 C2 C1 108.0(4) . . ? C3 C2 C1 129.8(4) . . ? C4 C3 C2 123.2(4) . . ? C4 C3 C17 115.8(4) . . ? C2 C3 C17 120.9(4) . . ? N2 C4 C3 125.3(4) . . ? N2 C4 C5 106.2(4) . . ? C3 C4 C5 128.4(4) . . ? C6 C5 C4 108.4(4) . . ? C6 C5 C25 128.6(5) . . ? C4 C5 C25 121.5(5) . . ? C5 C6 C7 108.1(4) . . ? C5 C6 C31 127.4(4) . . ? C7 C6 C31 123.5(5) . . ? N2 C7 C8 123.2(4) . . ? N2 C7 C6 107.0(4) . . ? C8 C7 C6 129.8(5) . . ? C7 C8 C9 123.1(4) . . ? C7 C8 C37 117.6(4) . . ? C9 C8 C37 119.2(4) . . ? N3 C9 C8 121.9(4) . . ? N3 C9 C10 107.2(4) . . ? C8 C9 C10 130.8(4) . . ? C10 C10 C9 108.2(2) 6 . ? C10 C10 C45 126.5(2) 6 . ? C9 C10 C45 124.7(4) . . ? C16 C11 C12 119.7(5) . . ? C16 C11 C1 122.1(5) . . ? C12 C11 C1 118.1(5) . . ? C11 C12 C13 117.4(6) . . ? C14 C13 C12 121.1(6) . . ? C13 C14 C15 121.0(7) . . ? C16 C15 C14 118.0(6) . . ? C11 C16 C15 122.8(6) . . ? C22 C17 C18 118.7(4) . . ? C22 C17 C3 121.6(4) . . ? C18 C17 C3 119.6(4) . . ? C17 C18 C19 121.5(4) . . ? C20 C19 C18 119.0(4) . . ? C20 C19 C24 120.6(5) . . ? C18 C19 C24 120.3(5) . . ? C19 C20 C21 121.0(4) . . ? C20 C21 C22 119.9(4) . . ? C20 C21 C23 118.6(5) . . ? C22 C21 C23 121.3(5) . . ? C17 C22 C21 119.8(4) . . ? O2 C23 O1 121.8(5) . . ? O2 C23 C21 122.0(5) . . ? O1 C23 C21 116.2(5) . . ? O3 C24 O4 125.2(5) . . ? O3 C24 C19 119.0(5) . . ? O4 C24 C19 115.8(5) . . ? C26 C25 C30 117.5(5) . . ? C26 C25 C5 119.9(5) . . ? C30 C25 C5 122.5(5) . . ? C27 C26 C25 123.4(6) . . ? C26 C27 C28 118.8(6) . . ? C29 C28 C27 120.5(6) . . ? C28 C29 C30 120.8(6) . . ? C25 C30 C29 118.9(6) . . ? C32 C31 C36 120.0 . . ? C32 C31 C6 118.4(5) . . ? C36 C31 C6 121.6(5) . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C42 119.0(5) . . ? C38 C37 C8 122.0(4) . . ? C42 C37 C8 119.1(5) . . ? C37 C38 C39 122.2(5) . . ? C38 C39 C40 117.4(6) . . ? C38 C39 C44 121.9(6) . . ? C40 C39 C44 120.7(6) . . ? C41 C40 C39 121.9(5) . . ? C40 C41 C42 119.4(5) . . ? C40 C41 C43 120.4(5) . . ? C42 C41 C43 120.2(6) . . ? C41 C42 C37 120.0(5) . . ? O5 C43 O6 123.1(6) . . ? O5 C43 C41 117.3(6) . . ? O6 C43 C41 119.5(6) . . ? O8 C44 O7 121.4(8) . . ? O8 C44 C39 122.8(7) . . ? O7 C44 C39 115.8(7) . . ? C46 C45 C50 119.5(5) . . ? C46 C45 C10 122.3(6) . . ? C50 C45 C10 118.1(5) . . ? C45 C46 C47 122.1(7) . . ? C46 C47 C48 116.4(7) . . ? C49 C48 C47 123.6(7) . . ? C48 C49 C50 118.6(7) . . ? C49 C50 C45 119.7(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 C2 N1 C2 C3 -176.6(3) 6 . . . ? C2 N1 C2 C1 1.3(6) 6 . . . ? C1 C1 C2 N1 -0.8(4) 6 . . . ? C11 C1 C2 N1 171.2(4) . . . . ? C1 C1 C2 C3 176.9(4) 6 . . . ? C11 C1 C2 C3 -11.1(8) . . . . ? N1 C2 C3 C4 -20.3(7) . . . . ? C1 C2 C3 C4 162.3(4) . . . . ? N1 C2 C3 C17 158.5(4) . . . . ? C1 C2 C3 C17 -19.0(7) . . . . ? C7 N2 C4 C3 -173.1(4) . . . . ? C7 N2 C4 C5 4.1(5) . . . . ? C2 C3 C4 N2 -36.0(7) . . . . ? C17 C3 C4 N2 145.2(4) . . . . ? C2 C3 C4 C5 147.4(5) . . . . ? C17 C3 C4 C5 -31.4(7) . . . . ? N2 C4 C5 C6 -3.2(5) . . . . ? C3 C4 C5 C6 173.9(5) . . . . ? N2 C4 C5 C25 163.7(5) . . . . ? C3 C4 C5 C25 -19.1(8) . . . . ? C4 C5 C6 C7 1.2(6) . . . . ? C25 C5 C6 C7 -164.6(5) . . . . ? C4 C5 C6 C31 169.8(5) . . . . ? C25 C5 C6 C31 4.1(9) . . . . ? C4 N2 C7 C8 174.7(4) . . . . ? C4 N2 C7 C6 -3.4(5) . . . . ? C5 C6 C7 N2 1.3(6) . . . . ? C31 C6 C7 N2 -167.9(5) . . . . ? C5 C6 C7 C8 -176.6(5) . . . . ? C31 C6 C7 C8 14.2(8) . . . . ? N2 C7 C8 C9 32.3(7) . . . . ? C6 C7 C8 C9 -150.0(5) . . . . ? N2 C7 C8 C37 -150.9(4) . . . . ? C6 C7 C8 C37 26.7(8) . . . . ? C9 N3 C9 C8 175.2(3) 6 . . . ? C9 N3 C9 C10 -1.7(7) 6 . . . ? C7 C8 C9 N3 24.6(8) . . . . ? C37 C8 C9 N3 -152.1(5) . . . . ? C7 C8 C9 C10 -159.3(5) . . . . ? C37 C8 C9 C10 24.0(8) . . . . ? N3 C9 C10 C10 1.0(4) . . . 6 ? C8 C9 C10 C10 -175.4(5) . . . 6 ? N3 C9 C10 C45 -170.7(5) . . . . ? C8 C9 C10 C45 12.9(9) . . . . ? C1 C1 C11 C16 -72.3(5) 6 . . . ? C2 C1 C11 C16 117.1(5) . . . . ? C1 C1 C11 C12 103.8(4) 6 . . . ? C2 C1 C11 C12 -66.8(6) . . . . ? C16 C11 C12 C13 1.3(7) . . . . ? C1 C11 C12 C13 -175.0(5) . . . . ? C11 C12 C13 C14 -1.4(9) . . . . ? C12 C13 C14 C15 1.5(10) . . . . ? C13 C14 C15 C16 -1.3(10) . . . . ? C12 C11 C16 C15 -1.2(8) . . . . ? C1 C11 C16 C15 174.8(5) . . . . ? C14 C15 C16 C11 1.2(9) . . . . ? C4 C3 C17 C22 129.0(5) . . . . ? C2 C3 C17 C22 -49.8(7) . . . . ? C4 C3 C17 C18 -46.6(6) . . . . ? C2 C3 C17 C18 134.6(5) . . . . ? C22 C17 C18 C19 0.1(8) . . . . ? C3 C17 C18 C19 175.8(5) . . . . ? C17 C18 C19 C20 -0.7(8) . . . . ? C17 C18 C19 C24 -177.8(5) . . . . ? C18 C19 C20 C21 2.0(8) . . . . ? C24 C19 C20 C21 179.1(6) . . . . ? C19 C20 C21 C22 -2.6(9) . . . . ? C19 C20 C21 C23 -177.3(6) . . . . ? C18 C17 C22 C21 -0.7(7) . . . . ? C3 C17 C22 C21 -176.4(5) . . . . ? C20 C21 C22 C17 2.0(8) . . . . ? C23 C21 C22 C17 176.5(5) . . . . ? C20 C21 C23 O2 -4.2(10) . . . . ? C22 C21 C23 O2 -178.8(6) . . . . ? C20 C21 C23 O1 176.1(6) . . . . ? C22 C21 C23 O1 1.5(9) . . . . ? C20 C19 C24 O3 -179.1(6) . . . . ? C18 C19 C24 O3 -2.0(9) . . . . ? C20 C19 C24 O4 -0.9(9) . . . . ? C18 C19 C24 O4 176.1(5) . . . . ? C6 C5 C25 C26 107.0(7) . . . . ? C4 C5 C25 C26 -57.1(8) . . . . ? C6 C5 C25 C30 -72.4(9) . . . . ? C4 C5 C25 C30 123.5(6) . . . . ? C30 C25 C26 C27 0.5(9) . . . . ? C5 C25 C26 C27 -179.0(6) . . . . ? C25 C26 C27 C28 -1.3(11) . . . . ? C26 C27 C28 C29 1.6(12) . . . . ? C27 C28 C29 C30 -1.3(13) . . . . ? C26 C25 C30 C29 -0.1(10) . . . . ? C5 C25 C30 C29 179.4(6) . . . . ? C28 C29 C30 C25 0.5(12) . . . . ? C5 C6 C31 C32 -112.8(6) . . . . ? C7 C6 C31 C32 54.3(6) . . . . ? C5 C6 C31 C36 69.4(7) . . . . ? C7 C6 C31 C36 -123.5(5) . . . . ? C36 C31 C32 C33 0.0 . . . . ? C6 C31 C32 C33 -177.8(4) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? C6 C31 C36 C35 177.8(4) . . . . ? C7 C8 C37 C38 -133.0(5) . . . . ? C9 C8 C37 C38 43.9(7) . . . . ? C7 C8 C37 C42 47.0(6) . . . . ? C9 C8 C37 C42 -136.1(5) . . . . ? C42 C37 C38 C39 -3.9(8) . . . . ? C8 C37 C38 C39 176.2(5) . . . . ? C37 C38 C39 C40 3.0(9) . . . . ? C37 C38 C39 C44 -176.9(6) . . . . ? C38 C39 C40 C41 -0.7(9) . . . . ? C44 C39 C40 C41 179.2(6) . . . . ? C39 C40 C41 C42 -0.6(9) . . . . ? C39 C40 C41 C43 -178.7(5) . . . . ? C40 C41 C42 C37 -0.2(8) . . . . ? C43 C41 C42 C37 177.8(5) . . . . ? C38 C37 C42 C41 2.4(7) . . . . ? C8 C37 C42 C41 -177.6(4) . . . . ? C40 C41 C43 O5 -172.6(6) . . . . ? C42 C41 C43 O5 9.4(8) . . . . ? C40 C41 C43 O6 5.4(9) . . . . ? C42 C41 C43 O6 -172.6(5) . . . . ? C38 C39 C44 O8 175.6(8) . . . . ? C40 C39 C44 O8 -4.4(13) . . . . ? C38 C39 C44 O7 -1.3(11) . . . . ? C40 C39 C44 O7 178.8(7) . . . . ? C10 C10 C45 C46 68.6(6) 6 . . . ? C9 C10 C45 C46 -121.2(6) . . . . ? C10 C10 C45 C50 -108.9(4) 6 . . . ? C9 C10 C45 C50 61.3(7) . . . . ? C50 C45 C46 C47 0.8(8) . . . . ? C10 C45 C46 C47 -176.6(5) . . . . ? C45 C46 C47 C48 0.4(10) . . . . ? C46 C47 C48 C49 -2.0(11) . . . . ? C47 C48 C49 C50 2.4(11) . . . . ? C48 C49 C50 C45 -1.1(9) . . . . ? C46 C45 C50 C49 -0.5(8) . . . . ? C10 C45 C50 C49 177.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 20.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.648 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.054 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 -0.002 -0.081 -0.001 6312 1698 ' ' 2 0.208 0.000 0.356 14 5 ' ' 3 0.791 0.000 0.644 14 4 ' ' 4 0.291 0.500 0.644 14 4 ' ' 5 0.708 0.500 0.356 14 5 ' ' _platon_squeeze_details 'Four EtOH and 2.5 cyclohexane molecules per asymmetric unit were deleted with the squeeze program'