# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'V. Ramamurthy' _publ_contact_author_address ; Department of Chemistry University of Miami Miami Florida 33124 UNITED STATES OF AMERICA ; _publ_contact_author_email MURTHY1@MIAMI.EDU _publ_section_title ; Template directed photodimerization of trans 1,2-bis(n-pyridyl)ethylenes and stilbazoles in water ; loop_ _publ_author_name 'V. Ramamurthy' 'Raja Kaliappan' 'Joel Mague' 'Arunkumar Natarajan' 'Mahesh Pattabiraman' #VR164RE.CIF data_vr164 _database_code_depnum_ccdc_archive 'CCDC 276220' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H99 Cl4 N36 O29.50' _chemical_formula_weight 2082.87 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 12.938(2) _cell_length_b 14.613(2) _cell_length_c 25.703(4) _cell_angle_alpha 88.608(2) _cell_angle_beta 89.882(2) _cell_angle_gamma 76.149(2) _cell_volume 4717(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8711 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 24.66 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2174 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9498 _exptl_absorpt_correction_T_max 0.9879 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32956 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.83 _reflns_number_total 16070 _reflns_number_gt 8785 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _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. H atoms were placed in calculated positions and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached atom. A considerable amount of electron density attibutable to partially disordered water of solvation was seen in the channels between the host molecules. Some of this could be modeled by oxygen atoms at full occupancy and some at 0.5 occupancy. The remainder was removed with the SQUEEZE option of PLATON (Spek, 2005). The hydrogen atoms associated with the solvent waters could not be located and so are omitted from the final refinement and structure factor calculations. They are, however, included in the reported chemical formula and derived values (e.g. formula weight, F_000, etc). ; _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^)+(0.2000P)^2^] 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 16070 _refine_ls_number_parameters 1266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1932 _refine_ls_R_factor_gt 0.1289 _refine_ls_wR_factor_ref 0.3856 _refine_ls_wR_factor_gt 0.3559 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.015 _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 0.68924(16) 0.85590(18) 0.15629(8) 0.0398(6) Uani 1 1 d . . . Cl2 Cl 0.1946(2) 0.8503(3) 0.34868(10) 0.0787(11) Uani 1 1 d . . . Cl3 Cl 0.6745(2) 0.4440(3) 0.27847(12) 0.0732(9) Uani 1 1 d . . . Cl4 Cl 0.0606(3) 0.5143(3) 0.39398(15) 0.0985(12) Uani 1 1 d . . . O1 O 0.5500(4) -0.3158(4) 0.3604(2) 0.0357(14) Uani 1 1 d . . . O2 O 0.4978(4) -0.1067(4) 0.2731(2) 0.0358(14) Uani 1 1 d . . . O3 O 0.3310(4) 0.1349(4) 0.2979(2) 0.0376(14) Uani 1 1 d . . . O4 O 0.1678(5) 0.2521(4) 0.4140(2) 0.0383(14) Uani 1 1 d . . . O5 O 0.5395(5) 0.3886(4) 0.4986(2) 0.0419(15) Uani 1 1 d . . . O6 O 0.6986(5) 0.2497(4) 0.4003(2) 0.0381(14) Uani 1 1 d . . . O7 O 0.8839(4) -0.0124(4) 0.3754(2) 0.0329(13) Uani 1 1 d . . . O8 O 0.9373(4) -0.2086(4) 0.4453(2) 0.0356(14) Uani 1 1 d . . . O9 O 0.0618(4) -0.3205(4) 0.1534(2) 0.0366(14) Uani 1 1 d . . . O10 O -0.0015(4) -0.1038(4) 0.2298(2) 0.0335(14) Uani 1 1 d . . . O11 O -0.1743(4) 0.1383(4) 0.1924(2) 0.0386(15) Uani 1 1 d . . . O12 O -0.3496(5) 0.2603(5) 0.0752(2) 0.0480(17) Uani 1 1 d . . . O13 O 0.0235(5) 0.3942(4) -0.0206(3) 0.0450(16) Uani 1 1 d . . . O14 O 0.1915(5) 0.2532(5) 0.0849(2) 0.0431(16) Uani 1 1 d . . . O15 O 0.3816(4) -0.0063(4) 0.1228(2) 0.0331(14) Uani 1 1 d . . . O16 O 0.4398(4) -0.2045(4) 0.0620(2) 0.0355(14) Uani 1 1 d . . . N1 N 0.7007(5) -0.3766(5) 0.4102(3) 0.0301(16) Uani 1 1 d . . . N2 N 0.7172(5) -0.3000(5) 0.3364(3) 0.0349(17) Uani 1 1 d . . . N3 N 0.6793(5) -0.1534(5) 0.2860(3) 0.0299(16) Uani 1 1 d . . . N4 N 0.6087(5) -0.0042(5) 0.2646(3) 0.0302(16) Uani 1 1 d . . . N5 N 0.5004(5) 0.1522(5) 0.2784(3) 0.0294(16) Uani 1 1 d . . . N6 N 0.3917(5) 0.2647(5) 0.3213(3) 0.0302(16) Uani 1 1 d . . . N7 N 0.2874(5) 0.3398(5) 0.3928(3) 0.0313(16) Uani 1 1 d . . . N8 N 0.2082(5) 0.3593(5) 0.4699(3) 0.0338(17) Uani 1 1 d . . . N9 N 0.3578(5) 0.4108(5) 0.5036(3) 0.0337(17) Uani 1 1 d . . . N10 N 0.4332(5) 0.4041(5) 0.4257(3) 0.0328(16) Uani 1 1 d . . . N11 N 0.5386(5) 0.3157(5) 0.3589(3) 0.0299(16) Uani 1 1 d . . . N12 N 0.6465(5) 0.1890(5) 0.3255(2) 0.0277(15) Uani 1 1 d . . . N13 N 0.7557(5) 0.0327(5) 0.3104(3) 0.0305(16) Uani 1 1 d . . . N14 N 0.8413(5) -0.1171(5) 0.3188(2) 0.0266(15) Uani 1 1 d . . . N15 N 0.8790(5) -0.2607(5) 0.3704(2) 0.0264(15) Uani 1 1 d . . . N16 N 0.8541(5) -0.3312(5) 0.4445(3) 0.0336(17) Uani 1 1 d . . . N17 N 0.3047(6) -0.3639(5) -0.0154(3) 0.0348(17) Uani 1 1 d . . . N18 N 0.3636(5) -0.3317(5) 0.0696(3) 0.0338(17) Uani 1 1 d . . . N19 N 0.3858(5) -0.2559(5) 0.1404(2) 0.0263(15) Uani 1 1 d . . . N20 N 0.3395(5) -0.1088(5) 0.1842(2) 0.0267(15) Uani 1 1 d . . . N21 N 0.2497(5) 0.0413(5) 0.1845(3) 0.0309(16) Uani 1 1 d . . . N22 N 0.1397(5) 0.1942(5) 0.1625(3) 0.0281(15) Uani 1 1 d . . . N23 N 0.0317(5) 0.3188(5) 0.1239(3) 0.0376(18) Uani 1 1 d . . . N24 N -0.0763(5) 0.3997(5) 0.0531(3) 0.0334(17) Uani 1 1 d . . . N25 N -0.1594(5) 0.4203(5) -0.0228(3) 0.0349(17) Uani 1 1 d . . . N26 N -0.2237(5) 0.3443(5) 0.0912(3) 0.0355(17) Uani 1 1 d . . . N27 N -0.1154(5) 0.2680(5) 0.1635(3) 0.0301(16) Uani 1 1 d . . . N28 N -0.0067(5) 0.1553(5) 0.2099(3) 0.0343(17) Uani 1 1 d . . . N29 N 0.1047(5) 0.0026(5) 0.2324(3) 0.0288(16) Uani 1 1 d . . . N30 N 0.1800(5) -0.1467(5) 0.2187(2) 0.0271(15) Uani 1 1 d . . . N31 N 0.2236(5) -0.2942(5) 0.1753(3) 0.0299(16) Uani 1 1 d . . . N32 N 0.2138(5) -0.3813(5) 0.1072(3) 0.0348(17) Uani 1 1 d . . . N33 N 0.4503(5) 1.0551(5) -0.0557(3) 0.0343(18) Uani 1 1 d . . . H33N H 0.5025 1.0699 -0.0734 0.041 Uiso 1 1 calc R . . N34 N -0.1102(5) 0.8756(5) 0.1064(3) 0.0315(16) Uani 1 1 d . . . H34N H -0.1683 0.8661 0.1211 0.038 Uiso 1 1 calc R . . N35 N 0.6068(5) 0.1201(6) 0.6018(3) 0.0380(18) Uani 1 1 d . . . H35N H 0.6637 0.1313 0.6166 0.046 Uiso 1 1 calc R . . N36 N 0.0500(5) -0.0626(5) 0.4459(3) 0.0322(16) Uani 1 1 d . . . H36N H -0.0015 -0.0787 0.4287 0.039 Uiso 1 1 calc R . . C1 C 0.6550(7) -0.4381(6) 0.4440(3) 0.034(2) Uani 1 1 d . . . H1A H 0.5846 -0.4404 0.4299 0.041 Uiso 1 1 calc R . . H1B H 0.7012 -0.5027 0.4431 0.041 Uiso 1 1 calc R . . C2 C 0.6467(7) -0.3288(6) 0.3679(3) 0.036(2) Uani 1 1 d . . . C3 C 0.6870(6) -0.2535(6) 0.2866(3) 0.0304(19) Uani 1 1 d . . . H3A H 0.7399 -0.2828 0.2603 0.036 Uiso 1 1 calc R . . H3B H 0.6173 -0.2643 0.2762 0.036 Uiso 1 1 calc R . . C4 C 0.5863(6) -0.0896(7) 0.2741(3) 0.035(2) Uani 1 1 d . . . C5 C 0.5299(6) 0.0745(6) 0.2438(3) 0.035(2) Uani 1 1 d . . . H5A H 0.4654 0.0528 0.2350 0.042 Uiso 1 1 calc R . . H5B H 0.5573 0.0970 0.2112 0.042 Uiso 1 1 calc R . . C6 C 0.4014(6) 0.1794(6) 0.2986(3) 0.0316(19) Uani 1 1 d . . . C7 C 0.2914(6) 0.3215(6) 0.3383(3) 0.0314(19) Uani 1 1 d . . . H7A H 0.2763 0.3824 0.3187 0.038 Uiso 1 1 calc R . . H7B H 0.2346 0.2892 0.3298 0.038 Uiso 1 1 calc R . . C8 C 0.2159(6) 0.3127(6) 0.4243(3) 0.0311(19) Uani 1 1 d . . . C9 C 0.2677(6) 0.4320(6) 0.4681(3) 0.0313(19) Uani 1 1 d . . . H9 H 0.2211 0.4964 0.4732 0.038 Uiso 1 1 calc R . . C10 C 0.3195(6) 0.4220(6) 0.4136(3) 0.0312(19) Uani 1 1 d . . . H10 H 0.2943 0.4800 0.3912 0.037 Uiso 1 1 calc R . . C11 C 0.4867(6) 0.3008(6) 0.3122(3) 0.0312(19) Uani 1 1 d . . . H11 H 0.4711 0.3582 0.2889 0.037 Uiso 1 1 calc R . . C12 C 0.5623(6) 0.2184(6) 0.2869(3) 0.0310(19) Uani 1 1 d . . . H12 H 0.5908 0.2385 0.2534 0.037 Uiso 1 1 calc R . . C13 C 0.7202(6) -0.0099(6) 0.2652(3) 0.0277(18) Uani 1 1 d . . . H13 H 0.7449 0.0144 0.2318 0.033 Uiso 1 1 calc R . . C14 C 0.7708(6) -0.1140(6) 0.2747(3) 0.0291(19) Uani 1 1 d . . . H14 H 0.8105 -0.1431 0.2434 0.035 Uiso 1 1 calc R . . C15 C 0.8256(6) -0.3336(6) 0.3543(3) 0.0325(19) Uani 1 1 d . . . H15 H 0.8695 -0.3770 0.3288 0.039 Uiso 1 1 calc R . . C16 C 0.8129(7) -0.3865(6) 0.4069(3) 0.035(2) Uani 1 1 d . . . H16 H 0.8534 -0.4540 0.4072 0.042 Uiso 1 1 calc R . . C17 C 0.8830(6) -0.3665(7) 0.4961(3) 0.036(2) Uani 1 1 d . . . H17A H 0.9314 -0.3308 0.5111 0.043 Uiso 1 1 calc R . . H17B H 0.9222 -0.4334 0.4946 0.043 Uiso 1 1 calc R . . C18 C 0.8938(6) -0.2616(6) 0.4216(3) 0.033(2) Uani 1 1 d . . . C19 C 0.9187(6) -0.1992(6) 0.3344(3) 0.034(2) Uani 1 1 d . . . H19A H 0.9790 -0.1801 0.3510 0.040 Uiso 1 1 calc R . . H19B H 0.9462 -0.2350 0.3031 0.040 Uiso 1 1 calc R . . C20 C 0.8326(6) -0.0312(6) 0.3394(3) 0.032(2) Uani 1 1 d . . . C21 C 0.7496(6) 0.1333(6) 0.3119(3) 0.0319(19) Uani 1 1 d . . . H21A H 0.8023 0.1440 0.3375 0.038 Uiso 1 1 calc R . . H21B H 0.7694 0.1550 0.2774 0.038 Uiso 1 1 calc R . . C22 C 0.6331(6) 0.2515(6) 0.3644(3) 0.032(2) Uani 1 1 d . . . C23 C 0.5121(6) 0.4009(6) 0.3871(3) 0.035(2) Uani 1 1 d . . . H23A H 0.5774 0.4101 0.4039 0.041 Uiso 1 1 calc R . . H23B H 0.4870 0.4542 0.3620 0.041 Uiso 1 1 calc R . . C24 C 0.4528(7) 0.4007(6) 0.4776(4) 0.033(2) Uani 1 1 d . . . C25 C 0.1564(7) -0.3319(6) 0.1455(3) 0.0320(19) Uani 1 1 d . . . C26 C 0.1923(6) -0.2483(5) 0.2225(3) 0.0278(18) Uani 1 1 d . . . H26A H 0.2462 -0.2748 0.2496 0.033 Uiso 1 1 calc R . . H26B H 0.1239 -0.2613 0.2337 0.033 Uiso 1 1 calc R . . C27 C 0.0837(6) -0.0860(6) 0.2274(3) 0.0284(19) Uani 1 1 d . . . C28 C 0.0230(6) 0.0825(6) 0.2486(3) 0.035(2) Uani 1 1 d . . . H28A H -0.0409 0.0603 0.2587 0.041 Uiso 1 1 calc R . . H28B H 0.0484 0.1091 0.2798 0.041 Uiso 1 1 calc R . . C29 C -0.1056(6) 0.1830(6) 0.1886(3) 0.033(2) Uani 1 1 d . . . C30 C -0.2176(6) 0.3240(6) 0.1473(3) 0.037(2) Uani 1 1 d . . . H30A H -0.2329 0.3842 0.1659 0.044 Uiso 1 1 calc R . . H30B H -0.2728 0.2902 0.1570 0.044 Uiso 1 1 calc R . . C31 C -0.2975(7) 0.3184(7) 0.0613(3) 0.039(2) Uani 1 1 d . . . C32 C -0.2463(6) 0.4357(6) 0.0145(3) 0.033(2) Uani 1 1 d . . . H32 H -0.2942 0.5002 0.0104 0.040 Uiso 1 1 calc R . . C33 C -0.1898(6) 0.4215(6) 0.0670(4) 0.034(2) Uani 1 1 d . . . H33 H -0.2100 0.4795 0.0882 0.041 Uiso 1 1 calc R . . C34 C -0.0239(6) 0.3050(6) 0.1710(3) 0.0297(19) Uani 1 1 d . . . H34 H -0.0417 0.3637 0.1917 0.036 Uiso 1 1 calc R . . C35 C 0.0554(6) 0.2245(6) 0.2008(3) 0.035(2) Uani 1 1 d . . . H35 H 0.0821 0.2459 0.2337 0.043 Uiso 1 1 calc R . . C36 C 0.2166(6) 0.0007(6) 0.2318(3) 0.0291(19) Uani 1 1 d . . . H36 H 0.2398 0.0279 0.2638 0.035 Uiso 1 1 calc R . . C37 C 0.2688(6) -0.1056(6) 0.2273(3) 0.0275(18) Uani 1 1 d . . . H37 H 0.3083 -0.1318 0.2599 0.033 Uiso 1 1 calc R . . C38 C 0.3346(6) -0.3285(6) 0.1598(3) 0.0270(18) Uani 1 1 d . . . H38 H 0.3779 -0.3688 0.1878 0.032 Uiso 1 1 calc R . . C39 C 0.3264(7) -0.3846(6) 0.1115(3) 0.034(2) Uani 1 1 d . . . H39 H 0.3705 -0.4507 0.1148 0.041 Uiso 1 1 calc R . . C40 C 0.3940(6) -0.3694(7) 0.0193(3) 0.038(2) Uani 1 1 d . . . H40A H 0.4330 -0.4363 0.0237 0.046 Uiso 1 1 calc R . . H40B H 0.4432 -0.3347 0.0031 0.046 Uiso 1 1 calc R . . C41 C 0.3987(6) -0.2574(6) 0.0886(3) 0.0297(19) Uani 1 1 d . . . C42 C 0.4215(6) -0.1921(6) 0.1725(3) 0.0291(19) Uani 1 1 d . . . H42A H 0.4812 -0.1725 0.1550 0.035 Uiso 1 1 calc R . . H42B H 0.4490 -0.2251 0.2055 0.035 Uiso 1 1 calc R . . C43 C 0.3299(6) -0.0239(6) 0.1605(3) 0.0278(18) Uani 1 1 d . . . C44 C 0.2443(6) 0.1406(6) 0.1788(3) 0.0313(19) Uani 1 1 d . . . H44A H 0.2974 0.1503 0.1527 0.038 Uiso 1 1 calc R . . H44B H 0.2628 0.1645 0.2124 0.038 Uiso 1 1 calc R . . C45 C 0.1290(7) 0.2551(6) 0.1207(4) 0.036(2) Uani 1 1 d . . . C46 C 0.0047(7) 0.4008(6) 0.0910(4) 0.037(2) Uani 1 1 d . . . H46A H 0.0696 0.4081 0.0725 0.044 Uiso 1 1 calc R . . H46B H -0.0197 0.4566 0.1129 0.044 Uiso 1 1 calc R . . C47 C -0.0632(7) 0.4050(6) 0.0012(4) 0.038(2) Uani 1 1 d . . . C49 C 0.4290(6) 0.9729(7) -0.0639(3) 0.036(2) Uani 1 1 d . . . H49 H 0.4702 0.9304 -0.0876 0.043 Uiso 1 1 calc R . . C50 C 0.3437(7) 0.9492(7) -0.0367(4) 0.045(2) Uani 1 1 d . . . H50 H 0.3253 0.8912 -0.0429 0.054 Uiso 1 1 calc R . . C51 C 0.2875(6) 1.0107(7) -0.0013(3) 0.037(2) Uani 1 1 d . . . C52 C 0.3135(6) 1.0959(7) 0.0054(3) 0.040(2) Uani 1 1 d . . . H52 H 0.2739 1.1400 0.0289 0.048 Uiso 1 1 calc R . . C53 C 0.3972(6) 1.1173(7) -0.0220(3) 0.037(2) Uani 1 1 d . . . H53 H 0.4166 1.1752 -0.0169 0.044 Uiso 1 1 calc R . . C54 C 0.1991(7) 0.9944(8) 0.0305(4) 0.046(2) Uani 1 1 d . . . H54 H 0.1666 1.0420 0.0539 0.056 Uiso 1 1 calc R . . C55 C 0.1623(8) 0.9194(8) 0.0287(4) 0.050(3) Uani 1 1 d . . . H55 H 0.1972 0.8699 0.0069 0.060 Uiso 1 1 calc R . . C56 C 0.0673(7) 0.9064(7) 0.0592(4) 0.042(2) Uani 1 1 d . . . C57 C 0.0163(7) 0.9666(8) 0.0953(4) 0.047(3) Uani 1 1 d . . . H57 H 0.0429 1.0190 0.1048 0.056 Uiso 1 1 calc R . . C58 C -0.0771(7) 0.9507(7) 0.1187(3) 0.041(2) Uani 1 1 d . . . H58 H -0.1154 0.9938 0.1431 0.049 Uiso 1 1 calc R . . C60 C -0.0591(7) 0.8132(7) 0.0725(4) 0.043(2) Uani 1 1 d . . . H60 H -0.0849 0.7592 0.0652 0.051 Uiso 1 1 calc R . . C61 C 0.0305(7) 0.8268(7) 0.0480(4) 0.047(2) Uani 1 1 d . . . H61 H 0.0670 0.7826 0.0237 0.056 Uiso 1 1 calc R . . C63 C 0.5616(8) 0.1763(8) 0.5652(4) 0.050(3) Uani 1 1 d . . . H63 H 0.5911 0.2276 0.5552 0.061 Uiso 1 1 calc R . . C64 C 0.4712(8) 0.1654(8) 0.5395(5) 0.057(3) Uani 1 1 d . . . H64 H 0.4392 0.2073 0.5121 0.068 Uiso 1 1 calc R . . C65 C 0.4315(7) 0.0932(10) 0.5551(4) 0.057(3) Uani 1 1 d . . . C66 C 0.4820(9) 0.0298(9) 0.5958(5) 0.066(3) Uani 1 1 d . . . H66 H 0.4547 -0.0221 0.6070 0.079 Uiso 1 1 calc R . . C67 C 0.5735(7) 0.0474(7) 0.6184(4) 0.046(2) Uani 1 1 d . . . H67 H 0.6105 0.0072 0.6454 0.055 Uiso 1 1 calc R . . C68 C 0.3342(9) 0.0756(9) 0.5259(5) 0.061(3) Uani 1 1 d . . . H68 H 0.2986 0.1245 0.5026 0.073 Uiso 1 1 calc R . . C69 C 0.2980(7) 0.0058(8) 0.5293(4) 0.052(3) Uani 1 1 d . . . H69 H 0.3297 -0.0410 0.5545 0.062 Uiso 1 1 calc R . . C70 C 0.2102(6) -0.0129(7) 0.4984(4) 0.039(2) Uani 1 1 d . . . C71 C 0.1845(6) -0.0985(7) 0.5086(3) 0.037(2) Uani 1 1 d . . . H71 H 0.2231 -0.1409 0.5343 0.044 Uiso 1 1 calc R . . C72 C 0.1038(6) -0.1218(6) 0.4818(3) 0.034(2) Uani 1 1 d . . . H72 H 0.0862 -0.1804 0.4889 0.041 Uiso 1 1 calc R . . C74 C 0.0715(7) 0.0209(7) 0.4349(3) 0.039(2) Uani 1 1 d . . . H74 H 0.0303 0.0628 0.4097 0.047 Uiso 1 1 calc R . . C75 C 0.1545(7) 0.0458(7) 0.4606(4) 0.043(2) Uani 1 1 d . . . H75 H 0.1726 0.1036 0.4520 0.052 Uiso 1 1 calc R . . C76 C -0.1724(7) 0.4481(7) -0.0778(3) 0.043(2) Uani 1 1 d . . . H76A H -0.2217 0.5112 -0.0813 0.052 Uiso 1 1 calc R . . H76B H -0.1027 0.4524 -0.0923 0.052 Uiso 1 1 calc R . . O17 O 0.4026(4) 0.2956(4) 0.18591(18) 0.0257(12) Uani 1 1 d . . . O18 O 0.3067(7) 0.5365(6) 0.2852(3) 0.079(2) Uani 1 1 d . . . O19 O 0.5175(7) 0.4462(6) 0.1858(3) 0.078(2) Uani 1 1 d . . . O20 O 0.5756(5) 0.5211(6) 0.0967(3) 0.066(2) Uani 1 1 d . . . O21 O 0.6923(8) 0.6634(6) 0.1086(4) 0.096(3) Uani 1 1 d . . . O22 O 0.4690(7) 0.6205(6) 0.2743(3) 0.069(2) Uani 1 1 d . . . O34 O 0.7974(7) 0.5452(6) 0.1919(4) 0.078(2) Uani 1 1 d . . . O23 O 0.9436(7) 0.6314(6) 0.2317(3) 0.081(3) Uani 1 1 d . . . O24 O 0.8964(7) 0.3053(7) 0.2965(4) 0.091(3) Uani 1 1 d . . . O25 O 0.9649(8) 0.2353(7) 0.3911(4) 0.029(2) Uiso 0.50 1 d P . . O26 O 0.8213(10) 0.3398(9) 0.4575(5) 0.046(3) Uiso 0.50 1 d P . . O27 O 0.7383(14) 0.3437(12) 0.5471(7) 0.078(5) Uiso 0.50 1 d P . . O28 O 0.8157(13) 0.3457(11) 0.6405(6) 0.071(4) Uiso 0.50 1 d P . . O29 O 0.5595(10) 0.7535(9) 0.9187(5) 0.047(3) Uiso 0.50 1 d P . . O30 O 0.2806(9) 0.3406(8) 1.0002(4) 0.033(3) Uiso 0.50 1 d P . . O31 O 0.1870(4) 0.4247(3) 0.20316(18) 0.0201(11) Uiso 1 1 d . . . O33 O 0.0366(12) 0.4215(10) 0.2968(6) 0.059(4) Uiso 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 Cl1 0.0241(10) 0.0765(17) 0.0260(11) 0.0036(10) 0.0004(8) -0.0267(11) Cl2 0.0431(15) 0.175(3) 0.0411(14) -0.0421(17) 0.0193(11) -0.0680(19) Cl3 0.0377(15) 0.117(3) 0.0675(19) 0.0064(17) 0.0051(13) -0.0236(16) Cl4 0.072(2) 0.130(3) 0.083(2) -0.003(2) -0.0005(18) -0.001(2) O1 0.022(3) 0.056(4) 0.037(3) -0.005(3) -0.002(2) -0.022(3) O2 0.023(3) 0.056(4) 0.033(3) -0.013(3) 0.002(2) -0.017(3) O3 0.028(3) 0.047(4) 0.044(4) -0.010(3) 0.000(3) -0.021(3) O4 0.034(3) 0.051(4) 0.038(3) -0.003(3) -0.003(3) -0.024(3) O5 0.034(4) 0.055(4) 0.044(4) 0.003(3) -0.007(3) -0.024(3) O6 0.035(3) 0.051(4) 0.029(3) -0.004(3) -0.009(3) -0.011(3) O7 0.024(3) 0.049(4) 0.029(3) -0.004(3) -0.005(2) -0.015(3) O8 0.031(3) 0.052(4) 0.031(3) -0.006(3) -0.001(2) -0.024(3) O9 0.026(3) 0.055(4) 0.039(3) -0.007(3) 0.007(3) -0.030(3) O10 0.019(3) 0.050(4) 0.037(3) -0.002(3) 0.003(2) -0.018(3) O11 0.030(3) 0.048(4) 0.046(4) -0.002(3) 0.007(3) -0.024(3) O12 0.050(4) 0.069(5) 0.039(4) -0.012(3) 0.009(3) -0.040(4) O13 0.029(3) 0.048(4) 0.066(4) -0.013(3) 0.016(3) -0.025(3) O14 0.026(3) 0.061(4) 0.043(4) 0.011(3) 0.003(3) -0.014(3) O15 0.020(3) 0.052(4) 0.031(3) 0.010(3) 0.002(2) -0.017(3) O16 0.022(3) 0.054(4) 0.036(3) 0.001(3) 0.003(2) -0.022(3) N1 0.023(4) 0.042(4) 0.031(4) 0.000(3) -0.005(3) -0.020(3) N2 0.031(4) 0.045(4) 0.035(4) -0.005(3) 0.006(3) -0.021(3) N3 0.015(3) 0.046(4) 0.032(4) -0.007(3) 0.002(3) -0.012(3) N4 0.026(4) 0.036(4) 0.034(4) -0.009(3) 0.003(3) -0.015(3) N5 0.018(3) 0.038(4) 0.035(4) -0.010(3) -0.002(3) -0.012(3) N6 0.011(3) 0.041(4) 0.043(4) -0.005(3) -0.001(3) -0.013(3) N7 0.026(4) 0.030(4) 0.041(4) -0.003(3) 0.004(3) -0.012(3) N8 0.024(4) 0.051(5) 0.032(4) -0.001(3) 0.001(3) -0.021(3) N9 0.031(4) 0.046(4) 0.031(4) -0.003(3) -0.008(3) -0.023(3) N10 0.019(3) 0.045(4) 0.038(4) -0.005(3) -0.002(3) -0.014(3) N11 0.026(4) 0.034(4) 0.034(4) -0.005(3) 0.001(3) -0.016(3) N12 0.015(3) 0.044(4) 0.028(4) -0.008(3) -0.001(3) -0.013(3) N13 0.027(4) 0.037(4) 0.031(4) -0.006(3) 0.005(3) -0.014(3) N14 0.019(3) 0.035(4) 0.028(4) -0.009(3) 0.005(3) -0.012(3) N15 0.018(3) 0.039(4) 0.029(4) -0.003(3) 0.004(3) -0.020(3) N16 0.027(4) 0.045(4) 0.037(4) -0.005(3) -0.001(3) -0.025(3) N17 0.040(4) 0.050(5) 0.022(4) -0.004(3) 0.004(3) -0.024(4) N18 0.029(4) 0.050(5) 0.030(4) -0.010(3) 0.011(3) -0.023(3) N19 0.024(3) 0.034(4) 0.022(3) -0.003(3) 0.004(3) -0.009(3) N20 0.016(3) 0.037(4) 0.031(4) 0.002(3) 0.002(3) -0.013(3) N21 0.015(3) 0.045(4) 0.035(4) 0.000(3) 0.003(3) -0.011(3) N22 0.016(3) 0.039(4) 0.033(4) 0.004(3) -0.002(3) -0.013(3) N23 0.015(3) 0.039(4) 0.061(5) 0.007(4) -0.001(3) -0.013(3) N24 0.025(4) 0.037(4) 0.043(4) 0.001(3) 0.007(3) -0.015(3) N25 0.020(4) 0.052(5) 0.036(4) -0.010(3) 0.007(3) -0.013(3) N26 0.031(4) 0.045(5) 0.033(4) -0.006(3) 0.001(3) -0.014(3) N27 0.025(4) 0.037(4) 0.033(4) 0.004(3) -0.001(3) -0.018(3) N28 0.031(4) 0.033(4) 0.042(4) -0.001(3) 0.010(3) -0.013(3) N29 0.019(3) 0.033(4) 0.039(4) -0.005(3) 0.006(3) -0.014(3) N30 0.014(3) 0.045(4) 0.026(4) -0.005(3) 0.003(3) -0.013(3) N31 0.022(3) 0.044(4) 0.029(4) -0.007(3) 0.002(3) -0.017(3) N32 0.028(4) 0.051(5) 0.033(4) -0.020(3) 0.010(3) -0.023(3) N33 0.015(3) 0.061(5) 0.030(4) 0.011(4) -0.001(3) -0.017(3) N34 0.017(3) 0.049(5) 0.032(4) 0.002(3) 0.001(3) -0.014(3) N35 0.024(4) 0.058(5) 0.036(4) -0.019(4) 0.002(3) -0.017(4) N36 0.025(4) 0.045(5) 0.033(4) -0.002(3) 0.002(3) -0.021(3) C1 0.031(5) 0.042(5) 0.037(5) -0.005(4) 0.002(4) -0.022(4) C2 0.049(6) 0.038(5) 0.028(5) -0.011(4) 0.005(4) -0.026(4) C3 0.028(4) 0.046(5) 0.023(4) -0.007(4) -0.004(3) -0.020(4) C4 0.023(5) 0.056(6) 0.027(4) -0.011(4) 0.000(3) -0.013(4) C5 0.027(4) 0.048(6) 0.036(5) 0.001(4) -0.003(4) -0.021(4) C6 0.026(4) 0.041(5) 0.031(5) 0.001(4) -0.007(3) -0.014(4) C7 0.028(4) 0.038(5) 0.030(5) -0.006(4) -0.003(3) -0.010(4) C8 0.026(4) 0.035(5) 0.035(5) 0.002(4) -0.006(4) -0.014(4) C9 0.029(4) 0.037(5) 0.034(5) -0.007(4) 0.000(4) -0.018(4) C10 0.031(5) 0.038(5) 0.031(5) -0.003(4) 0.004(4) -0.020(4) C11 0.023(4) 0.045(5) 0.028(4) 0.006(4) 0.000(3) -0.015(4) C12 0.033(5) 0.035(5) 0.029(4) 0.000(4) 0.001(4) -0.017(4) C13 0.022(4) 0.042(5) 0.024(4) -0.004(4) 0.003(3) -0.017(4) C14 0.017(4) 0.052(6) 0.027(4) -0.008(4) 0.003(3) -0.024(4) C15 0.024(4) 0.039(5) 0.036(5) -0.013(4) 0.004(4) -0.010(4) C16 0.034(5) 0.040(5) 0.036(5) -0.009(4) 0.003(4) -0.015(4) C17 0.021(4) 0.055(6) 0.033(5) 0.004(4) -0.002(3) -0.015(4) C18 0.018(4) 0.037(5) 0.046(6) -0.006(4) 0.001(4) -0.009(4) C19 0.017(4) 0.057(6) 0.027(4) -0.012(4) 0.002(3) -0.007(4) C20 0.018(4) 0.050(6) 0.029(5) 0.002(4) 0.001(3) -0.010(4) C21 0.022(4) 0.044(5) 0.033(5) -0.005(4) 0.003(3) -0.014(4) C22 0.016(4) 0.054(6) 0.029(5) 0.001(4) 0.005(3) -0.015(4) C23 0.026(4) 0.046(5) 0.038(5) -0.004(4) -0.005(4) -0.019(4) C24 0.029(5) 0.023(5) 0.051(6) -0.002(4) 0.000(4) -0.014(4) C25 0.029(5) 0.042(5) 0.031(5) 0.000(4) -0.001(4) -0.019(4) C26 0.019(4) 0.034(5) 0.037(5) -0.006(4) 0.006(3) -0.018(4) C27 0.024(4) 0.046(5) 0.017(4) 0.000(3) 0.001(3) -0.012(4) C28 0.026(4) 0.053(6) 0.026(4) -0.007(4) 0.007(3) -0.010(4) C29 0.019(4) 0.050(6) 0.030(5) -0.012(4) 0.010(3) -0.010(4) C30 0.027(5) 0.048(6) 0.036(5) -0.007(4) 0.012(4) -0.012(4) C31 0.028(5) 0.057(6) 0.038(5) -0.019(5) 0.013(4) -0.022(4) C32 0.025(4) 0.047(5) 0.034(5) -0.006(4) 0.006(4) -0.021(4) C33 0.022(4) 0.027(5) 0.054(6) -0.002(4) -0.002(4) -0.008(4) C34 0.019(4) 0.035(5) 0.037(5) -0.007(4) 0.003(3) -0.008(4) C35 0.029(5) 0.042(5) 0.043(5) -0.015(4) 0.011(4) -0.021(4) C36 0.016(4) 0.053(6) 0.025(4) 0.001(4) -0.001(3) -0.022(4) C37 0.024(4) 0.044(5) 0.019(4) 0.002(4) -0.001(3) -0.018(4) C38 0.011(4) 0.041(5) 0.031(4) 0.000(4) 0.006(3) -0.010(3) C39 0.033(5) 0.037(5) 0.035(5) -0.002(4) 0.010(4) -0.015(4) C40 0.025(4) 0.067(6) 0.032(5) -0.016(4) 0.009(4) -0.026(4) C41 0.012(4) 0.034(5) 0.045(5) 0.002(4) 0.001(3) -0.009(3) C42 0.012(4) 0.051(5) 0.027(4) 0.001(4) 0.003(3) -0.014(4) C43 0.018(4) 0.040(5) 0.029(4) -0.001(4) -0.002(3) -0.013(4) C44 0.018(4) 0.039(5) 0.040(5) -0.006(4) 0.004(3) -0.013(4) C45 0.024(5) 0.037(5) 0.050(6) -0.001(4) -0.003(4) -0.015(4) C46 0.031(5) 0.032(5) 0.050(6) 0.007(4) -0.011(4) -0.013(4) C47 0.028(5) 0.037(5) 0.049(6) -0.012(4) 0.009(4) -0.010(4) C49 0.025(4) 0.051(6) 0.037(5) 0.005(4) 0.001(4) -0.017(4) C50 0.025(5) 0.063(7) 0.055(6) 0.017(5) -0.015(4) -0.027(5) C51 0.013(4) 0.060(6) 0.037(5) 0.008(4) 0.003(4) -0.009(4) C52 0.007(4) 0.076(7) 0.036(5) 0.006(5) 0.005(3) -0.008(4) C53 0.015(4) 0.065(6) 0.031(5) 0.005(4) -0.001(3) -0.010(4) C54 0.034(5) 0.066(7) 0.041(5) 0.006(5) -0.006(4) -0.015(5) C55 0.038(6) 0.058(7) 0.055(6) -0.005(5) 0.004(5) -0.017(5) C56 0.022(4) 0.066(7) 0.040(5) 0.008(5) 0.004(4) -0.014(4) C57 0.038(5) 0.071(7) 0.043(6) 0.005(5) -0.009(4) -0.034(5) C58 0.046(6) 0.051(6) 0.030(5) -0.003(4) 0.005(4) -0.021(5) C60 0.031(5) 0.046(6) 0.053(6) -0.001(5) 0.014(4) -0.014(4) C61 0.031(5) 0.054(6) 0.052(6) -0.003(5) 0.013(4) -0.004(5) C63 0.047(6) 0.060(7) 0.048(6) -0.015(5) -0.007(5) -0.017(5) C64 0.033(6) 0.070(8) 0.069(7) -0.017(6) 0.001(5) -0.014(5) C65 0.018(5) 0.112(10) 0.038(6) -0.020(6) 0.001(4) -0.004(6) C66 0.059(7) 0.096(9) 0.063(7) -0.029(7) 0.030(6) -0.055(7) C67 0.041(5) 0.069(7) 0.036(5) -0.013(5) 0.001(4) -0.029(5) C68 0.045(6) 0.070(8) 0.063(7) 0.002(6) 0.005(5) -0.006(6) C69 0.027(5) 0.065(7) 0.072(7) -0.018(6) 0.016(5) -0.025(5) C70 0.015(4) 0.058(6) 0.046(5) -0.015(5) 0.000(4) -0.011(4) C71 0.022(4) 0.050(6) 0.037(5) 0.003(4) -0.005(4) -0.008(4) C72 0.017(4) 0.046(5) 0.044(5) -0.005(4) -0.004(4) -0.014(4) C74 0.025(5) 0.057(6) 0.034(5) 0.004(4) 0.002(4) -0.006(4) C75 0.037(5) 0.046(6) 0.056(6) -0.006(5) 0.015(5) -0.028(5) C76 0.036(5) 0.064(6) 0.042(5) -0.011(5) 0.018(4) -0.037(5) O17 0.037(3) 0.028(3) 0.016(3) 0.006(2) -0.002(2) -0.017(2) O18 0.093(6) 0.061(5) 0.086(6) 0.000(4) 0.009(5) -0.027(5) O19 0.069(5) 0.097(6) 0.078(6) -0.016(5) 0.004(4) -0.034(5) O20 0.020(3) 0.087(6) 0.085(6) -0.016(4) -0.008(3) 0.002(3) O21 0.086(7) 0.078(6) 0.109(8) -0.026(5) -0.023(6) 0.014(5) O22 0.079(6) 0.083(6) 0.043(4) -0.004(4) -0.015(4) -0.013(4) O34 0.072(6) 0.077(6) 0.093(6) -0.015(5) 0.003(5) -0.028(5) O23 0.074(6) 0.102(7) 0.078(6) -0.027(5) 0.026(5) -0.042(5) O24 0.073(6) 0.097(7) 0.087(6) -0.036(5) -0.011(5) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.235(10) . ? O2 C4 1.229(10) . ? O3 C6 1.239(9) . ? O4 C8 1.233(9) . ? O5 C24 1.219(10) . ? O6 C22 1.249(10) . ? O7 C20 1.215(10) . ? O8 C18 1.233(10) . ? O9 C25 1.212(9) . ? O10 C27 1.193(9) . ? O11 C29 1.224(10) . ? O12 C31 1.250(10) . ? O13 C47 1.230(10) . ? O14 C45 1.221(10) . ? O15 C43 1.232(9) . ? O16 C41 1.231(9) . ? N1 C2 1.375(11) . ? N1 C16 1.426(10) . ? N1 C1 1.459(10) . ? N2 C2 1.352(11) . ? N2 C15 1.442(11) . ? N2 C3 1.443(11) . ? N3 C4 1.364(11) . ? N3 C3 1.442(11) . ? N3 C14 1.461(9) . ? N4 C4 1.364(11) . ? N4 C13 1.425(10) . ? N4 C5 1.435(11) . ? N5 C6 1.353(10) . ? N5 C12 1.418(10) . ? N5 C5 1.437(11) . ? N6 C6 1.367(11) . ? N6 C7 1.436(10) . ? N6 C11 1.466(10) . ? N7 C8 1.352(10) . ? N7 C7 1.430(10) . ? N7 C10 1.474(10) . ? N8 C8 1.361(11) . ? N8 C17 1.450(10) 2_656 ? N8 C9 1.454(10) . ? N9 C24 1.375(11) . ? N9 C1 1.412(11) 2_656 ? N9 C9 1.450(10) . ? N10 C24 1.356(11) . ? N10 C23 1.416(10) . ? N10 C10 1.464(10) . ? N11 C22 1.356(10) . ? N11 C11 1.423(10) . ? N11 C23 1.425(11) . ? N12 C22 1.354(11) . ? N12 C21 1.433(10) . ? N12 C12 1.455(10) . ? N13 C20 1.393(11) . ? N13 C21 1.454(11) . ? N13 C13 1.457(10) . ? N14 C20 1.352(11) . ? N14 C19 1.416(10) . ? N14 C14 1.451(10) . ? N15 C18 1.329(11) . ? N15 C19 1.451(10) . ? N15 C15 1.470(10) . ? N16 C18 1.366(11) . ? N16 C17 1.428(11) . ? N16 C16 1.456(10) . ? N17 C31 1.332(11) 2 ? N17 C32 1.433(10) 2 ? N17 C40 1.446(11) . ? N18 C41 1.374(10) . ? N18 C40 1.436(10) . ? N18 C39 1.458(10) . ? N19 C41 1.342(10) . ? N19 C42 1.415(10) . ? N19 C38 1.458(10) . ? N20 C43 1.347(10) . ? N20 C37 1.431(9) . ? N20 C42 1.448(10) . ? N21 C43 1.386(10) . ? N21 C44 1.440(10) . ? N21 C36 1.448(10) . ? N22 C45 1.363(11) . ? N22 C44 1.448(10) . ? N22 C35 1.462(10) . ? N23 C45 1.378(11) . ? N23 C46 1.424(11) . ? N23 C34 1.440(11) . ? N24 C47 1.349(11) . ? N24 C46 1.434(11) . ? N24 C33 1.472(10) . ? N25 C47 1.358(11) . ? N25 C32 1.456(10) . ? N25 C76 1.460(12) . ? N26 C31 1.356(11) . ? N26 C33 1.434(11) . ? N26 C30 1.461(11) . ? N27 C29 1.364(11) . ? N27 C34 1.429(10) . ? N27 C30 1.435(11) . ? N28 C29 1.359(11) . ? N28 C28 1.422(11) . ? N28 C35 1.448(10) . ? N29 C27 1.394(10) . ? N29 C36 1.440(9) . ? N29 C28 1.444(10) . ? N30 C27 1.367(10) . ? N30 C37 1.437(9) . ? N30 C26 1.456(10) . ? N31 C25 1.378(10) . ? N31 C26 1.411(10) . ? N31 C38 1.462(9) . ? N32 C25 1.348(11) . ? N32 C76 1.449(11) 2 ? N32 C39 1.450(10) . ? N33 C49 1.316(11) . ? N33 C53 1.336(11) . ? N34 C58 1.317(11) . ? N34 C60 1.331(11) . ? N35 C63 1.280(12) . ? N35 C67 1.301(12) . ? N36 C72 1.328(11) . ? N36 C74 1.339(11) . ? C1 N9 1.412(11) 2_656 ? C9 C10 1.546(11) . ? C11 C12 1.516(12) . ? C13 C14 1.519(12) . ? C15 C16 1.570(12) . ? C17 N8 1.451(10) 2_656 ? C31 N17 1.332(11) 2 ? C32 N17 1.433(10) 2 ? C32 C33 1.520(12) . ? C34 C35 1.550(12) . ? C36 C37 1.545(12) . ? C38 C39 1.522(12) . ? C49 C50 1.412(12) . ? C50 C51 1.373(14) . ? C51 C52 1.380(13) . ? C51 C54 1.467(12) . ? C52 C53 1.383(11) . ? C54 C55 1.298(13) . ? C55 C56 1.503(12) . ? C56 C57 1.352(14) . ? C56 C61 1.394(14) . ? C57 C58 1.414(12) . ? C60 C61 1.372(12) . ? C63 C64 1.389(14) . ? C64 C65 1.332(16) . ? C65 C66 1.430(17) . ? C65 C68 1.544(15) . ? C66 C67 1.401(14) . ? C68 C69 1.222(14) . ? C69 C70 1.470(13) . ? C70 C75 1.365(13) . ? C70 C71 1.388(13) . ? C71 C72 1.366(11) . ? C74 C75 1.388(13) . ? C76 N32 1.449(11) 2 ? 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 C16 112.7(7) . . ? C2 N1 C1 122.2(7) . . ? C16 N1 C1 121.7(7) . . ? C2 N2 C15 112.5(7) . . ? C2 N2 C3 122.4(7) . . ? C15 N2 C3 124.4(7) . . ? C4 N3 C3 121.7(7) . . ? C4 N3 C14 110.9(7) . . ? C3 N3 C14 122.1(6) . . ? C4 N4 C13 112.3(7) . . ? C4 N4 C5 121.5(7) . . ? C13 N4 C5 124.5(7) . . ? C6 N5 C12 112.5(7) . . ? C6 N5 C5 122.3(7) . . ? C12 N5 C5 124.2(6) . . ? C6 N6 C7 122.8(6) . . ? C6 N6 C11 111.0(6) . . ? C7 N6 C11 124.0(7) . . ? C8 N7 C7 121.5(7) . . ? C8 N7 C10 110.9(7) . . ? C7 N7 C10 121.7(7) . . ? C8 N8 C17 121.5(7) . 2_656 ? C8 N8 C9 111.4(6) . . ? C17 N8 C9 121.3(7) 2_656 . ? C24 N9 C1 122.6(7) . 2_656 ? C24 N9 C9 111.7(7) . . ? C1 N9 C9 120.4(7) 2_656 . ? C24 N10 C23 124.1(7) . . ? C24 N10 C10 112.6(7) . . ? C23 N10 C10 123.0(7) . . ? C22 N11 C11 110.5(7) . . ? C22 N11 C23 123.0(7) . . ? C11 N11 C23 124.0(7) . . ? C22 N12 C21 121.8(6) . . ? C22 N12 C12 110.2(6) . . ? C21 N12 C12 121.6(6) . . ? C20 N13 C21 120.5(7) . . ? C20 N13 C13 112.5(7) . . ? C21 N13 C13 121.8(7) . . ? C20 N14 C19 124.2(7) . . ? C20 N14 C14 112.4(7) . . ? C19 N14 C14 123.0(7) . . ? C18 N15 C19 123.4(7) . . ? C18 N15 C15 112.5(6) . . ? C19 N15 C15 124.0(6) . . ? C18 N16 C17 122.4(7) . . ? C18 N16 C16 112.7(7) . . ? C17 N16 C16 121.6(7) . . ? C31 N17 C32 112.1(7) 2 2 ? C31 N17 C40 121.7(7) 2 . ? C32 N17 C40 121.1(7) 2 . ? C41 N18 C40 122.2(7) . . ? C41 N18 C39 111.1(7) . . ? C40 N18 C39 123.5(7) . . ? C41 N19 C42 123.2(6) . . ? C41 N19 C38 112.7(6) . . ? C42 N19 C38 124.1(6) . . ? C43 N20 C37 112.7(6) . . ? C43 N20 C42 124.3(6) . . ? C37 N20 C42 122.5(6) . . ? C43 N21 C44 120.3(6) . . ? C43 N21 C36 110.3(7) . . ? C44 N21 C36 122.0(7) . . ? C45 N22 C44 120.1(6) . . ? C45 N22 C35 112.0(7) . . ? C44 N22 C35 120.5(7) . . ? C45 N23 C46 121.7(7) . . ? C45 N23 C34 111.9(7) . . ? C46 N23 C34 124.6(7) . . ? C47 N24 C46 124.7(7) . . ? C47 N24 C33 111.2(7) . . ? C46 N24 C33 121.7(7) . . ? C47 N25 C32 111.7(7) . . ? C47 N25 C76 121.4(7) . . ? C32 N25 C76 124.1(7) . . ? C31 N26 C33 110.4(7) . . ? C31 N26 C30 121.1(7) . . ? C33 N26 C30 123.7(7) . . ? C29 N27 C34 112.0(6) . . ? C29 N27 C30 121.1(7) . . ? C34 N27 C30 124.0(7) . . ? C29 N28 C28 124.1(7) . . ? C29 N28 C35 112.0(7) . . ? C28 N28 C35 121.7(7) . . ? C27 N29 C36 113.5(6) . . ? C27 N29 C28 121.2(6) . . ? C36 N29 C28 123.8(7) . . ? C27 N30 C37 113.3(6) . . ? C27 N30 C26 120.9(6) . . ? C37 N30 C26 121.0(6) . . ? C25 N31 C26 123.1(6) . . ? C25 N31 C38 111.5(6) . . ? C26 N31 C38 123.5(6) . . ? C25 N32 C76 121.1(7) . 2 ? C25 N32 C39 112.4(7) . . ? C76 N32 C39 123.4(7) 2 . ? C49 N33 C53 123.8(7) . . ? C58 N34 C60 122.6(7) . . ? C63 N35 C67 123.8(9) . . ? C72 N36 C74 122.1(7) . . ? N9 C1 N1 114.9(7) 2_656 . ? O1 C2 N2 126.5(8) . . ? O1 C2 N1 124.9(8) . . ? N2 C2 N1 108.6(8) . . ? N3 C3 N2 114.2(6) . . ? O2 C4 N4 126.4(8) . . ? O2 C4 N3 125.4(8) . . ? N4 C4 N3 108.2(7) . . ? N4 C5 N5 114.3(7) . . ? O3 C6 N5 126.7(8) . . ? O3 C6 N6 124.9(8) . . ? N5 C6 N6 108.4(7) . . ? N7 C7 N6 113.9(7) . . ? O4 C8 N7 124.8(8) . . ? O4 C8 N8 125.1(8) . . ? N7 C8 N8 110.1(7) . . ? N9 C9 N8 112.1(7) . . ? N9 C9 C10 103.8(6) . . ? N8 C9 C10 103.7(6) . . ? N10 C10 N7 113.7(7) . . ? N10 C10 C9 102.8(6) . . ? N7 C10 C9 103.0(6) . . ? N11 C11 N6 113.3(6) . . ? N11 C11 C12 105.2(6) . . ? N6 C11 C12 102.7(7) . . ? N5 C12 N12 114.9(7) . . ? N5 C12 C11 104.8(6) . . ? N12 C12 C11 103.2(6) . . ? N4 C13 N13 113.7(6) . . ? N4 C13 C14 104.3(6) . . ? N13 C13 C14 102.2(6) . . ? N14 C14 N3 113.8(6) . . ? N14 C14 C13 104.8(6) . . ? N3 C14 C13 103.0(6) . . ? N2 C15 N15 115.8(7) . . ? N2 C15 C16 103.0(6) . . ? N15 C15 C16 102.9(6) . . ? N1 C16 N16 113.7(7) . . ? N1 C16 C15 103.0(7) . . ? N16 C16 C15 102.0(6) . . ? N16 C17 N8 112.9(7) . 2_656 ? O8 C18 N15 125.9(8) . . ? O8 C18 N16 124.4(8) . . ? N15 C18 N16 109.7(7) . . ? N14 C19 N15 113.9(6) . . ? O7 C20 N14 126.7(8) . . ? O7 C20 N13 126.1(8) . . ? N14 C20 N13 107.1(7) . . ? N12 C21 N13 113.9(6) . . ? O6 C22 N12 124.5(8) . . ? O6 C22 N11 125.1(8) . . ? N12 C22 N11 110.3(7) . . ? N10 C23 N11 114.9(7) . . ? O5 C24 N10 126.7(8) . . ? O5 C24 N9 124.6(8) . . ? N10 C24 N9 108.7(7) . . ? O9 C25 N32 127.3(8) . . ? O9 C25 N31 124.3(8) . . ? N32 C25 N31 108.4(7) . . ? N31 C26 N30 113.4(6) . . ? O10 C27 N30 127.8(8) . . ? O10 C27 N29 126.4(8) . . ? N30 C27 N29 105.8(6) . . ? N28 C28 N29 114.3(7) . . ? O11 C29 N28 124.6(8) . . ? O11 C29 N27 126.4(8) . . ? N28 C29 N27 109.0(7) . . ? N27 C30 N26 112.8(7) . . ? O12 C31 N17 126.1(8) . 2 ? O12 C31 N26 124.3(9) . . ? N17 C31 N26 109.5(7) 2 . ? N17 C32 N25 114.1(7) 2 . ? N17 C32 C33 102.9(7) 2 . ? N25 C32 C33 103.7(6) . . ? N26 C33 N24 114.1(7) . . ? N26 C33 C32 104.3(7) . . ? N24 C33 C32 103.6(7) . . ? N27 C34 N23 114.8(7) . . ? N27 C34 C35 103.9(6) . . ? N23 C34 C35 104.0(6) . . ? N28 C35 N22 112.7(7) . . ? N28 C35 C34 102.8(7) . . ? N22 C35 C34 102.5(7) . . ? N29 C36 N21 113.3(6) . . ? N29 C36 C37 102.5(6) . . ? N21 C36 C37 103.3(6) . . ? N20 C37 N30 115.3(6) . . ? N20 C37 C36 103.3(6) . . ? N30 C37 C36 103.6(6) . . ? N19 C38 N31 114.9(6) . . ? N19 C38 C39 103.0(6) . . ? N31 C38 C39 103.1(6) . . ? N32 C39 N18 112.5(7) . . ? N32 C39 C38 104.2(6) . . ? N18 C39 C38 104.0(6) . . ? N18 C40 N17 113.4(7) . . ? O16 C41 N19 126.4(8) . . ? O16 C41 N18 124.7(8) . . ? N19 C41 N18 108.8(7) . . ? N19 C42 N20 113.6(6) . . ? O15 C43 N20 126.4(8) . . ? O15 C43 N21 124.8(8) . . ? N20 C43 N21 108.8(7) . . ? N21 C44 N22 112.3(6) . . ? O14 C45 N22 127.2(8) . . ? O14 C45 N23 124.3(8) . . ? N22 C45 N23 108.5(7) . . ? N23 C46 N24 114.5(7) . . ? O13 C47 N24 124.5(8) . . ? O13 C47 N25 125.9(9) . . ? N24 C47 N25 109.5(7) . . ? N33 C49 C50 118.8(9) . . ? C51 C50 C49 119.4(9) . . ? C50 C51 C52 119.0(8) . . ? C50 C51 C54 125.4(9) . . ? C52 C51 C54 115.6(9) . . ? C51 C52 C53 120.1(9) . . ? N33 C53 C52 118.8(9) . . ? C55 C54 C51 124.3(10) . . ? C54 C55 C56 123.6(10) . . ? C57 C56 C61 119.4(8) . . ? C57 C56 C55 124.6(9) . . ? C61 C56 C55 116.1(9) . . ? C56 C57 C58 119.4(9) . . ? N34 C58 C57 119.2(9) . . ? N34 C60 C61 120.2(9) . . ? C60 C61 C56 119.1(9) . . ? N35 C63 C64 122.7(11) . . ? C65 C64 C63 116.8(11) . . ? C64 C65 C66 120.7(10) . . ? C64 C65 C68 118.5(11) . . ? C66 C65 C68 120.6(11) . . ? C67 C66 C65 117.3(10) . . ? N35 C67 C66 118.6(10) . . ? C69 C68 C65 127.2(12) . . ? C68 C69 C70 126.6(12) . . ? C75 C70 C71 118.6(8) . . ? C75 C70 C69 125.4(9) . . ? C71 C70 C69 116.1(9) . . ? C72 C71 C70 120.1(8) . . ? N36 C72 C71 119.9(8) . . ? N36 C74 C75 119.3(8) . . ? C70 C75 C74 119.9(9) . . ? N32 C76 N25 111.6(7) 2 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.232 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.158