data_bcn258_1sq _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H58 N8 O6 I4, C H Cl3, C6 H14' _chemical_formula_sum 'C81 H73 Cl3 I4 N8 O6' _chemical_formula_weight 1868.42 _publ_section_references ; Bruker-Nonius AXS. (2004). APEX2 and SAINT. Bruker-Nonius AXS, Madison, Wisconsin, USA. CCDC. (2004). enCIFer. The Cambridge Crystallographic Data Centre, Cambridge, UK. Sheldrick, G. M. (2001). XCIF, XL, and XS. Bruker-Nonius AXS, Madison, Wisconsin, USA. Sheldrick, G. M. (2003). XPREP. Bruker-Nonius AXS, Madison, Wisconsin, USA. ; 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' I I -0.4742 1.8119 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2502(7) _cell_length_b 16.0849(8) _cell_length_c 17.9953(10) _cell_angle_alpha 86.541(3) _cell_angle_beta 82.282(3) _cell_angle_gamma 82.283(3) _cell_volume 3762.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7234 _cell_measurement_theta_min 2.3367 _cell_measurement_theta_max 26.1734 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'blue green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 1.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5293 _exptl_absorpt_correction_T_max 0.9645 _exptl_absorpt_process_details 'Sheldrick, G. M. (2004). SADABS. University of G\"ottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-ApexII CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 63848 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13265 _reflns_number_gt 9458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2004)' _computing_cell_refinement 'Apex2 (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 2001)' _computing_publication_material 'enCIFer (CCDC, 2004)' _refine_special_details ; Badly disordered solvent is present. The volume was analyzed with SQUEEZE (Spek, 2006) and modeled as containing a disordered hexane molecule. The chemical formula and dependent values reflect this addition. The void space calculation revealed a void of 370 e.A-3 with a count of 92 electrons. This is a reasonable value for a molecule of hexane. The largest peaks in the final difference map, approximately 4 e^-^/\%A^3^, are located near the iodine positions and are likely artifacts. 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^)+(0.0851P)^2^+39.8820P] 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 13265 _refine_ls_number_parameters 902 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2155 _refine_ls_wR_factor_gt 0.2017 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.5827(5) 0.3704(4) 0.8270(3) 0.0175(13) Uani 1 1 d . . . N2 N 0.4097(5) 0.3368(4) 0.9105(3) 0.0207(14) Uani 1 1 d . . . H2N H 0.4203 0.3437 0.8613 0.025 Uiso 1 1 calc R . . N3 N 0.0109(5) 0.6524(4) 0.8532(3) 0.0190(13) Uani 1 1 d . . . H3N H 0.0475 0.6417 0.8095 0.023 Uiso 1 1 calc R . . N4 N 0.0746(5) 0.7654(4) 0.7483(3) 0.0197(14) Uani 1 1 d . . . N5 N 0.1692(5) 0.7020(4) 0.6187(4) 0.0237(15) Uani 1 1 d . . . H5N H 0.1394 0.6737 0.6570 0.028 Uiso 1 1 calc R . . N6 N 0.5717(5) 0.3861(4) 0.6811(3) 0.0226(14) Uani 1 1 d . . . H6N H 0.5225 0.3750 0.7168 0.027 Uiso 1 1 calc R . . O1 O 0.4803(5) 0.3398(5) 1.0167(3) 0.0423(17) Uani 1 1 d . . . O2 O -0.0617(5) 0.7560(4) 0.9309(3) 0.0351(15) Uani 1 1 d . . . O3 O 0.2061(5) 0.8304(4) 0.5743(3) 0.0399(16) Uani 1 1 d . . . O4 O 0.7377(4) 0.4112(4) 0.6558(3) 0.0308(14) Uani 1 1 d . . . C1 C 0.5816(6) 0.3687(5) 0.9009(4) 0.0195(16) Uani 1 1 d . . . C2 C 0.6612(6) 0.3923(6) 0.9340(5) 0.031(2) Uani 1 1 d . . . H2 H 0.6579 0.3919 0.9871 0.037 Uiso 1 1 calc R . . C3 C 0.7453(7) 0.4164(7) 0.8885(5) 0.038(2) Uani 1 1 d . . . H3 H 0.8013 0.4319 0.9102 0.045 Uiso 1 1 calc R . . C4 C 0.7484(6) 0.4180(6) 0.8109(5) 0.0303(19) Uani 1 1 d . . . H4 H 0.8053 0.4350 0.7784 0.036 Uiso 1 1 calc R . . C5 C 0.6656(6) 0.3938(5) 0.7833(4) 0.0201(16) Uani 1 1 d . . . C6 C 0.4856(6) 0.3463(5) 0.9483(4) 0.0241(17) Uani 1 1 d . . . C7 C 0.3097(6) 0.3160(5) 0.9440(4) 0.0233(17) Uani 1 1 d . . . H7A H 0.3112 0.3036 0.9985 0.028 Uiso 1 1 calc R . . H7B H 0.2958 0.2647 0.9216 0.028 Uiso 1 1 calc R . . C8 C 0.2235(5) 0.3858(5) 0.9331(4) 0.0185(16) Uani 1 1 d . . . C9 C 0.1376(6) 0.3687(5) 0.9046(4) 0.0199(16) Uani 1 1 d . . . H9 H 0.1323 0.3130 0.8923 0.024 Uiso 1 1 calc R . . C10 C 0.0587(5) 0.4326(5) 0.8938(4) 0.0189(16) Uani 1 1 d . . . H10 H 0.0001 0.4198 0.8737 0.023 Uiso 1 1 calc R . . C11 C 0.0635(5) 0.5140(5) 0.9117(4) 0.0173(15) Uani 1 1 d . . . C12 C 0.1510(6) 0.5308(5) 0.9394(4) 0.0207(16) Uani 1 1 d . . . H12 H 0.1571 0.5865 0.9510 0.025 Uiso 1 1 calc R . . C13 C 0.2298(6) 0.4670(5) 0.9503(4) 0.0211(16) Uani 1 1 d . . . H13 H 0.2888 0.4796 0.9698 0.025 Uiso 1 1 calc R . . C14 C -0.0231(6) 0.5826(5) 0.9007(4) 0.0212(16) Uani 1 1 d . . . H14A H -0.0764 0.5592 0.8779 0.025 Uiso 1 1 calc R . . H14B H -0.0545 0.6035 0.9503 0.025 Uiso 1 1 calc R . . C15 C -0.0113(6) 0.7325(5) 0.8730(4) 0.0228(17) Uani 1 1 d . . . C16 C 0.0317(6) 0.7951(5) 0.8147(4) 0.0202(16) Uani 1 1 d . . . C17 C 0.0267(7) 0.8774(6) 0.8320(5) 0.033(2) Uani 1 1 d . . . H17 H -0.0055 0.8960 0.8795 0.040 Uiso 1 1 calc R . . C18 C 0.0693(8) 0.9330(6) 0.7792(6) 0.043(2) Uani 1 1 d . . . H18 H 0.0670 0.9904 0.7898 0.051 Uiso 1 1 calc R . . C19 C 0.1158(7) 0.9030(6) 0.7101(5) 0.035(2) Uani 1 1 d . . . H19 H 0.1463 0.9394 0.6727 0.042 Uiso 1 1 calc R . . C20 C 0.1165(6) 0.8189(5) 0.6972(4) 0.0260(18) Uani 1 1 d . . . C21 C 0.1683(6) 0.7833(5) 0.6240(4) 0.0269(18) Uani 1 1 d . . . C22 C 0.2168(7) 0.6562(6) 0.5531(4) 0.0288(19) Uani 1 1 d . . . H22A H 0.2454 0.6963 0.5146 0.035 Uiso 1 1 calc R . . H22B H 0.1635 0.6309 0.5318 0.035 Uiso 1 1 calc R . . C23 C 0.3020(6) 0.5874(5) 0.5698(4) 0.0242(18) Uani 1 1 d . . . C24 C 0.3885(6) 0.6058(5) 0.5970(4) 0.0240(17) Uani 1 1 d . . . H24 H 0.3939 0.6620 0.6078 0.029 Uiso 1 1 calc R . . C25 C 0.4678(6) 0.5424(5) 0.6089(4) 0.0260(18) Uani 1 1 d . . . H25 H 0.5267 0.5555 0.6283 0.031 Uiso 1 1 calc R . . C26 C 0.4614(6) 0.4604(5) 0.5927(4) 0.0247(18) Uani 1 1 d . . . C27 C 0.3749(7) 0.4427(5) 0.5659(4) 0.0267(18) Uani 1 1 d . . . H27 H 0.3694 0.3866 0.5548 0.032 Uiso 1 1 calc R . . C28 C 0.2956(6) 0.5054(5) 0.5549(4) 0.0262(18) Uani 1 1 d . . . H28 H 0.2359 0.4919 0.5368 0.031 Uiso 1 1 calc R . . C29 C 0.5497(6) 0.3919(6) 0.6039(4) 0.0276(19) Uani 1 1 d . . . H29A H 0.5318 0.3374 0.5905 0.033 Uiso 1 1 calc R . . H29B H 0.6117 0.4043 0.5701 0.033 Uiso 1 1 calc R . . C30 C 0.6620(6) 0.3965(5) 0.7006(4) 0.0222(17) Uani 1 1 d . . . N7 N 0.5112(5) 0.7510(4) 0.8154(4) 0.0240(15) Uani 1 1 d . . . N8 N -0.0296(5) 0.1914(4) 0.6182(4) 0.0242(15) Uani 1 1 d . . . O5 O 0.3672(4) 0.3594(3) 0.7549(3) 0.0205(11) Uani 1 1 d . . . O6 O 0.1047(4) 0.5653(3) 0.7239(3) 0.0183(11) Uani 1 1 d . . . C31 C 0.2962(5) 0.4158(5) 0.7487(4) 0.0163(15) Uani 1 1 d . . . C32 C 0.2759(5) 0.5062(5) 0.7605(4) 0.0156(15) Uani 1 1 d . . . C33 C 0.1763(5) 0.5085(5) 0.7345(4) 0.0187(16) Uani 1 1 d . . . C34 C 0.1960(5) 0.4196(5) 0.7220(4) 0.0162(15) Uani 1 1 d . . . C35 C 0.3300(5) 0.5661(5) 0.7851(4) 0.0157(15) Uani 1 1 d . . . C36 C 0.4288(6) 0.5450(5) 0.8053(4) 0.0189(16) Uani 1 1 d . . . H36 H 0.4562 0.4874 0.8094 0.023 Uiso 1 1 calc R . . C37 C 0.4868(6) 0.6046(5) 0.8193(4) 0.0199(16) Uani 1 1 d . . . H37 H 0.5531 0.5881 0.8340 0.024 Uiso 1 1 calc R . . C38 C 0.4491(6) 0.6909(5) 0.8123(4) 0.0215(16) Uani 1 1 d . . . C39 C 0.3459(6) 0.7122(5) 0.7996(4) 0.0232(17) Uani 1 1 d . . . H39 H 0.3156 0.7692 0.8011 0.028 Uiso 1 1 calc R . . C40 C 0.2896(6) 0.6519(5) 0.7852(4) 0.0210(16) Uani 1 1 d . . . H40 H 0.2210 0.6679 0.7750 0.025 Uiso 1 1 calc R . . C41 C 0.6183(6) 0.7291(6) 0.8275(5) 0.0279(19) Uani 1 1 d . . . H41A H 0.6221 0.6866 0.8695 0.033 Uiso 1 1 calc R . . H41B H 0.6441 0.7797 0.8426 0.033 Uiso 1 1 calc R . . C42 C 0.6875(6) 0.6952(5) 0.7600(4) 0.0225(17) Uani 1 1 d . . . C43 C 0.7902(6) 0.6661(5) 0.7669(5) 0.0248(17) Uani 1 1 d . . . H43 H 0.8145 0.6684 0.8140 0.030 Uiso 1 1 calc R . . C44 C 0.8570(6) 0.6342(5) 0.7073(5) 0.0263(18) Uani 1 1 d . . . H44 H 0.9264 0.6140 0.7132 0.032 Uiso 1 1 calc R . . C45 C 0.8218(6) 0.6319(5) 0.6388(5) 0.0278(18) Uani 1 1 d . . . C46 C 0.7217(7) 0.6597(7) 0.6298(5) 0.037(2) Uani 1 1 d . . . H46 H 0.6982 0.6576 0.5824 0.044 Uiso 1 1 calc R . . C47 C 0.6560(6) 0.6904(6) 0.6901(5) 0.037(2) Uani 1 1 d . . . H47 H 0.5864 0.7090 0.6839 0.044 Uiso 1 1 calc R . . C48 C 0.4795(6) 0.8366(6) 0.7912(5) 0.034(2) Uani 1 1 d . . . H48A H 0.4403 0.8358 0.7481 0.041 Uiso 1 1 calc R . . H48B H 0.5416 0.8636 0.7731 0.041 Uiso 1 1 calc R . . C49 C 0.4138(8) 0.8902(6) 0.8512(7) 0.045(3) Uani 1 1 d . A . C50 C 0.3357(10) 0.9474(8) 0.8324(9) 0.077(4) Uani 1 1 d . . . H50 H 0.3170 0.9509 0.7830 0.092 Uiso 1 1 calc R . . C51 C 0.2818(9) 1.0023(8) 0.8881(11) 0.080(5) Uani 1 1 d . A . H51 H 0.2239 1.0399 0.8762 0.096 Uiso 1 1 calc R . . C52 C 0.3098(11) 1.0022(7) 0.9550(9) 0.067(4) Uani 1 1 d . . . C53 C 0.3814(15) 0.9414(9) 0.9756(9) 0.101(6) Uani 1 1 d . A . H53 H 0.3962 0.9369 1.0260 0.121 Uiso 1 1 calc R . . C54 C 0.4338(12) 0.8850(7) 0.9244(6) 0.073(4) Uani 1 1 d . . . H54 H 0.4842 0.8422 0.9400 0.088 Uiso 1 1 calc R A . C55 C 0.1409(6) 0.3613(5) 0.6957(4) 0.0212(16) Uani 1 1 d . . . C56 C 0.0373(6) 0.3851(5) 0.6858(4) 0.0164(15) Uani 1 1 d . . . H56 H 0.0066 0.4408 0.6960 0.020 Uiso 1 1 calc R . . C57 C -0.0203(6) 0.3297(5) 0.6619(4) 0.0222(17) Uani 1 1 d . . . H57 H -0.0908 0.3468 0.6575 0.027 Uiso 1 1 calc R . . C58 C 0.0245(6) 0.2473(5) 0.6438(4) 0.0204(16) Uani 1 1 d . . . C59 C 0.1296(6) 0.2250(5) 0.6526(5) 0.0260(18) Uani 1 1 d . . . H59 H 0.1628 0.1709 0.6392 0.031 Uiso 1 1 calc R . . C60 C 0.1841(6) 0.2800(5) 0.6801(5) 0.0249(17) Uani 1 1 d . . . H60 H 0.2530 0.2620 0.6886 0.030 Uiso 1 1 calc R . . C61 C -0.1329(6) 0.2153(5) 0.5986(5) 0.0291(19) Uani 1 1 d . . . H61A H -0.1386 0.1874 0.5520 0.035 Uiso 1 1 calc R . . H61B H -0.1424 0.2766 0.5873 0.035 Uiso 1 1 calc R . . C62 C -0.2185(7) 0.1945(5) 0.6568(6) 0.036(2) Uani 1 1 d . B . C63 C -0.2088(9) 0.1860(6) 0.7310(7) 0.053(3) Uani 1 1 d . . . H63 H -0.1454 0.1922 0.7478 0.063 Uiso 1 1 calc R . . C64 C -0.2943(12) 0.1676(7) 0.7840(8) 0.072(4) Uani 1 1 d . B . H64 H -0.2896 0.1614 0.8363 0.086 Uiso 1 1 calc R . . C65 C -0.3834(9) 0.1593(7) 0.7556(11) 0.076(5) Uani 1 1 d . . . C66 C -0.3933(10) 0.1688(8) 0.6813(9) 0.069(4) Uani 1 1 d . B . H66 H -0.4562 0.1632 0.6634 0.083 Uiso 1 1 calc R . . C67 C -0.3116(8) 0.1864(6) 0.6343(8) 0.054(3) Uani 1 1 d . . . H67 H -0.3181 0.1938 0.5823 0.065 Uiso 1 1 calc R B . C68 C 0.0164(7) 0.1064(5) 0.5993(5) 0.031(2) Uani 1 1 d . . . H68A H -0.0385 0.0696 0.6044 0.037 Uiso 1 1 calc R . . H68B H 0.0643 0.0851 0.6359 0.037 Uiso 1 1 calc R . . C69 C 0.0738(6) 0.1004(5) 0.5214(5) 0.0260(18) Uani 1 1 d . . . C70 C 0.0642(7) 0.1663(6) 0.4671(5) 0.034(2) Uani 1 1 d . . . H70 H 0.0243 0.2179 0.4807 0.041 Uiso 1 1 calc R . . C71 C 0.1110(7) 0.1579(6) 0.3946(5) 0.036(2) Uani 1 1 d . . . H71 H 0.1021 0.2028 0.3583 0.043 Uiso 1 1 calc R . . C72 C 0.1711(7) 0.0838(5) 0.3750(5) 0.032(2) Uani 1 1 d . . . C73 C 0.1837(7) 0.0184(6) 0.4271(6) 0.040(2) Uani 1 1 d . . . H73 H 0.2252 -0.0326 0.4134 0.048 Uiso 1 1 calc R . . C74 C 0.1356(7) 0.0278(5) 0.4996(6) 0.036(2) Uani 1 1 d . . . H74 H 0.1453 -0.0173 0.5356 0.043 Uiso 1 1 calc R . . I1 I 0.92475(5) 0.58786(4) 0.54683(3) 0.03875(19) Uani 1 1 d . . . I2 I 0.23101(9) 1.09269(5) 1.02619(7) 0.1062(5) Uani 1 1 d . A 1 I3 I -0.50748(10) 0.12387(6) 0.83222(9) 0.1206(6) Uani 1 1 d . B 1 I4 I 0.23605(5) 0.06758(4) 0.26321(4) 0.0463(2) Uani 1 1 d . . . C1S C -0.061(3) 0.1885(15) 0.9510(17) 0.064(10) Uani 0.540(7) 1 d P C 1 H1S H -0.0036 0.2035 0.9767 0.077 Uiso 0.540(7) 1 calc PR C 1 Cl1 Cl -0.0412(18) 0.0744(12) 0.9475(12) 0.077(5) Uani 0.540(7) 1 d P C 1 Cl2 Cl -0.0499(5) 0.2415(4) 0.8634(3) 0.0621(19) Uani 0.540(7) 1 d P C 1 Cl3 Cl -0.1760(5) 0.2234(4) 1.0093(4) 0.072(2) Uani 0.540(7) 1 d P C 1 C1S' C -0.012(3) 0.1728(19) 0.9262(18) 0.045(7) Uani 0.460(7) 1 d P C 2 H1S' H 0.0326 0.1763 0.9660 0.054 Uiso 0.460(7) 1 calc PR C 2 Cl1' Cl -0.076(2) 0.0828(13) 0.9393(15) 0.088(8) Uani 0.460(7) 1 d P C 2 Cl2' Cl -0.1187(6) 0.2521(4) 0.9329(5) 0.069(2) Uani 0.460(7) 1 d P C 2 Cl3' Cl 0.0556(5) 0.1777(4) 0.8357(3) 0.0489(18) Uani 0.460(7) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.013(3) 0.021(3) 0.016(3) -0.001(3) 0.000(2) 0.004(2) N2 0.013(3) 0.032(4) 0.015(3) 0.001(3) 0.003(3) 0.000(3) N3 0.017(3) 0.025(3) 0.013(3) -0.001(3) 0.003(2) -0.003(3) N4 0.019(3) 0.023(3) 0.017(3) 0.001(3) -0.005(3) 0.001(3) N5 0.022(3) 0.027(4) 0.018(3) 0.005(3) 0.003(3) 0.004(3) N6 0.016(3) 0.038(4) 0.012(3) -0.003(3) 0.004(3) -0.001(3) O1 0.032(4) 0.083(5) 0.015(3) 0.000(3) -0.003(3) -0.020(3) O2 0.042(4) 0.027(3) 0.029(3) -0.005(3) 0.014(3) 0.002(3) O3 0.051(4) 0.038(4) 0.024(3) 0.010(3) 0.010(3) -0.003(3) O4 0.019(3) 0.042(4) 0.027(3) 0.005(3) 0.008(2) 0.000(3) C1 0.015(4) 0.027(4) 0.015(4) -0.001(3) -0.003(3) 0.003(3) C2 0.023(4) 0.054(6) 0.017(4) -0.006(4) -0.005(3) -0.007(4) C3 0.022(4) 0.066(7) 0.028(5) -0.007(4) -0.003(4) -0.009(4) C4 0.019(4) 0.040(5) 0.032(5) -0.001(4) 0.002(4) -0.008(4) C5 0.013(4) 0.024(4) 0.022(4) -0.005(3) 0.002(3) 0.000(3) C6 0.019(4) 0.032(4) 0.020(4) -0.002(3) 0.002(3) -0.003(3) C7 0.016(4) 0.029(4) 0.023(4) 0.004(3) 0.005(3) -0.005(3) C8 0.015(4) 0.026(4) 0.011(3) 0.004(3) 0.009(3) -0.003(3) C9 0.017(4) 0.024(4) 0.018(4) -0.003(3) 0.007(3) -0.009(3) C10 0.011(3) 0.033(4) 0.012(4) -0.007(3) 0.005(3) -0.006(3) C11 0.013(4) 0.028(4) 0.009(3) -0.001(3) 0.006(3) -0.003(3) C12 0.021(4) 0.026(4) 0.015(4) -0.003(3) 0.006(3) -0.007(3) C13 0.019(4) 0.031(4) 0.013(4) 0.000(3) 0.004(3) -0.007(3) C14 0.015(4) 0.026(4) 0.021(4) -0.002(3) 0.004(3) -0.003(3) C15 0.022(4) 0.026(4) 0.018(4) -0.007(3) 0.007(3) -0.001(3) C16 0.022(4) 0.023(4) 0.013(4) 0.000(3) 0.000(3) 0.003(3) C17 0.037(5) 0.034(5) 0.026(5) -0.006(4) 0.003(4) -0.002(4) C18 0.061(7) 0.023(5) 0.041(6) 0.002(4) -0.002(5) -0.002(4) C19 0.046(6) 0.033(5) 0.025(5) 0.004(4) 0.002(4) -0.007(4) C20 0.028(4) 0.025(4) 0.023(4) 0.002(3) -0.007(3) 0.004(3) C21 0.026(4) 0.032(5) 0.020(4) 0.004(4) -0.004(3) 0.004(4) C22 0.028(5) 0.040(5) 0.016(4) 0.001(4) 0.001(3) 0.000(4) C23 0.020(4) 0.036(5) 0.011(4) 0.004(3) 0.010(3) 0.005(3) C24 0.028(4) 0.029(4) 0.014(4) -0.005(3) 0.003(3) -0.004(3) C25 0.025(4) 0.044(5) 0.010(4) -0.002(3) -0.003(3) -0.004(4) C26 0.019(4) 0.040(5) 0.011(4) -0.005(3) 0.004(3) 0.006(4) C27 0.034(5) 0.031(4) 0.014(4) -0.001(3) 0.003(3) -0.005(4) C28 0.025(4) 0.038(5) 0.013(4) 0.003(3) 0.001(3) -0.003(4) C29 0.020(4) 0.042(5) 0.016(4) 0.000(3) 0.004(3) 0.009(4) C30 0.012(4) 0.027(4) 0.024(4) 0.000(3) 0.004(3) 0.006(3) N7 0.013(3) 0.028(4) 0.031(4) -0.005(3) 0.001(3) -0.002(3) N8 0.025(4) 0.022(3) 0.027(4) 0.001(3) -0.010(3) -0.005(3) O5 0.014(3) 0.027(3) 0.019(3) -0.006(2) 0.002(2) 0.001(2) O6 0.012(3) 0.026(3) 0.016(3) -0.003(2) -0.003(2) 0.001(2) C31 0.013(4) 0.027(4) 0.008(3) -0.001(3) 0.003(3) -0.005(3) C32 0.011(3) 0.026(4) 0.008(3) 0.000(3) 0.004(3) 0.001(3) C33 0.011(4) 0.031(4) 0.013(4) -0.002(3) 0.007(3) -0.004(3) C34 0.011(3) 0.027(4) 0.010(3) -0.001(3) 0.001(3) -0.003(3) C35 0.012(3) 0.026(4) 0.007(3) -0.001(3) 0.004(3) -0.003(3) C36 0.018(4) 0.023(4) 0.012(4) -0.001(3) 0.001(3) 0.006(3) C37 0.015(4) 0.029(4) 0.015(4) -0.003(3) -0.002(3) 0.001(3) C38 0.015(4) 0.030(4) 0.018(4) -0.006(3) 0.005(3) -0.004(3) C39 0.016(4) 0.029(4) 0.022(4) -0.002(3) 0.006(3) 0.001(3) C40 0.011(4) 0.029(4) 0.020(4) 0.002(3) 0.005(3) -0.002(3) C41 0.016(4) 0.043(5) 0.026(4) -0.010(4) 0.002(3) -0.007(4) C42 0.015(4) 0.027(4) 0.027(4) -0.006(3) -0.001(3) -0.005(3) C43 0.017(4) 0.034(5) 0.024(4) 0.000(3) -0.004(3) -0.005(3) C44 0.014(4) 0.031(4) 0.035(5) 0.000(4) -0.011(3) 0.003(3) C45 0.022(4) 0.031(5) 0.028(4) -0.006(4) 0.005(3) -0.003(3) C46 0.022(4) 0.063(6) 0.025(5) -0.008(4) -0.002(4) -0.001(4) C47 0.014(4) 0.062(6) 0.035(5) -0.015(4) -0.002(4) -0.003(4) C48 0.019(4) 0.035(5) 0.049(6) -0.001(4) -0.002(4) -0.010(4) C49 0.034(5) 0.023(5) 0.074(8) -0.006(5) 0.010(5) -0.004(4) C50 0.052(8) 0.067(9) 0.117(12) -0.037(8) -0.029(8) 0.009(6) C51 0.035(6) 0.056(8) 0.150(15) -0.044(9) -0.016(8) 0.011(6) C52 0.063(8) 0.037(7) 0.093(10) -0.031(7) 0.036(8) -0.012(6) C53 0.151(16) 0.059(9) 0.067(9) -0.016(7) 0.059(10) 0.014(10) C54 0.112(11) 0.049(7) 0.035(6) 0.015(5) 0.027(7) 0.035(7) C55 0.016(4) 0.029(4) 0.016(4) -0.002(3) 0.006(3) -0.003(3) C56 0.024(4) 0.018(4) 0.005(3) -0.001(3) 0.001(3) 0.002(3) C57 0.018(4) 0.031(4) 0.017(4) -0.004(3) 0.001(3) -0.003(3) C58 0.024(4) 0.023(4) 0.016(4) 0.004(3) -0.008(3) -0.007(3) C59 0.028(4) 0.020(4) 0.028(4) -0.003(3) -0.005(4) 0.007(3) C60 0.019(4) 0.022(4) 0.030(4) -0.001(3) -0.001(3) 0.004(3) C61 0.026(4) 0.031(5) 0.031(5) 0.003(4) -0.007(4) -0.008(4) C62 0.039(5) 0.020(4) 0.049(6) -0.004(4) 0.002(4) -0.004(4) C63 0.062(7) 0.034(6) 0.062(7) -0.010(5) 0.014(6) -0.022(5) C64 0.099(11) 0.033(6) 0.073(9) -0.014(6) 0.044(8) -0.022(6) C65 0.037(7) 0.027(6) 0.151(15) -0.010(7) 0.046(8) -0.008(5) C66 0.045(7) 0.060(8) 0.091(11) 0.026(7) 0.007(7) 0.006(6) C67 0.029(5) 0.035(6) 0.096(9) 0.013(6) -0.007(6) -0.001(4) C68 0.042(5) 0.023(4) 0.032(5) 0.003(4) -0.017(4) -0.005(4) C69 0.029(4) 0.019(4) 0.033(5) -0.001(3) -0.013(4) -0.006(3) C70 0.035(5) 0.026(5) 0.039(5) -0.002(4) -0.006(4) 0.001(4) C71 0.038(5) 0.027(5) 0.041(5) 0.002(4) -0.004(4) -0.005(4) C72 0.030(5) 0.030(5) 0.040(5) -0.009(4) 0.002(4) -0.014(4) C73 0.033(5) 0.023(5) 0.062(7) -0.004(4) -0.002(5) 0.000(4) C74 0.040(5) 0.019(4) 0.050(6) -0.001(4) -0.015(5) -0.002(4) I1 0.0285(3) 0.0503(4) 0.0350(3) -0.0161(3) 0.0102(2) -0.0040(3) I2 0.0998(8) 0.0420(5) 0.1564(11) -0.0412(6) 0.0885(8) -0.0234(5) I3 0.1016(8) 0.0556(6) 0.1734(13) 0.0048(6) 0.0895(9) -0.0087(5) I4 0.0442(4) 0.0425(4) 0.0512(4) -0.0124(3) 0.0102(3) -0.0138(3) C1S 0.14(3) 0.006(11) 0.054(19) -0.005(11) -0.033(18) 0.000(16) Cl1 0.110(14) 0.041(6) 0.071(6) -0.014(4) 0.016(7) -0.005(6) Cl2 0.081(4) 0.063(3) 0.057(3) 0.012(3) -0.033(3) -0.041(3) Cl3 0.071(4) 0.063(4) 0.078(4) 0.009(3) -0.009(3) -0.003(3) C1S' 0.07(2) 0.020(15) 0.043(18) -0.010(11) -0.003(14) -0.006(13) Cl1' 0.111(17) 0.024(5) 0.114(13) 0.007(5) 0.040(11) -0.015(8) Cl2' 0.063(4) 0.044(4) 0.101(6) -0.025(4) -0.013(4) 0.003(3) Cl3' 0.074(4) 0.046(3) 0.032(3) -0.003(2) -0.005(3) -0.029(3) _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 1.328(9) . ? N1 C5 1.345(10) . ? N2 C6 1.317(10) . ? N2 C7 1.453(9) . ? N2 H2N 0.8800 . ? N3 C15 1.341(10) . ? N3 C14 1.452(10) . ? N3 H3N 0.8800 . ? N4 C20 1.337(10) . ? N4 C16 1.340(10) . ? N5 C21 1.316(11) . ? N5 C22 1.454(10) . ? N5 H5N 0.8800 . ? N6 C30 1.326(10) . ? N6 C29 1.453(10) . ? N6 H6N 0.8800 . ? O1 C6 1.222(10) . ? O2 C15 1.212(9) . ? O3 C21 1.234(10) . ? O4 C30 1.239(9) . ? C1 C2 1.384(11) . ? C1 C6 1.507(11) . ? C2 C3 1.377(12) . ? C2 H2 0.9500 . ? C3 C4 1.392(13) . ? C3 H3 0.9500 . ? C4 C5 1.373(11) . ? C4 H4 0.9500 . ? C5 C30 1.493(11) . ? C7 C8 1.514(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.375(11) . ? C8 C13 1.376(11) . ? C9 C10 1.389(11) . ? C9 H9 0.9500 . ? C10 C11 1.380(11) . ? C10 H10 0.9500 . ? C11 C12 1.385(11) . ? C11 C14 1.505(10) . ? C12 C13 1.387(11) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.518(11) . ? C16 C17 1.368(12) . ? C17 C18 1.381(13) . ? C17 H17 0.9500 . ? C18 C19 1.395(13) . ? C18 H18 0.9500 . ? C19 C20 1.385(12) . ? C19 H19 0.9500 . ? C20 C21 1.509(12) . ? C22 C23 1.519(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.376(12) . ? C23 C24 1.379(12) . ? C24 C25 1.392(12) . ? C24 H24 0.9500 . ? C25 C26 1.384(12) . ? C25 H25 0.9500 . ? C26 C27 1.371(12) . ? C26 C29 1.521(11) . ? C27 C28 1.382(12) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? N7 C38 1.358(10) . ? N7 C48 1.444(11) . ? N7 C41 1.459(10) . ? N8 C58 1.359(10) . ? N8 C61 1.455(10) . ? N8 C68 1.460(11) . ? O5 C31 1.228(9) . ? O6 C33 1.251(9) . ? C31 C34 1.465(10) . ? C31 C32 1.466(10) . ? C32 C35 1.399(10) . ? C32 C33 1.455(10) . ? C33 C34 1.445(11) . ? C34 C55 1.401(11) . ? C35 C36 1.399(10) . ? C35 C40 1.411(11) . ? C36 C37 1.361(11) . ? C36 H36 0.9500 . ? C37 C38 1.415(11) . ? C37 H37 0.9500 . ? C38 C39 1.410(11) . ? C39 C40 1.358(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.503(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C47 1.387(12) . ? C42 C43 1.398(11) . ? C43 C44 1.373(12) . ? C43 H43 0.9500 . ? C44 C45 1.380(12) . ? C44 H44 0.9500 . ? C45 C46 1.369(12) . ? C45 I1 2.092(8) . ? C46 C47 1.370(12) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.526(14) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.354(16) . ? C49 C54 1.373(17) . ? C50 C51 1.429(19) . ? C50 H50 0.9500 . ? C51 C52 1.31(2) . ? C51 H51 0.9500 . ? C52 C53 1.34(2) . ? C52 I2 2.075(11) . ? C53 C54 1.384(16) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.386(11) . ? C55 C56 1.405(11) . ? C56 C57 1.371(11) . ? C56 H56 0.9500 . ? C57 C58 1.417(11) . ? C57 H57 0.9500 . ? C58 C59 1.419(11) . ? C59 C60 1.366(12) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.496(13) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.354(15) . ? C62 C67 1.375(14) . ? C63 C64 1.431(16) . ? C63 H63 0.9500 . ? C64 C65 1.37(2) . ? C64 H64 0.9500 . ? C65 C66 1.36(2) . ? C65 I3 2.115(12) . ? C66 C67 1.331(17) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.504(12) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C74 1.378(12) . ? C69 C70 1.404(12) . ? C70 C71 1.372(13) . ? C70 H70 0.9500 . ? C71 C72 1.378(13) . ? C71 H71 0.9500 . ? C72 C73 1.375(13) . ? C72 I4 2.096(9) . ? C73 C74 1.381(14) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C1S Cl2 1.74(3) . ? C1S Cl3 1.78(4) . ? C1S Cl1 1.82(3) . ? C1S H1S 1.0000 . ? C1S' Cl3' 1.75(3) . ? C1S' Cl1' 1.76(4) . ? C1S' Cl2' 1.77(3) . ? C1S' H1S' 1.0000 . ? 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 C5 118.3(6) . . ? C6 N2 C7 124.8(7) . . ? C6 N2 H2N 117.6 . . ? C7 N2 H2N 117.6 . . ? C15 N3 C14 122.8(6) . . ? C15 N3 H3N 118.6 . . ? C14 N3 H3N 118.6 . . ? C20 N4 C16 118.0(7) . . ? C21 N5 C22 123.5(7) . . ? C21 N5 H5N 118.2 . . ? C22 N5 H5N 118.2 . . ? C30 N6 C29 123.4(7) . . ? C30 N6 H6N 118.3 . . ? C29 N6 H6N 118.3 . . ? N1 C1 C2 122.2(7) . . ? N1 C1 C6 117.0(7) . . ? C2 C1 C6 120.6(7) . . ? C3 C2 C1 118.7(8) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.0(8) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.0(8) . . ? C5 C4 H4 121.5 . . ? C3 C4 H4 121.5 . . ? N1 C5 C4 123.7(7) . . ? N1 C5 C30 116.3(6) . . ? C4 C5 C30 120.0(7) . . ? O1 C6 N2 124.1(7) . . ? O1 C6 C1 120.9(7) . . ? N2 C6 C1 115.0(7) . . ? N2 C7 C8 112.9(6) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C13 118.8(7) . . ? C9 C8 C7 120.0(7) . . ? C13 C8 C7 121.2(7) . . ? C8 C9 C10 120.3(7) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 121.4(7) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 117.8(7) . . ? C10 C11 C14 121.1(7) . . ? C12 C11 C14 121.1(7) . . ? C11 C12 C13 120.8(7) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C8 C13 C12 120.9(7) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? N3 C14 C11 112.4(6) . . ? N3 C14 H14A 109.1 . . ? C11 C14 H14A 109.1 . . ? N3 C14 H14B 109.1 . . ? C11 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O2 C15 N3 125.4(7) . . ? O2 C15 C16 120.7(7) . . ? N3 C15 C16 113.9(6) . . ? N4 C16 C17 123.3(7) . . ? N4 C16 C15 117.0(7) . . ? C17 C16 C15 119.8(7) . . ? C16 C17 C18 119.0(8) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C19 118.6(9) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C20 C19 C18 118.5(8) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? N4 C20 C19 122.7(8) . . ? N4 C20 C21 117.1(7) . . ? C19 C20 C21 120.3(8) . . ? O3 C21 N5 124.9(8) . . ? O3 C21 C20 119.6(8) . . ? N5 C21 C20 115.5(7) . . ? N5 C22 C23 113.4(6) . . ? N5 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? N5 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C28 C23 C24 118.9(7) . . ? C28 C23 C22 120.0(8) . . ? C24 C23 C22 121.0(8) . . ? C23 C24 C25 120.2(8) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.5(8) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 118.8(8) . . ? C27 C26 C29 121.1(8) . . ? C25 C26 C29 120.1(7) . . ? C26 C27 C28 120.8(8) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 120.8(8) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? N6 C29 C26 111.3(6) . . ? N6 C29 H29A 109.4 . . ? C26 C29 H29A 109.4 . . ? N6 C29 H29B 109.4 . . ? C26 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O4 C30 N6 124.6(7) . . ? O4 C30 C5 120.9(7) . . ? N6 C30 C5 114.5(6) . . ? C38 N7 C48 120.2(7) . . ? C38 N7 C41 121.4(7) . . ? C48 N7 C41 117.1(7) . . ? C58 N8 C61 122.2(7) . . ? C58 N8 C68 122.2(7) . . ? C61 N8 C68 115.2(6) . . ? O5 C31 C34 133.8(7) . . ? O5 C31 C32 136.7(7) . . ? C34 C31 C32 89.5(6) . . ? C35 C32 C33 134.8(7) . . ? C35 C32 C31 135.5(7) . . ? C33 C32 C31 89.7(6) . . ? O6 C33 C34 134.7(7) . . ? O6 C33 C32 134.5(7) . . ? C34 C33 C32 90.7(6) . . ? C55 C34 C33 134.6(7) . . ? C55 C34 C31 135.2(7) . . ? C33 C34 C31 90.1(6) . . ? C36 C35 C32 121.8(7) . . ? C36 C35 C40 117.0(7) . . ? C32 C35 C40 121.0(7) . . ? C37 C36 C35 121.8(7) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C36 C37 C38 120.5(7) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? N7 C38 C39 121.2(7) . . ? N7 C38 C37 121.1(7) . . ? C39 C38 C37 117.7(7) . . ? C40 C39 C38 120.4(7) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C35 121.9(7) . . ? C39 C40 H40 119.1 . . ? C35 C40 H40 119.1 . . ? N7 C41 C42 114.1(7) . . ? N7 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? N7 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C47 C42 C43 116.9(7) . . ? C47 C42 C41 124.1(7) . . ? C43 C42 C41 119.0(7) . . ? C44 C43 C42 121.7(7) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C43 C44 C45 118.9(7) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 121.2(8) . . ? C46 C45 I1 119.8(6) . . ? C44 C45 I1 119.0(6) . . ? C45 C46 C47 119.0(8) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C46 C47 C42 122.3(8) . . ? C46 C47 H47 118.9 . . ? C42 C47 H47 118.9 . . ? N7 C48 C49 114.9(8) . . ? N7 C48 H48A 108.5 . . ? C49 C48 H48A 108.5 . . ? N7 C48 H48B 108.5 . . ? C49 C48 H48B 108.5 . . ? H48A C48 H48B 107.5 . . ? C50 C49 C54 118.1(11) . . ? C50 C49 C48 120.0(11) . . ? C54 C49 C48 121.9(9) . . ? C49 C50 C51 118.7(14) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C52 C51 C50 121.8(12) . . ? C52 C51 H51 119.1 . . ? C50 C51 H51 119.1 . . ? C51 C52 C53 119.1(12) . . ? C51 C52 I2 116.9(11) . . ? C53 C52 I2 123.8(12) . . ? C52 C53 C54 120.8(16) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C49 C54 C53 120.7(13) . . ? C49 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C60 C55 C34 122.4(7) . . ? C60 C55 C56 118.2(7) . . ? C34 C55 C56 119.4(7) . . ? C57 C56 C55 121.5(7) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 120.5(7) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? N8 C58 C57 122.1(7) . . ? N8 C58 C59 120.7(7) . . ? C57 C58 C59 117.2(7) . . ? C60 C59 C58 121.2(7) . . ? C60 C59 H59 119.4 . . ? C58 C59 H59 119.4 . . ? C59 C60 C55 121.3(7) . . ? C59 C60 H60 119.3 . . ? C55 C60 H60 119.3 . . ? N8 C61 C62 115.8(7) . . ? N8 C61 H61A 108.3 . . ? C62 C61 H61A 108.3 . . ? N8 C61 H61B 108.3 . . ? C62 C61 H61B 108.3 . . ? H61A C61 H61B 107.4 . . ? C63 C62 C67 118.8(10) . . ? C63 C62 C61 122.7(9) . . ? C67 C62 C61 118.5(9) . . ? C62 C63 C64 119.9(12) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C65 C64 C63 116.8(14) . . ? C65 C64 H64 121.6 . . ? C63 C64 H64 121.6 . . ? C66 C65 C64 123.2(12) . . ? C66 C65 I3 119.4(11) . . ? C64 C65 I3 117.3(13) . . ? C67 C66 C65 117.7(13) . . ? C67 C66 H66 121.2 . . ? C65 C66 H66 121.2 . . ? C66 C67 C62 123.7(13) . . ? C66 C67 H67 118.2 . . ? C62 C67 H67 118.2 . . ? N8 C68 C69 114.1(7) . . ? N8 C68 H68A 108.7 . . ? C69 C68 H68A 108.7 . . ? N8 C68 H68B 108.7 . . ? C69 C68 H68B 108.7 . . ? H68A C68 H68B 107.6 . . ? C74 C69 C70 117.0(8) . . ? C74 C69 C68 120.9(8) . . ? C70 C69 C68 122.1(7) . . ? C71 C70 C69 121.6(8) . . ? C71 C70 H70 119.2 . . ? C69 C70 H70 119.2 . . ? C70 C71 C72 119.4(9) . . ? C70 C71 H71 120.3 . . ? C72 C71 H71 120.3 . . ? C73 C72 C71 120.5(9) . . ? C73 C72 I4 119.5(7) . . ? C71 C72 I4 119.8(7) . . ? C72 C73 C74 119.3(8) . . ? C72 C73 H73 120.4 . . ? C74 C73 H73 120.4 . . ? C69 C74 C73 122.1(9) . . ? C69 C74 H74 119.0 . . ? C73 C74 H74 119.0 . . ? Cl2 C1S Cl3 113.0(16) . . ? Cl2 C1S Cl1 114.6(16) . . ? Cl3 C1S Cl1 111(2) . . ? Cl2 C1S H1S 105.8 . . ? Cl3 C1S H1S 105.8 . . ? Cl1 C1S H1S 105.8 . . ? Cl3' C1S' Cl1' 110.6(18) . . ? Cl3' C1S' Cl2' 109.4(19) . . ? Cl1' C1S' Cl2' 100(2) . . ? Cl3' C1S' H1S' 112.0 . . ? Cl1' C1S' H1S' 112.0 . . ? Cl2' C1S' H1S' 112.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O5 0.88 2.12 2.921(8) 151.7 . N3 H3N O6 0.88 2.03 2.842(8) 152.7 . N5 H5N O6 0.88 2.12 2.952(8) 156.4 . N6 H6N O5 0.88 2.12 2.926(8) 151.8 . 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 1 0.500 0.000 0.500 369.8 92.2 _platon_squeeze_details ; ? ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.747 _refine_diff_density_min -4.404 _refine_diff_density_rms 0.167 _chemical_compound_source synthesized _vrf_PLAT220_bcn258_1sq ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.56 Ratio RESPONSE: This atom is on the periphery of the molecule on a phneyl group that exhibits some large thermal motion behavior. It in no way influences the overall strutcural analysis. ; _vrf_PLAT222_bcn258_1sq ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.05 Ratio RESPONSE: This hydrogen is bonded to the carbon described above. ; # end Validation Reply Form