# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'George Koutsantonis' _publ_contact_author_email GEORGE.KOUTSANTONIS@UWA.EDU.AU _publ_section_title ; Long Tailed Cage Amines: Synthesis, Metal Complexation, and Structure ; loop_ _publ_author_name 'G Koutsantonis' 'B Dittrich' 'Jack Harrowfield' 'Gareth L Nealon' 'Brian W Skelton' # Attachment 'gk161_204_165_165a_203_paper.cif' data_gnhcl # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 688325' _audit_creation_date 2009-06-10T19:58:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C15 H43.67 Cl4 N7 O2.33' _chemical_formula_moiety 'C15 H39 N7, 4(Cl),7/4(H2 O)' _chemical_formula_weight 501.37 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.116(5) _cell_length_b 16.196(4) _cell_length_c 45.918(11) _cell_angle_alpha 90 _cell_angle_beta 99.887(3) _cell_angle_gamma 90 _cell_volume 14738(6) _cell_formula_units_Z 24 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6106 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6464 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .84 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_number 93467 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 0.9 _diffrn_reflns_theta_max 25.87 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.909 _reflns_number_total 25982 _reflns_number_gt 18999 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEPII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+91.3350P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 25982 _refine_ls_number_parameters 1636 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0847 _refine_ls_wR_factor_ref 0.2125 _refine_ls_wR_factor_gt 0.2005 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_restrained_S_all 1.12 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.602 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.111 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.48397(7) 0.42091(8) 0.42883(3) 0.0237(3) Uani 1 1 d . . . Cl2 Cl 0.67969(7) -0.08120(8) 0.40101(3) 0.0258(3) Uani 1 1 d . . . Cl3 Cl 0.47160(7) 0.70547(9) 0.46739(3) 0.0247(3) Uani 1 1 d . . . Cl4 Cl 1.30572(7) 0.80364(9) 0.63414(3) 0.0235(3) Uani 1 1 d . . . Cl5 Cl 0.35134(7) 0.55449(8) 0.49695(3) 0.0258(3) Uani 1 1 d . . . Cl6 Cl 0.33476(7) 0.07181(8) 0.34661(3) 0.0241(3) Uani 1 1 d . . . Cl7 Cl 0.65005(7) 0.40705(9) 0.75938(3) 0.0273(3) Uani 1 1 d . . . Cl8 Cl 0.18335(7) 0.42703(8) 0.52404(3) 0.0209(3) Uani 1 1 d . . . Cl9 Cl 0.50804(7) 0.94967(8) 0.32260(3) 0.0264(3) Uani 1 1 d . . . Cl10 Cl 1.15922(7) 0.40981(9) 0.76220(3) 0.0265(3) Uani 1 1 d . . . Cl11 Cl 0.98625(8) 0.93961(8) 0.30824(3) 0.0280(3) Uani 1 1 d . . . Cl12 Cl 0.63914(7) 0.79465(10) 0.30111(3) 0.0283(3) Uani 1 1 d . . . Cl13 Cl 0.81385(8) 1.05583(9) 0.33068(4) 0.0339(4) Uani 1 1 d . . . Cl14 Cl 1.14500(7) 0.82653(9) 0.30331(3) 0.0247(3) Uani 1 1 d . . . Cl15 Cl 0.39301(8) -0.02849(10) 0.45627(3) 0.0346(4) Uani 1 1 d . . . Cl16 Cl 0.77543(8) 0.47728(10) 0.37439(3) 0.0330(4) Uani 1 1 d . . . Cl17 Cl 0.04362(7) 0.52628(9) 0.46045(3) 0.0252(3) Uani 1 1 d . . . Cl18 Cl 0.13174(7) 0.00771(9) 0.37139(3) 0.0240(3) Uani 1 1 d . . . Cl19 Cl -0.00545(8) 0.44071(9) 0.35510(3) 0.0336(4) Uani 1 1 d . . . Cl20 Cl 0.81053(7) 0.74342(11) 0.63633(3) 0.0346(4) Uani 1 1 d . . . Cl21 Cl 0.97081(8) 0.77726(9) 0.46061(3) 0.0294(3) Uani 1 1 d . . . Cl22 Cl 0.58231(9) 0.53960(11) 0.29315(4) 0.0430(4) Uani 1 1 d . . . Cl23 Cl 0.17589(12) -0.05789(12) 0.47494(5) 0.0636(6) Uani 1 1 d . . . Cl25 Cl 0.22553(11) 0.56812(13) 0.32914(4) 0.0403(7) Uani 0.816(5) 1 d P . . Cl26 Cl 0.2993(8) 0.5677(7) 0.3230(2) 0.073(6) Uani 0.184(5) 1 d P . . N10 N 0.2547(2) 0.9064(3) 0.35478(11) 0.0214(10) Uani 1 1 d . . . H10A H 0.2402 0.9134 0.3723 0.032 Uiso 1 1 calc R . . H10B H 0.2195 0.8906 0.3407 0.032 Uiso 1 1 calc R . . H10C H 0.2719 0.9549 0.3493 0.032 Uiso 1 1 calc R . . C11 C 0.3090(3) 0.8406(3) 0.35812(12) 0.0179(12) Uani 1 1 d . . . C12A C 0.3684(3) 0.8643(3) 0.38195(12) 0.0190(12) Uani 1 1 d . . . H12A H 0.3508 0.892 0.3983 0.023 Uiso 1 1 calc R . . H12B H 0.3916 0.8132 0.39 0.023 Uiso 1 1 calc R . . N13A N 0.4182(2) 0.9192(3) 0.37162(10) 0.0169(10) Uani 1 1 d . . . H13A H 0.3964 0.9656 0.3633 0.02 Uiso 1 1 calc R . . H13B H 0.4363 0.8924 0.3571 0.02 Uiso 1 1 calc R . . C14A C 0.4744(3) 0.9451(3) 0.39566(12) 0.0183(11) Uani 1 1 d . . . H14A H 0.4558 0.9797 0.4101 0.022 Uiso 1 1 calc R . . H14B H 0.507 0.9792 0.387 0.022 Uiso 1 1 calc R . . C15A C 0.5111(3) 0.8720(3) 0.41154(12) 0.0192(12) Uani 1 1 d . . . H15A H 0.5503 0.8916 0.4259 0.023 Uiso 1 1 calc R . . H15B H 0.4804 0.8419 0.4226 0.023 Uiso 1 1 calc R . . N16A N 0.5340(2) 0.8166(3) 0.39014(10) 0.0174(10) Uani 1 1 d D . . C17A C 0.5663(3) 0.7406(3) 0.40394(12) 0.0198(12) Uani 1 1 d . . . H17A H 0.5515 0.7318 0.4232 0.024 Uiso 1 1 calc R . . H17B H 0.6159 0.7486 0.4079 0.024 Uiso 1 1 calc R . . C12B C 0.3294(3) 0.8295(3) 0.32727(12) 0.0193(12) Uani 1 1 d . . . H12C H 0.2916 0.8047 0.3134 0.023 Uiso 1 1 calc R . . H12D H 0.3401 0.8839 0.3193 0.023 Uiso 1 1 calc R . . N13B N 0.3884(2) 0.7758(3) 0.33032(10) 0.0208(10) Uani 1 1 d D . . C14B C 0.4156(3) 0.7622(4) 0.30323(12) 0.0266(14) Uani 1 1 d . . . H14C H 0.4305 0.8151 0.2957 0.032 Uiso 1 1 calc R . . H14D H 0.3806 0.7378 0.2878 0.032 Uiso 1 1 calc R . . C15B C 0.4750(3) 0.7034(4) 0.31071(12) 0.0297(14) Uani 1 1 d . . . H15C H 0.4589 0.6496 0.317 0.036 Uiso 1 1 calc R . . H15D H 0.4956 0.694 0.2929 0.036 Uiso 1 1 calc R . . N16B N 0.5264(2) 0.7383(3) 0.33481(10) 0.0243(11) Uani 1 1 d . . . H16A H 0.5047 0.7705 0.3467 0.029 Uiso 1 1 calc R . . H16B H 0.5546 0.7722 0.3264 0.029 Uiso 1 1 calc R . . C17B C 0.5693(3) 0.6751(4) 0.35407(12) 0.0236(13) Uani 1 1 d . . . H17C H 0.6171 0.6925 0.3566 0.028 Uiso 1 1 calc R . . H17D H 0.5654 0.6213 0.3437 0.028 Uiso 1 1 calc R . . C12C C 0.2747(3) 0.7625(3) 0.36849(12) 0.0183(12) Uani 1 1 d . . . H12E H 0.2586 0.7749 0.3872 0.022 Uiso 1 1 calc R . . H12F H 0.235 0.7479 0.3535 0.022 Uiso 1 1 calc R . . N13C N 0.3209(2) 0.6921(3) 0.37301(10) 0.0198(10) Uani 1 1 d D . . C14C C 0.3354(3) 0.6618(4) 0.40365(13) 0.0249(13) Uani 1 1 d . . . H14E H 0.2924 0.648 0.4103 0.03 Uiso 1 1 calc R . . H14F H 0.3575 0.7063 0.4166 0.03 Uiso 1 1 calc R . . C15C C 0.3807(3) 0.5860(4) 0.40686(15) 0.0297(14) Uani 1 1 d . . . H15E H 0.3743 0.5557 0.4249 0.036 Uiso 1 1 calc R . . H15F H 0.3663 0.5492 0.3897 0.036 Uiso 1 1 calc R . . N16C N 0.4549(2) 0.6047(3) 0.40880(10) 0.0215(10) Uani 1 1 d . . . H16C H 0.4675 0.6417 0.424 0.026 Uiso 1 1 calc R . . H16D H 0.4788 0.5568 0.4137 0.026 Uiso 1 1 calc R . . C17C C 0.4752(3) 0.6394(3) 0.38126(12) 0.0196(12) Uani 1 1 d . . . H17E H 0.4474 0.6889 0.3751 0.023 Uiso 1 1 calc R . . H17F H 0.4651 0.598 0.3653 0.023 Uiso 1 1 calc R . . C18 C 0.5498(3) 0.6633(3) 0.38479(12) 0.0198(12) Uani 1 1 d . . . C19 C 0.5955(3) 0.5937(3) 0.39949(13) 0.0248(13) Uani 1 1 d . . . H19A H 0.5898 0.588 0.4202 0.037 Uiso 1 1 calc R . . H19B H 0.6427 0.607 0.3987 0.037 Uiso 1 1 calc R . . H19C H 0.5833 0.5417 0.389 0.037 Uiso 1 1 calc R . . N20 N 0.7471(2) 0.8903(3) 0.34605(10) 0.0195(10) Uani 1 1 d . . . H20A H 0.7309 0.9007 0.363 0.029 Uiso 1 1 calc R . . H20B H 0.7137 0.8684 0.3323 0.029 Uiso 1 1 calc R . . H20C H 0.762 0.9381 0.339 0.029 Uiso 1 1 calc R . . C21 C 0.8051(3) 0.8295(3) 0.35243(12) 0.0178(11) Uani 1 1 d . . . C22A C 0.8624(3) 0.8664(3) 0.37463(12) 0.0199(12) Uani 1 1 d . . . H22A H 0.8427 0.8976 0.3896 0.024 Uiso 1 1 calc R . . H22B H 0.8895 0.8208 0.385 0.024 Uiso 1 1 calc R . . N23A N 0.9080(2) 0.9221(3) 0.36172(10) 0.0190(10) Uani 1 1 d . . . H23A H 0.8827 0.9637 0.3517 0.023 Uiso 1 1 calc R . . H23B H 0.9273 0.8927 0.3482 0.023 Uiso 1 1 calc R . . C24A C 0.9630(3) 0.9600(3) 0.38371(13) 0.0236(13) Uani 1 1 d . . . H24A H 0.9426 0.9934 0.3979 0.028 Uiso 1 1 calc R . . H24B H 0.9899 0.9975 0.3733 0.028 Uiso 1 1 calc R . . C25A C 1.0091(3) 0.8958(3) 0.40044(12) 0.0211(12) Uani 1 1 d . . . H25A H 1.047 0.9237 0.4134 0.025 Uiso 1 1 calc R . . H25B H 0.9838 0.8633 0.4132 0.025 Uiso 1 1 calc R . . N26A N 1.0361(2) 0.8400(3) 0.37996(10) 0.0199(10) Uani 1 1 d D . . C27A C 1.0780(3) 0.7734(3) 0.39557(13) 0.0225(12) Uani 1 1 d . . . H27A H 1.0704 0.7713 0.4163 0.027 Uiso 1 1 calc R . . H27B H 1.1261 0.7868 0.3959 0.027 Uiso 1 1 calc R . . C22B C 0.8258(3) 0.8111(3) 0.32231(12) 0.0191(12) Uani 1 1 d . . . H22C H 0.7895 0.7797 0.3098 0.023 Uiso 1 1 calc R . . H22D H 0.8321 0.8637 0.3121 0.023 Uiso 1 1 calc R . . N23B N 0.8887(2) 0.7633(3) 0.32614(10) 0.0197(10) Uani 1 1 d D . . C24B C 0.9126(3) 0.7446(4) 0.29844(12) 0.0212(12) Uani 1 1 d . . . H24C H 0.9207 0.7963 0.2881 0.025 Uiso 1 1 calc R . . H24D H 0.8785 0.7115 0.2853 0.025 Uiso 1 1 calc R . . C25B C 0.9777(3) 0.6962(4) 0.30643(13) 0.0254(13) Uani 1 1 d . . . H25C H 0.968 0.6417 0.3145 0.03 Uiso 1 1 calc R . . H25D H 0.9975 0.6866 0.2884 0.03 Uiso 1 1 calc R . . N26B N 1.0273(2) 0.7416(3) 0.32873(10) 0.0190(10) Uani 1 1 d . . . H26A H 1.0038 0.7742 0.3399 0.023 Uiso 1 1 calc R . . H26B H 1.0522 0.7761 0.3188 0.023 Uiso 1 1 calc R . . C27B C 1.0756(3) 0.6876(4) 0.34946(12) 0.0227(13) Uani 1 1 d . . . H27C H 1.1222 0.7066 0.3492 0.027 Uiso 1 1 calc R . . H27D H 1.0718 0.6302 0.3419 0.027 Uiso 1 1 calc R . . C22C C 0.7773(3) 0.7530(3) 0.36613(12) 0.0175(11) Uani 1 1 d . . . H22E H 0.7598 0.7696 0.3841 0.021 Uiso 1 1 calc R . . H22F H 0.7392 0.7299 0.3519 0.021 Uiso 1 1 calc R . . N23C N 0.8289(2) 0.6893(3) 0.37383(10) 0.0174(10) Uani 1 1 d D . . C24C C 0.8477(3) 0.6726(3) 0.40540(12) 0.0208(12) Uani 1 1 d . . . H24E H 0.8079 0.6512 0.413 0.025 Uiso 1 1 calc R . . H24F H 0.8617 0.7248 0.4159 0.025 Uiso 1 1 calc R . . C25C C 0.9049(3) 0.6105(4) 0.41196(13) 0.0225(13) Uani 1 1 d . . . H25E H 0.9041 0.586 0.4317 0.027 Uiso 1 1 calc R . . H25F H 0.8963 0.5654 0.3972 0.027 Uiso 1 1 calc R . . N26C N 0.9745(2) 0.6443(3) 0.41163(10) 0.0200(10) Uani 1 1 d . . . H26C H 0.9791 0.6932 0.422 0.024 Uiso 1 1 calc R . . H26D H 1.0056 0.6078 0.4214 0.024 Uiso 1 1 calc R . . C27C C 0.9905(3) 0.6594(3) 0.38165(12) 0.0201(12) Uani 1 1 d . . . H27E H 0.9593 0.702 0.3717 0.024 Uiso 1 1 calc R . . H27F H 0.9822 0.608 0.37 0.024 Uiso 1 1 calc R . . C28 C 1.0632(3) 0.6877(3) 0.38152(12) 0.0197(12) Uani 1 1 d . . . C29 C 1.1146(3) 0.6256(4) 0.39804(13) 0.0249(13) Uani 1 1 d . . . H29A H 1.1145 0.6293 0.4193 0.037 Uiso 1 1 calc R . . H29B H 1.1598 0.6386 0.3941 0.037 Uiso 1 1 calc R . . H29C H 1.1022 0.5695 0.3912 0.037 Uiso 1 1 calc R . . N30 N 0.4137(2) 0.8848(3) 0.68382(10) 0.0174(10) Uani 1 1 d . . . H30A H 0.4312 0.9321 0.6775 0.026 Uiso 1 1 calc R . . H30B H 0.3975 0.895 0.7008 0.026 Uiso 1 1 calc R . . H30C H 0.3796 0.8664 0.6697 0.026 Uiso 1 1 calc R . . C31 C 0.4683(3) 0.8198(3) 0.68960(12) 0.0171(11) Uani 1 1 d . . . C32A C 0.5259(3) 0.8490(3) 0.71379(11) 0.0170(11) Uani 1 1 d . . . H32A H 0.5064 0.8808 0.7287 0.02 Uiso 1 1 calc R . . H32B H 0.5488 0.8 0.7238 0.02 Uiso 1 1 calc R . . N33A N 0.5769(2) 0.9009(3) 0.70281(9) 0.0161(9) Uani 1 1 d . . . H33A H 0.5556 0.9463 0.6935 0.019 Uiso 1 1 calc R . . H33B H 0.595 0.8713 0.689 0.019 Uiso 1 1 calc R . . C34A C 0.6335(3) 0.9299(3) 0.72632(12) 0.0210(12) Uani 1 1 d . . . H34A H 0.6148 0.9648 0.7407 0.025 Uiso 1 1 calc R . . H34B H 0.665 0.9642 0.7171 0.025 Uiso 1 1 calc R . . C35A C 0.6719(3) 0.8583(4) 0.74250(12) 0.0234(13) Uani 1 1 d . . . H35A H 0.7102 0.8796 0.757 0.028 Uiso 1 1 calc R . . H35B H 0.6417 0.8269 0.7534 0.028 Uiso 1 1 calc R . . N36A N 0.6973(2) 0.8035(3) 0.72135(11) 0.0229(11) Uani 1 1 d D . . C37A C 0.7315(3) 0.7305(4) 0.73667(13) 0.0264(13) Uani 1 1 d . . . H37A H 0.7186 0.7256 0.7565 0.032 Uiso 1 1 calc R . . H37B H 0.7809 0.7389 0.7395 0.032 Uiso 1 1 calc R . . C32B C 0.4913(3) 0.8043(3) 0.65965(11) 0.0188(12) Uani 1 1 d . . . H32C H 0.4545 0.7771 0.6459 0.023 Uiso 1 1 calc R . . H32D H 0.5014 0.8576 0.6508 0.023 Uiso 1 1 calc R . . N33B N 0.5512(2) 0.7520(3) 0.66383(10) 0.0200(10) Uani 1 1 d D . . C34B C 0.5777(3) 0.7352(4) 0.63657(12) 0.0243(13) Uani 1 1 d . . . H34C H 0.5928 0.7872 0.6284 0.029 Uiso 1 1 calc R . . H34D H 0.5423 0.71 0.6216 0.029 Uiso 1 1 calc R . . C35B C 0.6366(3) 0.6765(4) 0.64429(13) 0.0239(13) Uani 1 1 d . . . H35C H 0.6205 0.6236 0.6514 0.029 Uiso 1 1 calc R . . H35D H 0.6565 0.6651 0.6264 0.029 Uiso 1 1 calc R . . N36B N 0.6891(2) 0.7131(3) 0.66780(10) 0.0211(10) Uani 1 1 d . . . H36A H 0.6677 0.7481 0.679 0.025 Uiso 1 1 calc R . . H36B H 0.7174 0.7447 0.6587 0.025 Uiso 1 1 calc R . . C37B C 0.7320(3) 0.6543(4) 0.68858(13) 0.0293(14) Uani 1 1 d . . . H37C H 0.7798 0.6717 0.6905 0.035 Uiso 1 1 calc R . . H37D H 0.7282 0.5985 0.6797 0.035 Uiso 1 1 calc R . . C32C C 0.4354(3) 0.7430(3) 0.70094(13) 0.0206(12) Uani 1 1 d . . . H32E H 0.4174 0.7579 0.719 0.025 Uiso 1 1 calc R . . H32F H 0.3969 0.7253 0.6858 0.025 Uiso 1 1 calc R . . N33C N 0.4822(2) 0.6742(3) 0.70763(10) 0.0195(10) Uani 1 1 d D . . C34C C 0.4987(3) 0.6503(4) 0.73877(12) 0.0240(13) Uani 1 1 d . . . H34E H 0.4566 0.6375 0.7462 0.029 Uiso 1 1 calc R . . H34F H 0.5209 0.6973 0.7504 0.029 Uiso 1 1 calc R . . C35C C 0.5454(3) 0.5753(4) 0.74324(14) 0.0257(13) Uani 1 1 d . . . H35E H 0.5395 0.5472 0.7618 0.031 Uiso 1 1 calc R . . H35F H 0.5315 0.5362 0.7268 0.031 Uiso 1 1 calc R . . N36C N 0.6193(2) 0.5954(3) 0.74479(11) 0.0294(12) Uani 1 1 d . . . H36C H 0.6314 0.6337 0.7596 0.035 Uiso 1 1 calc R . . H36D H 0.6439 0.5483 0.7502 0.035 Uiso 1 1 calc R . . C37C C 0.6392(3) 0.6277(4) 0.71743(13) 0.0251(13) Uani 1 1 d . . . H37E H 0.6123 0.678 0.7114 0.03 Uiso 1 1 calc R . . H37F H 0.6271 0.5862 0.7016 0.03 Uiso 1 1 calc R . . C38 C 0.7137(3) 0.6490(3) 0.71958(12) 0.0200(12) Uani 1 1 d . . . C39 C 0.7588(3) 0.5813(4) 0.73601(13) 0.0260(13) Uani 1 1 d . . . H39A H 0.7525 0.5795 0.7567 0.039 Uiso 1 1 calc R . . H39B H 0.8062 0.5935 0.7352 0.039 Uiso 1 1 calc R . . H39C H 0.7465 0.5278 0.7267 0.039 Uiso 1 1 calc R . . N40 N 0.9190(3) 0.8943(3) 0.68725(12) 0.0343(13) Uani 1 1 d . . . H40A H 0.9377 0.9434 0.6834 0.051 Uiso 1 1 calc R . . H40B H 0.8993 0.8994 0.7036 0.051 Uiso 1 1 calc R . . H40C H 0.8872 0.8796 0.6715 0.051 Uiso 1 1 calc R . . C41 C 0.9730(3) 0.8289(3) 0.69259(12) 0.0209(12) Uani 1 1 d . . . C42A C 1.0262(3) 0.8526(3) 0.71931(12) 0.0237(13) Uani 1 1 d . . . H42A H 1.0036 0.8839 0.7334 0.028 Uiso 1 1 calc R . . H42B H 1.0444 0.8013 0.7294 0.028 Uiso 1 1 calc R . . N43A N 1.0834(2) 0.9023(3) 0.71274(10) 0.0231(11) Uani 1 1 d . . . H43A H 1.0669 0.9511 0.7041 0.028 Uiso 1 1 calc R . . H43B H 1.1036 0.8743 0.6992 0.028 Uiso 1 1 calc R . . C44A C 1.1361(3) 0.9221(4) 0.73909(14) 0.0316(15) Uani 1 1 d . . . H44A H 1.1144 0.9492 0.7544 0.038 Uiso 1 1 calc R . . H44B H 1.1691 0.9614 0.7332 0.038 Uiso 1 1 calc R . . C45A C 1.1729(3) 0.8457(4) 0.75212(13) 0.0275(14) Uani 1 1 d . . . H45A H 1.2088 0.8616 0.7688 0.033 Uiso 1 1 calc R . . H45B H 1.141 0.8086 0.7599 0.033 Uiso 1 1 calc R . . N46A N 1.2029(2) 0.8024(3) 0.72965(11) 0.0228(11) Uani 1 1 d D . . C47A C 1.2367(3) 0.7250(3) 0.74087(12) 0.0214(12) Uani 1 1 d . . . H47A H 1.2235 0.7113 0.7601 0.026 Uiso 1 1 calc R . . H47B H 1.2861 0.7338 0.7443 0.026 Uiso 1 1 calc R . . C42B C 0.9998(3) 0.8231(4) 0.66357(12) 0.0218(12) Uani 1 1 d . . . H42C H 0.9647 0.7987 0.6482 0.026 Uiso 1 1 calc R . . H42D H 1.01 0.8792 0.657 0.026 Uiso 1 1 calc R . . N43B N 1.0608(2) 0.7724(3) 0.66694(10) 0.0197(10) Uani 1 1 d D . . C44B C 1.0903(3) 0.7669(4) 0.64007(12) 0.0245(13) Uani 1 1 d . . . H44C H 1.1055 0.8221 0.6347 0.029 Uiso 1 1 calc R . . H44D H 1.0563 0.7462 0.6235 0.029 Uiso 1 1 calc R . . C45B C 1.1494(3) 0.7084(4) 0.64597(12) 0.0231(13) Uani 1 1 d . . . H45C H 1.1331 0.6525 0.65 0.028 Uiso 1 1 calc R . . H45D H 1.171 0.7049 0.6282 0.028 Uiso 1 1 calc R . . N46B N 1.2002(2) 0.7367(3) 0.67181(10) 0.0222(10) Uani 1 1 d . . . H46A H 1.1781 0.7665 0.6843 0.027 Uiso 1 1 calc R . . H46B H 1.23 0.7719 0.665 0.027 Uiso 1 1 calc R . . C47B C 1.2401(3) 0.6690(4) 0.68946(12) 0.0234(13) Uani 1 1 d . . . H47C H 1.2884 0.6844 0.6928 0.028 Uiso 1 1 calc R . . H47D H 1.235 0.6177 0.6776 0.028 Uiso 1 1 calc R . . C42C C 0.9395(3) 0.7488(3) 0.70116(12) 0.0206(12) Uani 1 1 d . . . H42E H 0.9213 0.7579 0.7196 0.025 Uiso 1 1 calc R . . H42F H 0.9014 0.7339 0.6854 0.025 Uiso 1 1 calc R . . N43C N 0.9885(2) 0.6811(3) 0.70547(10) 0.0176(10) Uani 1 1 d D . . C44C C 0.9988(3) 0.6420(3) 0.73455(12) 0.0220(12) Uani 1 1 d . . . H44E H 0.9548 0.623 0.7389 0.026 Uiso 1 1 calc R . . H44F H 1.0172 0.6832 0.7497 0.026 Uiso 1 1 calc R . . C45C C 1.0469(3) 0.5688(3) 0.73632(13) 0.0237(13) Uani 1 1 d . . . H45E H 1.0391 0.5328 0.7528 0.028 Uiso 1 1 calc R . . H45F H 1.0355 0.5363 0.7179 0.028 Uiso 1 1 calc R . . N46C N 1.1207(2) 0.5899(3) 0.74070(10) 0.0204(10) Uani 1 1 d . . . H46C H 1.1307 0.6239 0.7569 0.024 Uiso 1 1 calc R . . H46D H 1.1452 0.5421 0.7449 0.024 Uiso 1 1 calc R . . C47C C 1.1435(3) 0.6313(3) 0.71497(11) 0.0169(11) Uani 1 1 d . . . H47E H 1.118 0.6835 0.7107 0.02 Uiso 1 1 calc R . . H47F H 1.1321 0.5953 0.6974 0.02 Uiso 1 1 calc R . . C48 C 1.2193(3) 0.6510(3) 0.71954(12) 0.0201(12) Uani 1 1 d . . . C49 C 1.2624(3) 0.5776(4) 0.73255(14) 0.0290(14) Uani 1 1 d . . . H49A H 1.2553 0.5678 0.7529 0.044 Uiso 1 1 calc R . . H49B H 1.3101 0.5898 0.7326 0.044 Uiso 1 1 calc R . . H49C H 1.2492 0.5284 0.7206 0.044 Uiso 1 1 calc R . . N50 N 0.4212(2) 0.3864(3) 0.48503(10) 0.0180(10) Uani 1 1 d . . . H50A H 0.4394 0.3955 0.4685 0.027 Uiso 1 1 calc R . . H50B H 0.4535 0.3662 0.4996 0.027 Uiso 1 1 calc R . . H50C H 0.4049 0.4347 0.4911 0.027 Uiso 1 1 calc R . . C51 C 0.3645(3) 0.3247(3) 0.47821(12) 0.0162(11) Uani 1 1 d . . . C52A C 0.3069(3) 0.3611(3) 0.45587(12) 0.0182(12) Uani 1 1 d . . . H52A H 0.3265 0.3937 0.4412 0.022 Uiso 1 1 calc R . . H52B H 0.2809 0.3151 0.4452 0.022 Uiso 1 1 calc R . . N53A N 0.2598(2) 0.4146(3) 0.46880(9) 0.0172(10) Uani 1 1 d . . . H53A H 0.2841 0.4565 0.4791 0.021 Uiso 1 1 calc R . . H53B H 0.2408 0.3839 0.4821 0.021 Uiso 1 1 calc R . . C54A C 0.2042(3) 0.4519(3) 0.44694(12) 0.0214(12) Uani 1 1 d . . . H54A H 0.2241 0.4873 0.4331 0.026 Uiso 1 1 calc R . . H54B H 0.1762 0.4874 0.4576 0.026 Uiso 1 1 calc R . . C55A C 0.1597(3) 0.3869(3) 0.42945(12) 0.0223(12) Uani 1 1 d . . . H55A H 0.1212 0.4141 0.4167 0.027 Uiso 1 1 calc R . . H55B H 0.1859 0.3566 0.4165 0.027 Uiso 1 1 calc R . . N56A N 0.1344(2) 0.3289(3) 0.44929(10) 0.0200(10) Uani 1 1 d D . . C57A C 0.0931(3) 0.2627(4) 0.43312(13) 0.0239(13) Uani 1 1 d . . . H57A H 0.1001 0.2629 0.4123 0.029 Uiso 1 1 calc R . . H57B H 0.0449 0.2746 0.4332 0.029 Uiso 1 1 calc R . . C52B C 0.3439(3) 0.3027(3) 0.50814(11) 0.0179(12) Uani 1 1 d . . . H52C H 0.3807 0.2713 0.5204 0.022 Uiso 1 1 calc R . . H52D H 0.3363 0.3539 0.5188 0.022 Uiso 1 1 calc R . . N53B N 0.2821(2) 0.2529(3) 0.50329(10) 0.0188(10) Uani 1 1 d D . . C54B C 0.2592(3) 0.2270(4) 0.53030(12) 0.0217(12) Uani 1 1 d . . . H54C H 0.249 0.2758 0.5417 0.026 Uiso 1 1 calc R . . H54D H 0.2947 0.1942 0.5428 0.026 Uiso 1 1 calc R . . C55B C 0.1966(3) 0.1755(4) 0.52133(13) 0.0246(13) Uani 1 1 d . . . H55C H 0.2083 0.1241 0.5117 0.029 Uiso 1 1 calc R . . H55D H 0.1777 0.1601 0.5391 0.029 Uiso 1 1 calc R . . N56B N 0.1447(2) 0.2230(3) 0.50032(10) 0.0208(10) Uani 1 1 d . . . H56A H 0.1669 0.2591 0.4899 0.025 Uiso 1 1 calc R . . H56B H 0.1196 0.2539 0.5112 0.025 Uiso 1 1 calc R . . C57B C 0.0969(3) 0.1715(4) 0.47847(12) 0.0226(13) Uani 1 1 d . . . H57C H 0.0502 0.1898 0.4789 0.027 Uiso 1 1 calc R . . H57D H 0.1007 0.1131 0.485 0.027 Uiso 1 1 calc R . . C52C C 0.3941(3) 0.2506(3) 0.46366(12) 0.0175(11) Uani 1 1 d . . . H52E H 0.4117 0.2699 0.446 0.021 Uiso 1 1 calc R . . H52F H 0.4323 0.2274 0.4777 0.021 Uiso 1 1 calc R . . N53C N 0.3439(2) 0.1854(3) 0.45485(10) 0.0178(10) Uani 1 1 d D . . C54C C 0.3245(3) 0.1732(3) 0.42328(12) 0.0198(12) Uani 1 1 d . . . H54E H 0.3648 0.1568 0.4149 0.024 Uiso 1 1 calc R . . H54F H 0.3077 0.2261 0.414 0.024 Uiso 1 1 calc R . . C55C C 0.2702(3) 0.1077(4) 0.41560(13) 0.0252(13) Uani 1 1 d . . . H55E H 0.2726 0.086 0.3956 0.03 Uiso 1 1 calc R . . H55F H 0.2805 0.0614 0.4297 0.03 Uiso 1 1 calc R . . N56C N 0.1992(2) 0.1361(3) 0.41598(10) 0.0209(10) Uani 1 1 d . . . H56C H 0.1917 0.184 0.4051 0.025 Uiso 1 1 calc R . . H56D H 0.1699 0.0969 0.4068 0.025 Uiso 1 1 calc R . . C57C C 0.1834(3) 0.1517(4) 0.44618(12) 0.0210(12) Uani 1 1 d . . . H57E H 0.2133 0.1962 0.4557 0.025 Uiso 1 1 calc R . . H57F H 0.1937 0.1011 0.4582 0.025 Uiso 1 1 calc R . . C58 C 0.1098(3) 0.1763(3) 0.44626(12) 0.0192(12) Uani 1 1 d . . . C59 C 0.0598(3) 0.1144(4) 0.42896(13) 0.0270(14) Uani 1 1 d . . . H59A H 0.0597 0.1208 0.4077 0.04 Uiso 1 1 calc R . . H59B H 0.0144 0.1251 0.4331 0.04 Uiso 1 1 calc R . . H59C H 0.0734 0.058 0.435 0.04 Uiso 1 1 calc R . . N60 N 0.9015(2) 0.4100(3) 0.46717(10) 0.0214(10) Uani 1 1 d . . . H60A H 0.8825 0.4577 0.4722 0.032 Uiso 1 1 calc R . . H60B H 0.9121 0.4153 0.4488 0.032 Uiso 1 1 calc R . . H60C H 0.9397 0.3994 0.4804 0.032 Uiso 1 1 calc R . . C61 C 0.8526(3) 0.3401(3) 0.46732(12) 0.0193(12) Uani 1 1 d . . . C62A C 0.7897(3) 0.3552(3) 0.44408(12) 0.0170(11) Uani 1 1 d . . . H62A H 0.8037 0.378 0.4261 0.02 Uiso 1 1 calc R . . H62B H 0.7671 0.3016 0.4387 0.02 Uiso 1 1 calc R . . N63A N 0.7404(2) 0.4125(3) 0.45396(10) 0.0182(10) Uani 1 1 d . . . H63A H 0.7623 0.4605 0.4606 0.022 Uiso 1 1 calc R . . H63B H 0.7243 0.389 0.4696 0.022 Uiso 1 1 calc R . . C64A C 0.6815(3) 0.4334(3) 0.43007(12) 0.0204(12) Uani 1 1 d . . . H64A H 0.6495 0.4689 0.4385 0.024 Uiso 1 1 calc R . . H64B H 0.6979 0.465 0.4143 0.024 Uiso 1 1 calc R . . C65A C 0.6453(3) 0.3572(3) 0.41695(12) 0.0208(12) Uani 1 1 d . . . H65A H 0.6046 0.3733 0.4028 0.025 Uiso 1 1 calc R . . H65B H 0.6752 0.3253 0.4061 0.025 Uiso 1 1 calc R . . N66A N 0.6257(2) 0.3057(3) 0.44038(10) 0.0178(10) Uani 1 1 d D . . C67A C 0.5951(3) 0.2268(3) 0.42920(12) 0.0190(12) Uani 1 1 d . . . H67A H 0.6082 0.2148 0.4098 0.023 Uiso 1 1 calc R . . H67B H 0.5454 0.2323 0.4261 0.023 Uiso 1 1 calc R . . C62B C 0.8364(3) 0.3337(3) 0.49881(13) 0.0221(12) Uani 1 1 d . . . H62C H 0.8762 0.3121 0.5124 0.027 Uiso 1 1 calc R . . H62D H 0.8259 0.3892 0.5058 0.027 Uiso 1 1 calc R . . N63B N 0.7788(2) 0.2786(3) 0.49895(10) 0.0203(10) Uani 1 1 d D . . C64B C 0.7544(3) 0.2719(4) 0.52696(12) 0.0220(12) Uani 1 1 d . . . H64C H 0.7395 0.3266 0.533 0.026 Uiso 1 1 calc R . . H64D H 0.7909 0.2515 0.5426 0.026 Uiso 1 1 calc R . . C65B C 0.6961(3) 0.2123(3) 0.52275(12) 0.0215(12) Uani 1 1 d . . . H65C H 0.7122 0.1568 0.5182 0.026 Uiso 1 1 calc R . . H65D H 0.6774 0.2084 0.5413 0.026 Uiso 1 1 calc R . . N66B N 0.6421(2) 0.2400(3) 0.49815(9) 0.0170(10) Uani 1 1 d . . . H66A H 0.6619 0.2703 0.485 0.02 Uiso 1 1 calc R . . H66B H 0.6133 0.2747 0.5059 0.02 Uiso 1 1 calc R . . C67B C 0.6006(3) 0.1719(3) 0.48128(12) 0.0199(12) Uani 1 1 d . . . H67C H 0.5523 0.1869 0.4792 0.024 Uiso 1 1 calc R . . H67D H 0.6075 0.1207 0.4932 0.024 Uiso 1 1 calc R . . C62C C 0.8891(3) 0.2619(3) 0.45848(13) 0.0229(13) Uani 1 1 d . . . H62E H 0.9023 0.2709 0.4389 0.028 Uiso 1 1 calc R . . H62F H 0.9308 0.2528 0.473 0.028 Uiso 1 1 calc R . . N63C N 0.8464(2) 0.1885(3) 0.45721(10) 0.0204(10) Uani 1 1 d D . . C64C C 0.8306(3) 0.1505(4) 0.42804(13) 0.0244(13) Uani 1 1 d . . . H64E H 0.8731 0.1339 0.4215 0.029 Uiso 1 1 calc R . . H64F H 0.8078 0.1915 0.4137 0.029 Uiso 1 1 calc R . . C65C C 0.7855(3) 0.0754(3) 0.42811(14) 0.0256(13) Uani 1 1 d . . . H65E H 0.8003 0.0439 0.4466 0.031 Uiso 1 1 calc R . . H65F H 0.7913 0.0392 0.4114 0.031 Uiso 1 1 calc R . . N66C N 0.7111(2) 0.0963(3) 0.42576(10) 0.0183(10) Uani 1 1 d . . . H66C H 0.6992 0.1321 0.4102 0.022 Uiso 1 1 calc R . . H66D H 0.6864 0.0487 0.4215 0.022 Uiso 1 1 calc R . . C67C C 0.6924(3) 0.1344(3) 0.45306(12) 0.0169(11) Uani 1 1 d . . . H67E H 0.7181 0.1863 0.4575 0.02 Uiso 1 1 calc R . . H67F H 0.7059 0.0964 0.4699 0.02 Uiso 1 1 calc R . . C68 C 0.6165(3) 0.1534(3) 0.45030(12) 0.0188(12) Uani 1 1 d . . . C69 C 0.5734(3) 0.0783(4) 0.43900(13) 0.0245(13) Uani 1 1 d . . . H69A H 0.5756 0.0692 0.4181 0.037 Uiso 1 1 calc R . . H69B H 0.5265 0.0882 0.4412 0.037 Uiso 1 1 calc R . . H69C H 0.5906 0.0294 0.4505 0.037 Uiso 1 1 calc R . . O1 O 0.6237(3) 0.4206(3) 0.34384(12) 0.0537(14) Uani 1 1 d . . . O2 O 0.03071(19) 0.3585(2) 0.49235(9) 0.0263(9) Uani 1 1 d . . . O3 O 0.2486(3) 0.8980(3) 0.42008(9) 0.0422(12) Uani 1 1 d . . . O4 O 0.9465(3) 0.0798(4) 0.50024(17) 0.086(2) Uani 1 1 d . . . O5 O 0.7482(2) 0.5494(4) 0.61784(10) 0.0543(15) Uani 1 1 d . . . O6 O 0.1299(3) 0.4415(4) 0.68030(14) 0.0696(18) Uani 1 1 d . . . O7 O 0.2685(3) 0.4056(3) 0.67801(12) 0.0593(15) Uani 1 1 d . . . O8 O 0.5448(3) 0.9080(4) 0.49335(14) 0.0754(18) Uani 1 1 d . . . O9 O 0.0793(3) 1.0247(4) 0.54924(15) 0.080(2) Uani 1 1 d . . . O10 O 0.7025(10) 0.9662(11) 0.4985(3) 0.053(5) Uani 0.5 1 d P . . O10' O 0.6827(9) 0.9448(11) 0.4877(3) 0.043(4) Uani 0.5 1 d P . . O11 O 0.5137(6) 0.5404(6) 0.6578(2) 0.031(3) Uani 0.5 1 d P . . O11' O 0.5075(6) 0.5640(7) 0.6434(3) 0.036(3) Uani 0.5 1 d P . . O12 O 1.0882(4) 0.5984(5) 0.5924(2) 0.0315(14) Uani 0.5 1 d P . . O12' O 1.0363(4) 0.5953(5) 0.5842(2) 0.0315(14) Uani 0.5 1 d P . . O13 O 0.9218(3) 0.4909(4) 0.69567(14) 0.0557(19) Uani 0.816(5) 1 d P . . O13' O 0.8761(16) 0.4710(19) 0.6946(6) 0.052(8) Uiso 0.184(5) 1 d P . . O14 O 0.6348(4) 0.4331(4) 0.68932(14) 0.059(2) Uani 0.816(5) 1 d P . . O14' O 0.8753(13) 0.5804(16) 0.6507(6) 0.046(7) Uiso 0.184(5) 1 d P . . H16E H 0.564(3) 0.843(4) 0.3837(16) 0.055 Uiso 1 1 d D . . H13F H 0.381(4) 0.732(3) 0.3390(15) 0.055 Uiso 1 1 d D . . H13G H 0.302(4) 0.654(4) 0.3637(15) 0.055 Uiso 1 1 d D . . H26E H 1.056(3) 0.872(4) 0.3701(15) 0.055 Uiso 1 1 d D . . H23F H 0.882(4) 0.718(3) 0.3341(16) 0.055 Uiso 1 1 d D . . H23G H 0.813(4) 0.647(3) 0.3660(16) 0.055 Uiso 1 1 d D . . H36E H 0.724(3) 0.831(4) 0.7134(16) 0.055 Uiso 1 1 d D . . H33F H 0.545(4) 0.706(3) 0.6715(16) 0.055 Uiso 1 1 d D . . H33G H 0.468(4) 0.633(3) 0.6986(15) 0.055 Uiso 1 1 d D . . H46E H 1.227(3) 0.834(4) 0.7211(15) 0.055 Uiso 1 1 d D . . H43F H 1.050(4) 0.725(3) 0.6717(16) 0.055 Uiso 1 1 d D . . H43G H 0.973(4) 0.642(4) 0.6947(14) 0.055 Uiso 1 1 d D . . H56E H 0.111(3) 0.350(4) 0.4600(15) 0.055 Uiso 1 1 d D . . H53F H 0.291(4) 0.211(3) 0.4933(15) 0.055 Uiso 1 1 d D . . H53G H 0.361(4) 0.144(3) 0.4644(15) 0.055 Uiso 1 1 d D . . H66E H 0.599(3) 0.334(4) 0.4472(16) 0.055 Uiso 1 1 d D . . H63F H 0.791(4) 0.232(3) 0.4944(16) 0.055 Uiso 1 1 d D . . H63G H 0.866(3) 0.159(4) 0.4701(13) 0.055 Uiso 1 1 d 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 0.0249(7) 0.0183(7) 0.0303(7) 0.0076(6) 0.0117(6) 0.0057(6) Cl2 0.0282(8) 0.0192(7) 0.0334(8) -0.0104(6) 0.0149(6) -0.0100(6) Cl3 0.0184(7) 0.0338(8) 0.0225(7) 0.0022(6) 0.0052(6) 0.0025(6) Cl4 0.0187(7) 0.0336(8) 0.0186(7) -0.0009(6) 0.0041(5) -0.0012(6) Cl5 0.0270(8) 0.0169(7) 0.0352(8) -0.0079(6) 0.0100(6) -0.0038(6) Cl6 0.0310(8) 0.0166(7) 0.0280(7) 0.0043(6) 0.0142(6) 0.0030(6) Cl7 0.0307(8) 0.0233(7) 0.0311(8) 0.0053(6) 0.0147(6) 0.0072(6) Cl8 0.0256(7) 0.0151(6) 0.0233(7) -0.0029(5) 0.0083(6) -0.0016(5) Cl9 0.0304(8) 0.0196(7) 0.0320(8) 0.0071(6) 0.0138(6) 0.0049(6) Cl10 0.0303(8) 0.0216(7) 0.0305(8) 0.0056(6) 0.0137(6) 0.0062(6) Cl11 0.0344(8) 0.0185(7) 0.0349(8) 0.0069(6) 0.0162(7) 0.0074(6) Cl12 0.0188(7) 0.0458(9) 0.0203(7) -0.0007(6) 0.0035(6) 0.0010(6) Cl13 0.0299(8) 0.0211(7) 0.0536(10) 0.0147(7) 0.0155(7) 0.0054(6) Cl14 0.0201(7) 0.0325(8) 0.0214(7) 0.0028(6) 0.0039(6) -0.0006(6) Cl15 0.0399(9) 0.0360(9) 0.0307(8) 0.0053(7) 0.0142(7) 0.0060(7) Cl16 0.0304(8) 0.0374(9) 0.0313(8) -0.0051(7) 0.0052(7) -0.0043(7) Cl17 0.0233(7) 0.0282(8) 0.0230(7) 0.0068(6) 0.0004(6) 0.0018(6) Cl18 0.0208(7) 0.0259(7) 0.0252(7) -0.0063(6) 0.0037(6) -0.0030(6) Cl19 0.0480(10) 0.0260(8) 0.0303(8) -0.0140(6) 0.0164(7) -0.0159(7) Cl20 0.0218(8) 0.0615(11) 0.0208(7) 0.0097(7) 0.0048(6) 0.0005(7) Cl21 0.0384(9) 0.0301(8) 0.0221(7) -0.0021(6) 0.0123(6) -0.0025(7) Cl22 0.0457(10) 0.0492(11) 0.0345(9) -0.0075(8) 0.0080(8) -0.0029(8) Cl23 0.0923(17) 0.0414(11) 0.0634(13) 0.0126(10) 0.0311(12) 0.0366(11) Cl25 0.0476(14) 0.0340(12) 0.0341(11) -0.0048(9) -0.0077(9) -0.0072(9) Cl26 0.147(15) 0.040(6) 0.028(5) -0.015(4) 0.003(7) -0.046(7) N10 0.017(2) 0.018(2) 0.030(3) 0.000(2) 0.005(2) 0.0046(19) C11 0.015(3) 0.013(3) 0.027(3) 0.000(2) 0.006(2) 0.004(2) C12A 0.021(3) 0.018(3) 0.017(3) -0.001(2) 0.003(2) -0.007(2) N13A 0.016(2) 0.015(2) 0.020(2) 0.0006(19) 0.0053(19) -0.0012(18) C14A 0.018(3) 0.018(3) 0.018(3) -0.004(2) 0.002(2) -0.005(2) C15A 0.016(3) 0.021(3) 0.021(3) -0.002(2) 0.003(2) -0.004(2) N16A 0.020(3) 0.014(2) 0.018(2) 0.0029(19) 0.0046(19) -0.0025(19) C17A 0.017(3) 0.018(3) 0.024(3) 0.003(2) 0.001(2) -0.001(2) C12B 0.017(3) 0.021(3) 0.019(3) -0.001(2) -0.001(2) 0.003(2) N13B 0.016(2) 0.028(3) 0.018(2) 0.003(2) 0.0009(19) 0.007(2) C14B 0.025(3) 0.038(4) 0.015(3) -0.002(3) 0.000(2) 0.011(3) C15B 0.033(4) 0.040(4) 0.014(3) -0.005(3) 0.000(3) 0.014(3) N16B 0.024(3) 0.031(3) 0.018(2) 0.004(2) 0.004(2) 0.011(2) C17B 0.023(3) 0.025(3) 0.022(3) 0.002(2) 0.001(2) 0.011(2) C12C 0.013(3) 0.020(3) 0.021(3) -0.004(2) -0.002(2) -0.003(2) N13C 0.017(2) 0.015(2) 0.026(3) 0.002(2) 0.000(2) -0.0038(19) C14C 0.021(3) 0.022(3) 0.032(3) 0.005(3) 0.004(3) -0.003(2) C15C 0.019(3) 0.023(3) 0.045(4) 0.012(3) -0.003(3) -0.004(2) N16C 0.017(2) 0.016(2) 0.028(3) 0.004(2) -0.004(2) 0.0008(19) C17C 0.024(3) 0.014(3) 0.018(3) -0.002(2) -0.002(2) -0.001(2) C18 0.018(3) 0.014(3) 0.027(3) 0.002(2) 0.002(2) 0.003(2) C19 0.024(3) 0.021(3) 0.028(3) 0.002(3) 0.000(3) 0.004(2) N20 0.020(2) 0.016(2) 0.024(3) 0.0051(19) 0.007(2) 0.0039(19) C21 0.019(3) 0.011(3) 0.023(3) 0.003(2) 0.005(2) 0.004(2) C22A 0.021(3) 0.017(3) 0.023(3) 0.001(2) 0.008(2) -0.003(2) N23A 0.020(2) 0.016(2) 0.021(2) 0.0034(19) 0.004(2) -0.0012(19) C24A 0.025(3) 0.018(3) 0.026(3) -0.003(2) 0.003(3) -0.005(2) C25A 0.022(3) 0.022(3) 0.019(3) -0.001(2) 0.003(2) -0.003(2) N26A 0.023(3) 0.014(2) 0.023(3) 0.0017(19) 0.005(2) -0.0007(19) C27A 0.017(3) 0.023(3) 0.027(3) 0.002(2) 0.002(2) 0.000(2) C22B 0.018(3) 0.020(3) 0.019(3) 0.003(2) 0.002(2) 0.001(2) N23B 0.018(2) 0.021(3) 0.020(2) 0.004(2) 0.0019(19) 0.003(2) C24B 0.022(3) 0.025(3) 0.016(3) 0.000(2) 0.002(2) 0.003(2) C25B 0.026(3) 0.022(3) 0.031(3) 0.000(3) 0.011(3) 0.002(2) N26B 0.018(2) 0.019(2) 0.022(2) 0.004(2) 0.010(2) 0.0026(19) C27B 0.019(3) 0.024(3) 0.026(3) 0.003(2) 0.004(2) 0.007(2) C22C 0.015(3) 0.015(3) 0.023(3) 0.001(2) 0.003(2) -0.002(2) N23C 0.019(2) 0.014(2) 0.019(2) -0.0001(19) 0.0037(19) -0.0013(19) C24C 0.017(3) 0.024(3) 0.023(3) 0.006(2) 0.006(2) 0.001(2) C25C 0.018(3) 0.026(3) 0.024(3) 0.010(2) 0.006(2) 0.002(2) N26C 0.020(2) 0.018(2) 0.023(3) 0.004(2) 0.005(2) 0.0023(19) C27C 0.021(3) 0.020(3) 0.021(3) 0.004(2) 0.008(2) 0.003(2) C28 0.018(3) 0.018(3) 0.023(3) 0.003(2) 0.003(2) 0.005(2) C29 0.019(3) 0.031(3) 0.025(3) 0.004(3) 0.005(2) 0.004(3) N30 0.017(2) 0.017(2) 0.019(2) -0.0005(19) 0.0044(19) 0.0015(19) C31 0.016(3) 0.016(3) 0.019(3) 0.000(2) 0.003(2) 0.003(2) C32A 0.018(3) 0.018(3) 0.015(3) 0.001(2) 0.003(2) -0.001(2) N33A 0.018(2) 0.015(2) 0.016(2) -0.0030(18) 0.0051(19) -0.0021(18) C34A 0.025(3) 0.018(3) 0.021(3) -0.005(2) 0.006(2) -0.009(2) C35A 0.016(3) 0.029(3) 0.023(3) 0.000(3) -0.002(2) -0.005(2) N36A 0.020(3) 0.020(3) 0.027(3) 0.001(2) 0.002(2) -0.003(2) C37A 0.019(3) 0.027(3) 0.030(3) 0.004(3) -0.005(3) 0.003(2) C32B 0.018(3) 0.022(3) 0.016(3) -0.001(2) 0.003(2) 0.001(2) N33B 0.021(3) 0.020(2) 0.020(2) -0.004(2) 0.006(2) 0.003(2) C34B 0.029(3) 0.029(3) 0.015(3) -0.004(2) 0.004(2) 0.002(3) C35B 0.022(3) 0.025(3) 0.026(3) -0.006(3) 0.010(3) 0.005(2) N36B 0.021(3) 0.027(3) 0.016(2) 0.003(2) 0.0071(19) 0.006(2) C37B 0.025(3) 0.031(3) 0.034(4) 0.005(3) 0.010(3) 0.011(3) C32C 0.014(3) 0.015(3) 0.033(3) 0.000(2) 0.003(2) -0.002(2) N33C 0.018(2) 0.016(2) 0.023(3) 0.001(2) 0.001(2) 0.0003(19) C34C 0.023(3) 0.025(3) 0.025(3) 0.008(3) 0.010(3) 0.002(2) C35C 0.020(3) 0.023(3) 0.035(3) 0.014(3) 0.006(3) -0.001(2) N36C 0.025(3) 0.027(3) 0.038(3) 0.010(2) 0.010(2) 0.005(2) C37C 0.021(3) 0.024(3) 0.030(3) 0.010(3) 0.005(3) 0.001(2) C38 0.017(3) 0.021(3) 0.023(3) 0.000(2) 0.006(2) 0.000(2) C39 0.022(3) 0.026(3) 0.029(3) 0.006(3) 0.004(3) 0.007(3) N40 0.031(3) 0.041(3) 0.035(3) 0.018(3) 0.016(2) 0.019(3) C41 0.022(3) 0.019(3) 0.021(3) 0.008(2) 0.001(2) 0.009(2) C42A 0.035(3) 0.015(3) 0.022(3) 0.000(2) 0.008(3) -0.002(2) N43A 0.026(3) 0.018(2) 0.025(3) 0.003(2) 0.002(2) 0.002(2) C44A 0.039(4) 0.022(3) 0.030(3) -0.009(3) -0.003(3) 0.001(3) C45A 0.031(3) 0.026(3) 0.024(3) 0.000(3) 0.000(3) 0.000(3) N46A 0.026(3) 0.016(2) 0.026(3) 0.002(2) 0.003(2) -0.004(2) C47A 0.020(3) 0.021(3) 0.021(3) 0.002(2) -0.002(2) 0.000(2) C42B 0.021(3) 0.025(3) 0.020(3) 0.006(2) 0.002(2) 0.008(2) N43B 0.019(2) 0.021(3) 0.019(2) 0.009(2) 0.0039(19) 0.004(2) C44B 0.025(3) 0.029(3) 0.021(3) 0.009(3) 0.008(2) 0.002(3) C45B 0.021(3) 0.030(3) 0.019(3) 0.005(2) 0.003(2) 0.003(2) N46B 0.018(2) 0.020(2) 0.030(3) 0.005(2) 0.008(2) 0.000(2) C47B 0.019(3) 0.025(3) 0.026(3) 0.005(3) 0.005(2) 0.005(2) C42C 0.013(3) 0.030(3) 0.018(3) 0.002(2) 0.000(2) -0.003(2) N43C 0.017(2) 0.013(2) 0.022(2) 0.0023(19) 0.0012(19) -0.0033(19) C44C 0.023(3) 0.024(3) 0.021(3) 0.002(2) 0.009(2) 0.002(2) C45C 0.021(3) 0.020(3) 0.031(3) 0.010(3) 0.008(3) -0.002(2) N46C 0.021(2) 0.018(2) 0.022(2) 0.002(2) 0.004(2) 0.001(2) C47C 0.017(3) 0.015(3) 0.017(3) 0.001(2) 0.001(2) 0.001(2) C48 0.019(3) 0.019(3) 0.022(3) 0.003(2) 0.002(2) 0.004(2) C49 0.022(3) 0.029(3) 0.037(4) 0.006(3) 0.009(3) 0.011(3) N50 0.019(2) 0.014(2) 0.022(2) -0.0016(19) 0.0055(19) -0.0022(19) C51 0.012(3) 0.015(3) 0.021(3) -0.002(2) 0.002(2) -0.002(2) C52A 0.019(3) 0.017(3) 0.019(3) -0.005(2) 0.005(2) 0.003(2) N53A 0.018(2) 0.016(2) 0.018(2) -0.0011(19) 0.0044(19) 0.0001(19) C54A 0.021(3) 0.018(3) 0.025(3) 0.003(2) 0.004(2) 0.006(2) C55A 0.024(3) 0.025(3) 0.017(3) 0.002(2) 0.001(2) 0.003(2) N56A 0.021(3) 0.022(3) 0.017(2) -0.004(2) 0.003(2) -0.003(2) C57A 0.017(3) 0.032(3) 0.023(3) -0.006(3) 0.003(2) -0.003(2) C52B 0.016(3) 0.022(3) 0.014(3) 0.001(2) -0.001(2) -0.001(2) N53B 0.016(2) 0.020(2) 0.021(2) -0.003(2) 0.0048(19) -0.0007(19) C54B 0.024(3) 0.026(3) 0.016(3) -0.001(2) 0.005(2) -0.002(2) C55B 0.022(3) 0.026(3) 0.028(3) 0.009(3) 0.011(3) -0.003(2) N56B 0.020(2) 0.022(2) 0.022(2) -0.004(2) 0.009(2) -0.005(2) C57B 0.018(3) 0.027(3) 0.023(3) -0.008(2) 0.006(2) -0.008(2) C52C 0.018(3) 0.015(3) 0.021(3) 0.001(2) 0.006(2) -0.002(2) N53C 0.020(2) 0.018(2) 0.017(2) 0.0000(19) 0.0049(19) 0.0003(19) C54C 0.014(3) 0.027(3) 0.020(3) -0.004(2) 0.007(2) -0.002(2) C55C 0.020(3) 0.026(3) 0.032(3) -0.013(3) 0.011(3) -0.002(2) N56C 0.018(2) 0.029(3) 0.017(2) -0.008(2) 0.0038(19) -0.006(2) C57C 0.023(3) 0.024(3) 0.016(3) -0.004(2) 0.004(2) -0.006(2) C58 0.016(3) 0.024(3) 0.018(3) -0.006(2) 0.005(2) -0.006(2) C59 0.021(3) 0.035(4) 0.025(3) -0.014(3) 0.006(3) -0.010(3) N60 0.021(3) 0.018(2) 0.026(3) -0.002(2) 0.006(2) -0.001(2) C61 0.017(3) 0.017(3) 0.025(3) -0.007(2) 0.005(2) -0.006(2) C62A 0.016(3) 0.012(3) 0.023(3) -0.001(2) 0.004(2) 0.005(2) N63A 0.020(2) 0.014(2) 0.021(2) -0.0010(19) 0.008(2) 0.0000(19) C64A 0.022(3) 0.015(3) 0.025(3) 0.002(2) 0.004(2) 0.005(2) C65A 0.018(3) 0.024(3) 0.019(3) 0.004(2) -0.001(2) 0.004(2) N66A 0.019(3) 0.014(2) 0.020(2) -0.0007(19) 0.0024(19) 0.0014(19) C67A 0.019(3) 0.018(3) 0.020(3) -0.001(2) 0.001(2) 0.000(2) C62B 0.017(3) 0.016(3) 0.030(3) -0.005(2) -0.003(2) -0.003(2) N63B 0.020(3) 0.019(2) 0.022(2) -0.002(2) 0.003(2) -0.003(2) C64B 0.021(3) 0.026(3) 0.018(3) -0.002(2) -0.002(2) -0.001(2) C65B 0.022(3) 0.022(3) 0.019(3) 0.002(2) 0.001(2) 0.000(2) N66B 0.016(2) 0.020(2) 0.016(2) -0.0032(19) 0.0052(18) -0.0028(19) C67B 0.019(3) 0.017(3) 0.024(3) 0.000(2) 0.003(2) -0.004(2) C62C 0.018(3) 0.016(3) 0.035(3) -0.003(2) 0.003(2) -0.001(2) N63C 0.022(3) 0.014(2) 0.023(3) -0.0004(19) -0.001(2) 0.0014(19) C64C 0.020(3) 0.027(3) 0.028(3) -0.011(3) 0.009(3) -0.003(2) C65C 0.016(3) 0.018(3) 0.043(4) -0.013(3) 0.004(3) 0.002(2) N66C 0.018(2) 0.013(2) 0.024(2) -0.0060(19) 0.004(2) -0.0026(18) C67C 0.017(3) 0.015(3) 0.018(3) -0.003(2) -0.001(2) 0.000(2) C68 0.020(3) 0.015(3) 0.020(3) -0.002(2) 0.001(2) -0.002(2) C69 0.020(3) 0.025(3) 0.028(3) -0.009(3) 0.003(2) -0.010(2) O1 0.044(3) 0.054(3) 0.061(3) -0.010(3) 0.002(3) -0.009(3) O2 0.022(2) 0.028(2) 0.029(2) -0.0049(18) 0.0028(18) -0.0002(17) O3 0.072(4) 0.029(2) 0.026(2) 0.003(2) 0.008(2) 0.003(2) O4 0.073(5) 0.079(5) 0.107(6) 0.011(4) 0.025(4) -0.006(4) O5 0.038(3) 0.100(4) 0.026(3) -0.015(3) 0.010(2) -0.003(3) O6 0.077(4) 0.049(3) 0.087(5) -0.023(3) 0.027(4) -0.021(3) O7 0.062(4) 0.056(3) 0.055(3) -0.002(3) -0.003(3) -0.014(3) O8 0.067(4) 0.077(4) 0.078(4) 0.017(4) -0.001(3) 0.002(3) O9 0.070(4) 0.081(5) 0.092(5) 0.031(4) 0.027(4) 0.030(4) O10 0.075(13) 0.051(11) 0.040(10) 0.012(7) 0.030(8) 0.033(9) O10' 0.054(9) 0.036(8) 0.037(9) -0.002(6) 0.002(7) 0.015(6) O11 0.049(7) 0.017(6) 0.031(6) -0.017(5) 0.016(6) -0.019(5) O11' 0.031(6) 0.035(7) 0.041(7) -0.014(5) 0.004(6) -0.014(5) O12 0.032(3) 0.023(3) 0.042(4) -0.001(3) 0.015(3) 0.002(3) O12' 0.032(3) 0.023(3) 0.042(4) -0.001(3) 0.015(3) 0.002(3) O13 0.046(4) 0.068(5) 0.052(4) -0.029(3) 0.005(3) -0.029(4) O14 0.078(5) 0.056(4) 0.044(4) -0.001(3) 0.012(4) -0.028(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl25 Cl26 1.556(16) . ? Cl26 O14 1.528(17) 3_666 ? N10 C11 1.514(6) . ? N10 H10A 0.91 . ? N10 H10B 0.91 . ? N10 H10C 0.91 . ? C11 C12A 1.524(7) . ? C11 C12B 1.551(7) . ? C11 C12C 1.554(7) . ? C12A N13A 1.478(7) . ? C12A H12A 0.99 . ? C12A H12B 0.99 . ? N13A C14A 1.498(7) . ? N13A H13A 0.92 . ? N13A H13B 0.92 . ? C14A C15A 1.514(7) . ? C14A H14A 0.99 . ? C14A H14B 0.99 . ? C15A N16A 1.462(7) . ? C15A H15A 0.99 . ? C15A H15B 0.99 . ? N16A C17A 1.483(7) . ? N16A H16E 0.83(4) . ? C17A C18 1.534(7) . ? C17A H17A 0.99 . ? C17A H17B 0.99 . ? C12B N13B 1.459(7) . ? C12B H12C 0.99 . ? C12B H12D 0.99 . ? N13B C14B 1.459(7) . ? N13B H13F 0.84(4) . ? C14B C15B 1.519(8) . ? C14B H14C 0.99 . ? C14B H14D 0.99 . ? C15B N16B 1.490(7) . ? C15B H15C 0.99 . ? C15B H15D 0.99 . ? N16B C17B 1.520(7) . ? N16B H16A 0.92 . ? N16B H16B 0.92 . ? C17B C18 1.540(8) . ? C17B H17C 0.99 . ? C17B H17D 0.99 . ? C12C N13C 1.463(7) . ? C12C H12E 0.99 . ? C12C H12F 0.99 . ? N13C C14C 1.471(7) . ? N13C H13G 0.81(4) . ? C14C C15C 1.521(8) . ? C14C H14E 0.99 . ? C14C H14F 0.99 . ? C15C N16C 1.511(7) . ? C15C H15E 0.99 . ? C15C H15F 0.99 . ? N16C C17C 1.502(7) . ? N16C H16C 0.92 . ? N16C H16D 0.92 . ? C17C C18 1.532(8) . ? C17C H17E 0.99 . ? C17C H17F 0.99 . ? C18 C19 1.536(7) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? N20 C21 1.515(6) . ? N20 H20A 0.91 . ? N20 H20B 0.91 . ? N20 H20C 0.91 . ? C21 C22A 1.524(8) . ? C21 C22C 1.538(7) . ? C21 C22B 1.541(7) . ? C22A N23A 1.481(7) . ? C22A H22A 0.99 . ? C22A H22B 0.99 . ? N23A C24A 1.496(7) . ? N23A H23A 0.92 . ? N23A H23B 0.92 . ? C24A C25A 1.512(8) . ? C24A H24A 0.99 . ? C24A H24B 0.99 . ? C25A N26A 1.474(7) . ? C25A H25A 0.99 . ? C25A H25B 0.99 . ? N26A C27A 1.477(7) . ? N26A H26E 0.83(4) . ? C27A C28 1.538(8) . ? C27A H27A 0.99 . ? C27A H27B 0.99 . ? C22B N23B 1.468(7) . ? C22B H22C 0.99 . ? C22B H22D 0.99 . ? N23B C24B 1.466(7) . ? N23B H23F 0.84(4) . ? C24B C25B 1.517(8) . ? C24B H24C 0.99 . ? C24B H24D 0.99 . ? C25B N26B 1.494(7) . ? C25B H25C 0.99 . ? C25B H25D 0.99 . ? N26B C27B 1.515(7) . ? N26B H26A 0.92 . ? N26B H26B 0.92 . ? C27B C28 1.534(7) . ? C27B H27C 0.99 . ? C27B H27D 0.99 . ? C22C N23C 1.463(7) . ? C22C H22E 0.99 . ? C22C H22F 0.99 . ? N23C C24C 1.459(7) . ? N23C H23G 0.82(4) . ? C24C C25C 1.518(7) . ? C24C H24E 0.99 . ? C24C H24F 0.99 . ? C25C N26C 1.506(7) . ? C25C H25E 0.99 . ? C25C H25F 0.99 . ? N26C C27C 1.487(7) . ? N26C H26C 0.92 . ? N26C H26D 0.92 . ? C27C C28 1.534(8) . ? C27C H27E 0.99 . ? C27C H27F 0.99 . ? C28 C29 1.545(7) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? N30 C31 1.512(6) . ? N30 H30A 0.91 . ? N30 H30B 0.91 . ? N30 H30C 0.91 . ? C31 C32A 1.536(7) . ? C31 C32C 1.541(7) . ? C31 C32B 1.544(7) . ? C32A N33A 1.479(6) . ? C32A H32A 0.99 . ? C32A H32B 0.99 . ? N33A C34A 1.504(7) . ? N33A H33A 0.92 . ? N33A H33B 0.92 . ? C34A C35A 1.515(8) . ? C34A H34A 0.99 . ? C34A H34B 0.99 . ? C35A N36A 1.471(7) . ? C35A H35A 0.99 . ? C35A H35B 0.99 . ? N36A C37A 1.484(7) . ? N36A H36E 0.83(4) . ? C37A C38 1.545(8) . ? C37A H37A 0.99 . ? C37A H37B 0.99 . ? C32B N33B 1.458(7) . ? C32B H32C 0.99 . ? C32B H32D 0.99 . ? N33B C34B 1.469(7) . ? N33B H33F 0.84(4) . ? C34B C35B 1.512(8) . ? C34B H34C 0.99 . ? C34B H34D 0.99 . ? C35B N36B 1.497(7) . ? C35B H35C 0.99 . ? C35B H35D 0.99 . ? N36B C37B 1.510(7) . ? N36B H36A 0.92 . ? N36B H36B 0.92 . ? C37B C38 1.533(8) . ? C37B H37C 0.99 . ? C37B H37D 0.99 . ? C32C N33C 1.456(7) . ? C32C H32E 0.99 . ? C32C H32F 0.99 . ? N33C C34C 1.464(7) . ? N33C H33G 0.82(4) . ? C34C C35C 1.527(8) . ? C34C H34E 0.99 . ? C34C H34F 0.99 . ? C35C N36C 1.513(7) . ? C35C H35E 0.99 . ? C35C H35F 0.99 . ? N36C C37C 1.478(7) . ? N36C H36C 0.92 . ? N36C H36D 0.92 . ? C37C C38 1.526(8) . ? C37C H37E 0.99 . ? C37C H37F 0.99 . ? C38 C39 1.536(7) . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? N40 C41 1.508(7) . ? N40 H40A 0.91 . ? N40 H40B 0.91 . ? N40 H40C 0.91 . ? C41 C42B 1.523(8) . ? C41 C42A 1.532(8) . ? C41 C42C 1.544(8) . ? C42A N43A 1.478(7) . ? C42A H42A 0.99 . ? C42A H42B 0.99 . ? N43A C44A 1.499(7) . ? N43A H43A 0.92 . ? N43A H43B 0.92 . ? C44A C45A 1.512(8) . ? C44A H44A 0.99 . ? C44A H44B 0.99 . ? C45A N46A 1.460(8) . ? C45A H45A 0.99 . ? C45A H45B 0.99 . ? N46A C47A 1.476(7) . ? N46A H46E 0.85(4) . ? C47A C48 1.549(8) . ? C47A H47A 0.99 . ? C47A H47B 0.99 . ? C42B N43B 1.463(7) . ? C42B H42C 0.99 . ? C42B H42D 0.99 . ? N43B C44B 1.461(7) . ? N43B H43F 0.84(4) . ? C44B C45B 1.508(8) . ? C44B H44C 0.99 . ? C44B H44D 0.99 . ? C45B N46B 1.499(7) . ? C45B H45C 0.99 . ? C45B H45D 0.99 . ? N46B C47B 1.510(7) . ? N46B H46A 0.92 . ? N46B H46B 0.92 . ? C47B C48 1.538(8) . ? C47B H47C 0.99 . ? C47B H47D 0.99 . ? C42C N43C 1.465(7) . ? C42C H42E 0.99 . ? C42C H42F 0.99 . ? N43C C44C 1.461(7) . ? N43C H43G 0.83(4) . ? C44C C45C 1.524(8) . ? C44C H44E 0.99 . ? C44C H44F 0.99 . ? C45C N46C 1.503(7) . ? C45C H45E 0.99 . ? C45C H45F 0.99 . ? N46C C47C 1.498(7) . ? N46C H46C 0.92 . ? N46C H46D 0.92 . ? C47C C48 1.536(7) . ? C47C H47E 0.99 . ? C47C H47F 0.99 . ? C48 C49 1.531(7) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? N50 C51 1.508(6) . ? N50 H50A 0.91 . ? N50 H50B 0.91 . ? N50 H50C 0.91 . ? C51 C52A 1.527(7) . ? C51 C52C 1.542(7) . ? C51 C52B 1.544(7) . ? C52A N53A 1.481(6) . ? C52A H52A 0.99 . ? C52A H52B 0.99 . ? N53A C54A 1.495(7) . ? N53A H53A 0.92 . ? N53A H53B 0.92 . ? C54A C55A 1.520(8) . ? C54A H54A 0.99 . ? C54A H54B 0.99 . ? C55A N56A 1.459(7) . ? C55A H55A 0.99 . ? C55A H55B 0.99 . ? N56A C57A 1.476(7) . ? N56A H56E 0.82(4) . ? C57A C58 1.538(8) . ? C57A H57A 0.99 . ? C57A H57B 0.99 . ? C52B N53B 1.467(7) . ? C52B H52C 0.99 . ? C52B H52D 0.99 . ? N53B C54B 1.457(7) . ? N53B H53F 0.85(4) . ? C54B C55B 1.509(8) . ? C54B H54C 0.99 . ? C54B H54D 0.99 . ? C55B N56B 1.505(7) . ? C55B H55C 0.99 . ? C55B H55D 0.99 . ? N56B C57B 1.515(7) . ? N56B H56A 0.92 . ? N56B H56B 0.92 . ? C57B C58 1.547(7) . ? C57B H57C 0.99 . ? C57B H57D 0.99 . ? C52C N53C 1.469(7) . ? C52C H52E 0.99 . ? C52C H52F 0.99 . ? N53C C54C 1.449(7) . ? N53C H53G 0.83(4) . ? C54C C55C 1.519(7) . ? C54C H54E 0.99 . ? C54C H54F 0.99 . ? C55C N56C 1.503(7) . ? C55C H55E 0.99 . ? C55C H55F 0.99 . ? N56C C57C 1.496(6) . ? N56C H56C 0.92 . ? N56C H56D 0.92 . ? C57C C58 1.534(8) . ? C57C H57E 0.99 . ? C57C H57F 0.99 . ? C58 C59 1.541(7) . ? C59 H59A 0.98 . ? C59 H59B 0.98 . ? C59 H59C 0.98 . ? N60 C61 1.501(7) . ? N60 H60A 0.91 . ? N60 H60B 0.91 . ? N60 H60C 0.91 . ? C61 C62A 1.529(7) . ? C61 C62B 1.539(8) . ? C61 C62C 1.553(7) . ? C62A N63A 1.484(6) . ? C62A H62A 0.99 . ? C62A H62B 0.99 . ? N63A C64A 1.509(7) . ? N63A H63A 0.92 . ? N63A H63B 0.92 . ? C64A C65A 1.505(8) . ? C64A H64A 0.99 . ? C64A H64B 0.99 . ? C65A N66A 1.468(7) . ? C65A H65A 0.99 . ? C65A H65B 0.99 . ? N66A C67A 1.472(7) . ? N66A H66E 0.81(4) . ? C67A C68 1.548(7) . ? C67A H67A 0.99 . ? C67A H67B 0.99 . ? C62B N63B 1.465(7) . ? C62B H62C 0.99 . ? C62B H62D 0.99 . ? N63B C64B 1.457(7) . ? N63B H63F 0.83(4) . ? C64B C65B 1.504(8) . ? C64B H64C 0.99 . ? C64B H64D 0.99 . ? C65B N66B 1.496(7) . ? C65B H65C 0.99 . ? C65B H65D 0.99 . ? N66B C67B 1.513(7) . ? N66B H66A 0.92 . ? N66B H66B 0.92 . ? C67B C68 1.540(7) . ? C67B H67C 0.99 . ? C67B H67D 0.99 . ? C62C N63C 1.463(7) . ? C62C H62E 0.99 . ? C62C H62F 0.99 . ? N63C C64C 1.459(7) . ? N63C H63G 0.81(4) . ? C64C C65C 1.518(8) . ? C64C H64E 0.99 . ? C64C H64F 0.99 . ? C65C N66C 1.520(7) . ? C65C H65E 0.99 . ? C65C H65F 0.99 . ? N66C C67C 1.502(7) . ? N66C H66C 0.92 . ? N66C H66D 0.92 . ? C67C C68 1.542(7) . ? C67C H67E 0.99 . ? C67C H67F 0.99 . ? C68 C69 1.532(7) . ? C69 H69A 0.98 . ? C69 H69B 0.98 . ? C69 H69C 0.98 . ? 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 O14 Cl26 Cl25 168.8(8) 3_666 . ? C11 N10 H10A 109.5 . . ? C11 N10 H10B 109.5 . . ? H10A N10 H10B 109.5 . . ? C11 N10 H10C 109.5 . . ? H10A N10 H10C 109.5 . . ? H10B N10 H10C 109.5 . . ? N10 C11 C12A 111.0(4) . . ? N10 C11 C12B 106.8(4) . . ? C12A C11 C12B 112.8(4) . . ? N10 C11 C12C 104.7(4) . . ? C12A C11 C12C 108.6(4) . . ? C12B C11 C12C 112.8(4) . . ? N13A C12A C11 114.4(4) . . ? N13A C12A H12A 108.7 . . ? C11 C12A H12A 108.7 . . ? N13A C12A H12B 108.7 . . ? C11 C12A H12B 108.7 . . ? H12A C12A H12B 107.6 . . ? C12A N13A C14A 113.6(4) . . ? C12A N13A H13A 108.8 . . ? C14A N13A H13A 108.8 . . ? C12A N13A H13B 108.8 . . ? C14A N13A H13B 108.8 . . ? H13A N13A H13B 107.7 . . ? N13A C14A C15A 112.3(4) . . ? N13A C14A H14A 109.1 . . ? C15A C14A H14A 109.1 . . ? N13A C14A H14B 109.1 . . ? C15A C14A H14B 109.1 . . ? H14A C14A H14B 107.9 . . ? N16A C15A C14A 109.8(4) . . ? N16A C15A H15A 109.7 . . ? C14A C15A H15A 109.7 . . ? N16A C15A H15B 109.7 . . ? C14A C15A H15B 109.7 . . ? H15A C15A H15B 108.2 . . ? C15A N16A C17A 112.8(4) . . ? C15A N16A H16E 104(5) . . ? C17A N16A H16E 107(5) . . ? N16A C17A C18 113.4(4) . . ? N16A C17A H17A 108.9 . . ? C18 C17A H17A 108.9 . . ? N16A C17A H17B 108.9 . . ? C18 C17A H17B 108.9 . . ? H17A C17A H17B 107.7 . . ? N13B C12B C11 108.7(4) . . ? N13B C12B H12C 110 . . ? C11 C12B H12C 110 . . ? N13B C12B H12D 110 . . ? C11 C12B H12D 110 . . ? H12C C12B H12D 108.3 . . ? C12B N13B C14B 115.2(4) . . ? C12B N13B H13F 110(5) . . ? C14B N13B H13F 114(5) . . ? N13B C14B C15B 107.3(4) . . ? N13B C14B H14C 110.3 . . ? C15B C14B H14C 110.3 . . ? N13B C14B H14D 110.3 . . ? C15B C14B H14D 110.3 . . ? H14C C14B H14D 108.5 . . ? N16B C15B C14B 110.5(5) . . ? N16B C15B H15C 109.6 . . ? C14B C15B H15C 109.6 . . ? N16B C15B H15D 109.6 . . ? C14B C15B H15D 109.6 . . ? H15C C15B H15D 108.1 . . ? C15B N16B C17B 115.4(5) . . ? C15B N16B H16A 108.4 . . ? C17B N16B H16A 108.4 . . ? C15B N16B H16B 108.4 . . ? C17B N16B H16B 108.4 . . ? H16A N16B H16B 107.5 . . ? N16B C17B C18 114.1(4) . . ? N16B C17B H17C 108.7 . . ? C18 C17B H17C 108.7 . . ? N16B C17B H17D 108.7 . . ? C18 C17B H17D 108.7 . . ? H17C C17B H17D 107.6 . . ? N13C C12C C11 112.0(4) . . ? N13C C12C H12E 109.2 . . ? C11 C12C H12E 109.2 . . ? N13C C12C H12F 109.2 . . ? C11 C12C H12F 109.2 . . ? H12E C12C H12F 107.9 . . ? C12C N13C C14C 114.3(4) . . ? C12C N13C H13G 107(6) . . ? C14C N13C H13G 104(6) . . ? N13C C14C C15C 112.2(5) . . ? N13C C14C H14E 109.2 . . ? C15C C14C H14E 109.2 . . ? N13C C14C H14F 109.2 . . ? C15C C14C H14F 109.2 . . ? H14E C14C H14F 107.9 . . ? N16C C15C C14C 114.4(5) . . ? N16C C15C H15E 108.6 . . ? C14C C15C H15E 108.6 . . ? N16C C15C H15F 108.6 . . ? C14C C15C H15F 108.6 . . ? H15E C15C H15F 107.6 . . ? C17C N16C C15C 115.7(4) . . ? C17C N16C H16C 108.4 . . ? C15C N16C H16C 108.4 . . ? C17C N16C H16D 108.4 . . ? C15C N16C H16D 108.4 . . ? H16C N16C H16D 107.4 . . ? N16C C17C C18 114.1(4) . . ? N16C C17C H17E 108.7 . . ? C18 C17C H17E 108.7 . . ? N16C C17C H17F 108.7 . . ? C18 C17C H17F 108.7 . . ? H17E C17C H17F 107.6 . . ? C17C C18 C17A 112.2(4) . . ? C17C C18 C19 111.3(4) . . ? C17A C18 C19 107.0(4) . . ? C17C C18 C17B 109.5(4) . . ? C17A C18 C17B 111.1(5) . . ? C19 C18 C17B 105.4(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 N20 H20A 109.5 . . ? C21 N20 H20B 109.5 . . ? H20A N20 H20B 109.5 . . ? C21 N20 H20C 109.5 . . ? H20A N20 H20C 109.5 . . ? H20B N20 H20C 109.5 . . ? N20 C21 C22A 110.1(4) . . ? N20 C21 C22C 106.3(4) . . ? C22A C21 C22C 109.2(4) . . ? N20 C21 C22B 105.7(4) . . ? C22A C21 C22B 112.7(4) . . ? C22C C21 C22B 112.6(4) . . ? N23A C22A C21 114.9(4) . . ? N23A C22A H22A 108.6 . . ? C21 C22A H22A 108.6 . . ? N23A C22A H22B 108.6 . . ? C21 C22A H22B 108.6 . . ? H22A C22A H22B 107.5 . . ? C22A N23A C24A 114.6(4) . . ? C22A N23A H23A 108.6 . . ? C24A N23A H23A 108.6 . . ? C22A N23A H23B 108.6 . . ? C24A N23A H23B 108.6 . . ? H23A N23A H23B 107.6 . . ? N23A C24A C25A 112.3(4) . . ? N23A C24A H24A 109.1 . . ? C25A C24A H24A 109.1 . . ? N23A C24A H24B 109.1 . . ? C25A C24A H24B 109.1 . . ? H24A C24A H24B 107.9 . . ? N26A C25A C24A 111.0(5) . . ? N26A C25A H25A 109.4 . . ? C24A C25A H25A 109.4 . . ? N26A C25A H25B 109.4 . . ? C24A C25A H25B 109.4 . . ? H25A C25A H25B 108 . . ? C25A N26A C27A 112.4(4) . . ? C25A N26A H26E 103(5) . . ? C27A N26A H26E 116(5) . . ? N26A C27A C28 113.8(4) . . ? N26A C27A H27A 108.8 . . ? C28 C27A H27A 108.8 . . ? N26A C27A H27B 108.8 . . ? C28 C27A H27B 108.8 . . ? H27A C27A H27B 107.7 . . ? N23B C22B C21 110.8(4) . . ? N23B C22B H22C 109.5 . . ? C21 C22B H22C 109.5 . . ? N23B C22B H22D 109.5 . . ? C21 C22B H22D 109.5 . . ? H22C C22B H22D 108.1 . . ? C24B N23B C22B 114.2(4) . . ? C24B N23B H23F 107(5) . . ? C22B N23B H23F 109(5) . . ? N23B C24B C25B 107.2(4) . . ? N23B C24B H24C 110.3 . . ? C25B C24B H24C 110.3 . . ? N23B C24B H24D 110.3 . . ? C25B C24B H24D 110.3 . . ? H24C C24B H24D 108.5 . . ? N26B C25B C24B 111.0(5) . . ? N26B C25B H25C 109.4 . . ? C24B C25B H25C 109.4 . . ? N26B C25B H25D 109.4 . . ? C24B C25B H25D 109.4 . . ? H25C C25B H25D 108 . . ? C25B N26B C27B 115.3(4) . . ? C25B N26B H26A 108.5 . . ? C27B N26B H26A 108.5 . . ? C25B N26B H26B 108.5 . . ? C27B N26B H26B 108.5 . . ? H26A N26B H26B 107.5 . . ? N26B C27B C28 114.3(4) . . ? N26B C27B H27C 108.7 . . ? C28 C27B H27C 108.7 . . ? N26B C27B H27D 108.7 . . ? C28 C27B H27D 108.7 . . ? H27C C27B H27D 107.6 . . ? N23C C22C C21 112.0(4) . . ? N23C C22C H22E 109.2 . . ? C21 C22C H22E 109.2 . . ? N23C C22C H22F 109.2 . . ? C21 C22C H22F 109.2 . . ? H22E C22C H22F 107.9 . . ? C24C N23C C22C 115.0(4) . . ? C24C N23C H23G 107(5) . . ? C22C N23C H23G 106(5) . . ? N23C C24C C25C 112.3(5) . . ? N23C C24C H24E 109.2 . . ? C25C C24C H24E 109.2 . . ? N23C C24C H24F 109.2 . . ? C25C C24C H24F 109.2 . . ? H24E C24C H24F 107.9 . . ? N26C C25C C24C 115.5(5) . . ? N26C C25C H25E 108.4 . . ? C24C C25C H25E 108.4 . . ? N26C C25C H25F 108.4 . . ? C24C C25C H25F 108.4 . . ? H25E C25C H25F 107.5 . . ? C27C N26C C25C 114.8(4) . . ? C27C N26C H26C 108.6 . . ? C25C N26C H26C 108.6 . . ? C27C N26C H26D 108.6 . . ? C25C N26C H26D 108.6 . . ? H26C N26C H26D 107.6 . . ? N26C C27C C28 114.3(4) . . ? N26C C27C H27E 108.7 . . ? C28 C27C H27E 108.7 . . ? N26C C27C H27F 108.7 . . ? C28 C27C H27F 108.7 . . ? H27E C27C H27F 107.6 . . ? C27C C28 C27B 108.4(4) . . ? C27C C28 C27A 112.5(4) . . ? C27B C28 C27A 110.6(5) . . ? C27C C28 C29 111.3(4) . . ? C27B C28 C29 105.4(4) . . ? C27A C28 C29 108.4(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 N30 H30A 109.5 . . ? C31 N30 H30B 109.5 . . ? H30A N30 H30B 109.5 . . ? C31 N30 H30C 109.5 . . ? H30A N30 H30C 109.5 . . ? H30B N30 H30C 109.5 . . ? N30 C31 C32A 110.3(4) . . ? N30 C31 C32C 106.3(4) . . ? C32A C31 C32C 108.6(4) . . ? N30 C31 C32B 106.0(4) . . ? C32A C31 C32B 113.0(4) . . ? C32C C31 C32B 112.4(4) . . ? N33A C32A C31 114.2(4) . . ? N33A C32A H32A 108.7 . . ? C31 C32A H32A 108.7 . . ? N33A C32A H32B 108.7 . . ? C31 C32A H32B 108.7 . . ? H32A C32A H32B 107.6 . . ? C32A N33A C34A 114.6(4) . . ? C32A N33A H33A 108.6 . . ? C34A N33A H33A 108.6 . . ? C32A N33A H33B 108.6 . . ? C34A N33A H33B 108.6 . . ? H33A N33A H33B 107.6 . . ? N33A C34A C35A 111.8(4) . . ? N33A C34A H34A 109.3 . . ? C35A C34A H34A 109.3 . . ? N33A C34A H34B 109.3 . . ? C35A C34A H34B 109.3 . . ? H34A C34A H34B 107.9 . . ? N36A C35A C34A 110.1(5) . . ? N36A C35A H35A 109.6 . . ? C34A C35A H35A 109.6 . . ? N36A C35A H35B 109.6 . . ? C34A C35A H35B 109.6 . . ? H35A C35A H35B 108.2 . . ? C35A N36A C37A 110.7(5) . . ? C35A N36A H36E 107(5) . . ? C37A N36A H36E 111(5) . . ? N36A C37A C38 113.1(5) . . ? N36A C37A H37A 109 . . ? C38 C37A H37A 109 . . ? N36A C37A H37B 109 . . ? C38 C37A H37B 109 . . ? H37A C37A H37B 107.8 . . ? N33B C32B C31 110.1(4) . . ? N33B C32B H32C 109.6 . . ? C31 C32B H32C 109.6 . . ? N33B C32B H32D 109.6 . . ? C31 C32B H32D 109.6 . . ? H32C C32B H32D 108.2 . . ? C32B N33B C34B 114.1(4) . . ? C32B N33B H33F 113(5) . . ? C34B N33B H33F 107(5) . . ? N33B C34B C35B 107.5(4) . . ? N33B C34B H34C 110.2 . . ? C35B C34B H34C 110.2 . . ? N33B C34B H34D 110.2 . . ? C35B C34B H34D 110.2 . . ? H34C C34B H34D 108.5 . . ? N36B C35B C34B 110.3(4) . . ? N36B C35B H35C 109.6 . . ? C34B C35B H35C 109.6 . . ? N36B C35B H35D 109.6 . . ? C34B C35B H35D 109.6 . . ? H35C C35B H35D 108.1 . . ? C35B N36B C37B 117.6(5) . . ? C35B N36B H36A 107.9 . . ? C37B N36B H36A 107.9 . . ? C35B N36B H36B 107.9 . . ? C37B N36B H36B 107.9 . . ? H36A N36B H36B 107.2 . . ? N36B C37B C38 114.8(5) . . ? N36B C37B H37C 108.6 . . ? C38 C37B H37C 108.6 . . ? N36B C37B H37D 108.6 . . ? C38 C37B H37D 108.6 . . ? H37C C37B H37D 107.5 . . ? N33C C32C C31 112.9(4) . . ? N33C C32C H32E 109 . . ? C31 C32C H32E 109 . . ? N33C C32C H32F 109 . . ? C31 C32C H32F 109 . . ? H32E C32C H32F 107.8 . . ? C32C N33C C34C 116.0(5) . . ? C32C N33C H33G 112(6) . . ? C34C N33C H33G 106(6) . . ? N33C C34C C35C 111.9(5) . . ? N33C C34C H34E 109.2 . . ? C35C C34C H34E 109.2 . . ? N33C C34C H34F 109.2 . . ? C35C C34C H34F 109.2 . . ? H34E C34C H34F 107.9 . . ? N36C C35C C34C 114.3(5) . . ? N36C C35C H35E 108.7 . . ? C34C C35C H35E 108.7 . . ? N36C C35C H35F 108.7 . . ? C34C C35C H35F 108.7 . . ? H35E C35C H35F 107.6 . . ? C37C N36C C35C 116.3(5) . . ? C37C N36C H36C 108.2 . . ? C35C N36C H36C 108.2 . . ? C37C N36C H36D 108.2 . . ? C35C N36C H36D 108.2 . . ? H36C N36C H36D 107.4 . . ? N36C C37C C38 115.5(5) . . ? N36C C37C H37E 108.4 . . ? C38 C37C H37E 108.4 . . ? N36C C37C H37F 108.4 . . ? C38 C37C H37F 108.4 . . ? H37E C37C H37F 107.5 . . ? C37C C38 C37B 110.1(5) . . ? C37C C38 C39 111.2(5) . . ? C37B C38 C39 106.3(4) . . ? C37C C38 C37A 111.4(5) . . ? C37B C38 C37A 110.6(5) . . ? C39 C38 C37A 107.1(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 N40 H40A 109.5 . . ? C41 N40 H40B 109.5 . . ? H40A N40 H40B 109.5 . . ? C41 N40 H40C 109.5 . . ? H40A N40 H40C 109.5 . . ? H40B N40 H40C 109.5 . . ? N40 C41 C42B 104.7(4) . . ? N40 C41 C42A 109.8(5) . . ? C42B C41 C42A 114.4(5) . . ? N40 C41 C42C 107.3(4) . . ? C42B C41 C42C 114.0(5) . . ? C42A C41 C42C 106.4(4) . . ? N43A C42A C41 115.8(5) . . ? N43A C42A H42A 108.3 . . ? C41 C42A H42A 108.3 . . ? N43A C42A H42B 108.3 . . ? C41 C42A H42B 108.3 . . ? H42A C42A H42B 107.4 . . ? C42A N43A C44A 114.8(5) . . ? C42A N43A H43A 108.6 . . ? C44A N43A H43A 108.6 . . ? C42A N43A H43B 108.6 . . ? C44A N43A H43B 108.6 . . ? H43A N43A H43B 107.6 . . ? N43A C44A C45A 112.0(5) . . ? N43A C44A H44A 109.2 . . ? C45A C44A H44A 109.2 . . ? N43A C44A H44B 109.2 . . ? C45A C44A H44B 109.2 . . ? H44A C44A H44B 107.9 . . ? N46A C45A C44A 110.3(5) . . ? N46A C45A H45A 109.6 . . ? C44A C45A H45A 109.6 . . ? N46A C45A H45B 109.6 . . ? C44A C45A H45B 109.6 . . ? H45A C45A H45B 108.1 . . ? C45A N46A C47A 112.5(5) . . ? C45A N46A H46E 112(5) . . ? C47A N46A H46E 114(5) . . ? N46A C47A C48 113.3(4) . . ? N46A C47A H47A 108.9 . . ? C48 C47A H47A 108.9 . . ? N46A C47A H47B 108.9 . . ? C48 C47A H47B 108.9 . . ? H47A C47A H47B 107.7 . . ? N43B C42B C41 111.0(4) . . ? N43B C42B H42C 109.4 . . ? C41 C42B H42C 109.4 . . ? N43B C42B H42D 109.4 . . ? C41 C42B H42D 109.4 . . ? H42C C42B H42D 108 . . ? C44B N43B C42B 113.6(4) . . ? C44B N43B H43F 109(5) . . ? C42B N43B H43F 107(5) . . ? N43B C44B C45B 107.9(4) . . ? N43B C44B H44C 110.1 . . ? C45B C44B H44C 110.1 . . ? N43B C44B H44D 110.1 . . ? C45B C44B H44D 110.1 . . ? H44C C44B H44D 108.4 . . ? N46B C45B C44B 111.0(5) . . ? N46B C45B H45C 109.4 . . ? C44B C45B H45C 109.4 . . ? N46B C45B H45D 109.4 . . ? C44B C45B H45D 109.4 . . ? H45C C45B H45D 108 . . ? C45B N46B C47B 115.4(4) . . ? C45B N46B H46A 108.4 . . ? C47B N46B H46A 108.4 . . ? C45B N46B H46B 108.4 . . ? C47B N46B H46B 108.4 . . ? H46A N46B H46B 107.5 . . ? N46B C47B C48 114.7(4) . . ? N46B C47B H47C 108.6 . . ? C48 C47B H47C 108.6 . . ? N46B C47B H47D 108.6 . . ? C48 C47B H47D 108.6 . . ? H47C C47B H47D 107.6 . . ? N43C C42C C41 110.5(4) . . ? N43C C42C H42E 109.6 . . ? C41 C42C H42E 109.6 . . ? N43C C42C H42F 109.6 . . ? C41 C42C H42F 109.6 . . ? H42E C42C H42F 108.1 . . ? C44C N43C C42C 115.8(4) . . ? C44C N43C H43G 101(5) . . ? C42C N43C H43G 109(5) . . ? N43C C44C C45C 112.1(4) . . ? N43C C44C H44E 109.2 . . ? C45C C44C H44E 109.2 . . ? N43C C44C H44F 109.2 . . ? C45C C44C H44F 109.2 . . ? H44E C44C H44F 107.9 . . ? N46C C45C C44C 115.7(5) . . ? N46C C45C H45E 108.4 . . ? C44C C45C H45E 108.4 . . ? N46C C45C H45F 108.4 . . ? C44C C45C H45F 108.4 . . ? H45E C45C H45F 107.4 . . ? C47C N46C C45C 115.2(4) . . ? C47C N46C H46C 108.5 . . ? C45C N46C H46C 108.5 . . ? C47C N46C H46D 108.5 . . ? C45C N46C H46D 108.5 . . ? H46C N46C H46D 107.5 . . ? N46C C47C C48 114.6(4) . . ? N46C C47C H47E 108.6 . . ? C48 C47C H47E 108.6 . . ? N46C C47C H47F 108.6 . . ? C48 C47C H47F 108.6 . . ? H47E C47C H47F 107.6 . . ? C49 C48 C47C 111.9(5) . . ? C49 C48 C47B 105.9(4) . . ? C47C C48 C47B 109.5(4) . . ? C49 C48 C47A 107.6(5) . . ? C47C C48 C47A 111.0(4) . . ? C47B C48 C47A 110.8(5) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 N50 H50A 109.5 . . ? C51 N50 H50B 109.5 . . ? H50A N50 H50B 109.5 . . ? C51 N50 H50C 109.5 . . ? H50A N50 H50C 109.5 . . ? H50B N50 H50C 109.5 . . ? N50 C51 C52A 110.1(4) . . ? N50 C51 C52C 105.8(4) . . ? C52A C51 C52C 108.3(4) . . ? N50 C51 C52B 106.1(4) . . ? C52A C51 C52B 113.5(4) . . ? C52C C51 C52B 112.8(4) . . ? N53A C52A C51 114.8(4) . . ? N53A C52A H52A 108.6 . . ? C51 C52A H52A 108.6 . . ? N53A C52A H52B 108.6 . . ? C51 C52A H52B 108.6 . . ? H52A C52A H52B 107.5 . . ? C52A N53A C54A 115.1(4) . . ? C52A N53A H53A 108.5 . . ? C54A N53A H53A 108.5 . . ? C52A N53A H53B 108.5 . . ? C54A N53A H53B 108.5 . . ? H53A N53A H53B 107.5 . . ? N53A C54A C55A 112.3(4) . . ? N53A C54A H54A 109.1 . . ? C55A C54A H54A 109.1 . . ? N53A C54A H54B 109.1 . . ? C55A C54A H54B 109.1 . . ? H54A C54A H54B 107.9 . . ? N56A C55A C54A 110.6(4) . . ? N56A C55A H55A 109.5 . . ? C54A C55A H55A 109.5 . . ? N56A C55A H55B 109.5 . . ? C54A C55A H55B 109.5 . . ? H55A C55A H55B 108.1 . . ? C55A N56A C57A 112.3(4) . . ? C55A N56A H56E 114(6) . . ? C57A N56A H56E 106(6) . . ? N56A C57A C58 113.4(4) . . ? N56A C57A H57A 108.9 . . ? C58 C57A H57A 108.9 . . ? N56A C57A H57B 108.9 . . ? C58 C57A H57B 108.9 . . ? H57A C57A H57B 107.7 . . ? N53B C52B C51 110.0(4) . . ? N53B C52B H52C 109.7 . . ? C51 C52B H52C 109.7 . . ? N53B C52B H52D 109.7 . . ? C51 C52B H52D 109.7 . . ? H52C C52B H52D 108.2 . . ? C54B N53B C52B 114.4(4) . . ? C54B N53B H53F 111(5) . . ? C52B N53B H53F 105(5) . . ? N53B C54B C55B 107.3(4) . . ? N53B C54B H54C 110.2 . . ? C55B C54B H54C 110.2 . . ? N53B C54B H54D 110.2 . . ? C55B C54B H54D 110.2 . . ? H54C C54B H54D 108.5 . . ? N56B C55B C54B 110.3(4) . . ? N56B C55B H55C 109.6 . . ? C54B C55B H55C 109.6 . . ? N56B C55B H55D 109.6 . . ? C54B C55B H55D 109.6 . . ? H55C C55B H55D 108.1 . . ? C55B N56B C57B 115.8(4) . . ? C55B N56B H56A 108.3 . . ? C57B N56B H56A 108.3 . . ? C55B N56B H56B 108.3 . . ? C57B N56B H56B 108.3 . . ? H56A N56B H56B 107.4 . . ? N56B C57B C58 114.5(4) . . ? N56B C57B H57C 108.6 . . ? C58 C57B H57C 108.6 . . ? N56B C57B H57D 108.6 . . ? C58 C57B H57D 108.6 . . ? H57C C57B H57D 107.6 . . ? N53C C52C C51 112.4(4) . . ? N53C C52C H52E 109.1 . . ? C51 C52C H52E 109.1 . . ? N53C C52C H52F 109.1 . . ? C51 C52C H52F 109.1 . . ? H52E C52C H52F 107.9 . . ? C54C N53C C52C 115.3(4) . . ? C54C N53C H53G 116(5) . . ? C52C N53C H53G 103(5) . . ? N53C C54C C55C 112.8(5) . . ? N53C C54C H54E 109 . . ? C55C C54C H54E 109 . . ? N53C C54C H54F 109 . . ? C55C C54C H54F 109 . . ? H54E C54C H54F 107.8 . . ? N56C C55C C54C 115.4(5) . . ? N56C C55C H55E 108.4 . . ? C54C C55C H55E 108.4 . . ? N56C C55C H55F 108.4 . . ? C54C C55C H55F 108.4 . . ? H55E C55C H55F 107.5 . . ? C57C N56C C55C 114.6(4) . . ? C57C N56C H56C 108.6 . . ? C55C N56C H56C 108.6 . . ? C57C N56C H56D 108.6 . . ? C55C N56C H56D 108.6 . . ? H56C N56C H56D 107.6 . . ? N56C C57C C58 113.9(4) . . ? N56C C57C H57E 108.8 . . ? C58 C57C H57E 108.8 . . ? N56C C57C H57F 108.8 . . ? C58 C57C H57F 108.8 . . ? H57E C57C H57F 107.7 . . ? C57C C58 C57A 112.4(4) . . ? C57C C58 C59 112.0(5) . . ? C57A C58 C59 108.1(5) . . ? C57C C58 C57B 108.0(4) . . ? C57A C58 C57B 111.1(4) . . ? C59 C58 C57B 105.0(4) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 N60 H60A 109.5 . . ? C61 N60 H60B 109.5 . . ? H60A N60 H60B 109.5 . . ? C61 N60 H60C 109.5 . . ? H60A N60 H60C 109.5 . . ? H60B N60 H60C 109.5 . . ? N60 C61 C62A 110.0(4) . . ? N60 C61 C62B 107.5(4) . . ? C62A C61 C62B 112.6(4) . . ? N60 C61 C62C 105.8(4) . . ? C62A C61 C62C 108.7(4) . . ? C62B C61 C62C 112.1(5) . . ? N63A C62A C61 113.7(4) . . ? N63A C62A H62A 108.8 . . ? C61 C62A H62A 108.8 . . ? N63A C62A H62B 108.8 . . ? C61 C62A H62B 108.8 . . ? H62A C62A H62B 107.7 . . ? C62A N63A C64A 113.6(4) . . ? C62A N63A H63A 108.8 . . ? C64A N63A H63A 108.8 . . ? C62A N63A H63B 108.8 . . ? C64A N63A H63B 108.8 . . ? H63A N63A H63B 107.7 . . ? C65A C64A N63A 111.9(4) . . ? C65A C64A H64A 109.2 . . ? N63A C64A H64A 109.2 . . ? C65A C64A H64B 109.2 . . ? N63A C64A H64B 109.2 . . ? H64A C64A H64B 107.9 . . ? N66A C65A C64A 110.2(4) . . ? N66A C65A H65A 109.6 . . ? C64A C65A H65A 109.6 . . ? N66A C65A H65B 109.6 . . ? C64A C65A H65B 109.6 . . ? H65A C65A H65B 108.1 . . ? C65A N66A C67A 112.7(4) . . ? C65A N66A H66E 105(6) . . ? C67A N66A H66E 111(6) . . ? N66A C67A C68 113.2(4) . . ? N66A C67A H67A 108.9 . . ? C68 C67A H67A 108.9 . . ? N66A C67A H67B 108.9 . . ? C68 C67A H67B 108.9 . . ? H67A C67A H67B 107.7 . . ? N63B C62B C61 109.9(4) . . ? N63B C62B H62C 109.7 . . ? C61 C62B H62C 109.7 . . ? N63B C62B H62D 109.7 . . ? C61 C62B H62D 109.7 . . ? H62C C62B H62D 108.2 . . ? C64B N63B C62B 115.9(4) . . ? C64B N63B H63F 108(5) . . ? C62B N63B H63F 107(5) . . ? N63B C64B C65B 107.9(4) . . ? N63B C64B H64C 110.1 . . ? C65B C64B H64C 110.1 . . ? N63B C64B H64D 110.1 . . ? C65B C64B H64D 110.1 . . ? H64C C64B H64D 108.4 . . ? N66B C65B C64B 110.8(4) . . ? N66B C65B H65C 109.5 . . ? C64B C65B H65C 109.5 . . ? N66B C65B H65D 109.5 . . ? C64B C65B H65D 109.5 . . ? H65C C65B H65D 108.1 . . ? C65B N66B C67B 115.7(4) . . ? C65B N66B H66A 108.4 . . ? C67B N66B H66A 108.4 . . ? C65B N66B H66B 108.4 . . ? C67B N66B H66B 108.4 . . ? H66A N66B H66B 107.4 . . ? N66B C67B C68 115.6(4) . . ? N66B C67B H67C 108.4 . . ? C68 C67B H67C 108.4 . . ? N66B C67B H67D 108.4 . . ? C68 C67B H67D 108.4 . . ? H67C C67B H67D 107.5 . . ? N63C C62C C61 111.8(4) . . ? N63C C62C H62E 109.3 . . ? C61 C62C H62E 109.3 . . ? N63C C62C H62F 109.3 . . ? C61 C62C H62F 109.3 . . ? H62E C62C H62F 107.9 . . ? C64C N63C C62C 114.4(5) . . ? C64C N63C H63G 115(6) . . ? C62C N63C H63G 104(6) . . ? N63C C64C C65C 111.8(5) . . ? N63C C64C H64E 109.2 . . ? C65C C64C H64E 109.2 . . ? N63C C64C H64F 109.2 . . ? C65C C64C H64F 109.2 . . ? H64E C64C H64F 107.9 . . ? C64C C65C N66C 113.7(4) . . ? C64C C65C H65E 108.8 . . ? N66C C65C H65E 108.8 . . ? C64C C65C H65F 108.8 . . ? N66C C65C H65F 108.8 . . ? H65E C65C H65F 107.7 . . ? C67C N66C C65C 114.6(4) . . ? C67C N66C H66C 108.6 . . ? C65C N66C H66C 108.6 . . ? C67C N66C H66D 108.6 . . ? C65C N66C H66D 108.6 . . ? H66C N66C H66D 107.6 . . ? N66C C67C C68 113.6(4) . . ? N66C C67C H67E 108.8 . . ? C68 C67C H67E 108.8 . . ? N66C C67C H67F 108.8 . . ? C68 C67C H67F 108.8 . . ? H67E C67C H67F 107.7 . . ? C69 C68 C67B 105.8(4) . . ? C69 C68 C67C 111.3(4) . . ? C67B C68 C67C 108.8(4) . . ? C69 C68 C67A 108.6(4) . . ? C67B C68 C67A 110.5(4) . . ? C67C C68 C67A 111.7(4) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? 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 N10 H10A O3 0.91 2.18 3.025(6) 153.3 . N10 H10A Cl18 0.91 2.66 3.169(4) 116.4 1_565 N10 H10B Cl14 0.91 2.32 3.216(5) 167.5 1_455 N10 H10C Cl6 0.91 2.29 3.180(5) 165.1 1_565 N13A H13A Cl6 0.92 2.18 3.096(5) 172.9 1_565 N13A H13B N13B 0.92 2.37 2.994(7) 125.1 . N13A H13B Cl9 0.92 2.5 3.158(4) 128.9 . N16B H16A N16A 0.92 2.12 2.821(6) 132.6 . N16B H16A N13B 0.92 2.33 2.816(6) 112.4 . N16B H16B Cl12 0.92 2.25 3.094(5) 152.6 . N16C H16C Cl3 0.92 2.23 3.115(5) 160 . N16C H16D Cl1 0.92 2.31 3.141(5) 150.9 . N20 H20A Cl2 0.91 2.19 3.098(5) 172.7 1_565 N20 H20B Cl12 0.91 2.23 3.136(5) 170.6 . N20 H20C Cl13 0.91 2.24 3.133(5) 167.9 . N23A H23A Cl13 0.92 2.15 3.064(5) 173.2 . N23A H23B N23B 0.92 2.4 3.036(7) 126.4 . N23A H23B Cl11 0.92 2.47 3.149(5) 131 . N26B H26A N26A 0.92 2.13 2.822(6) 131.1 . N26B H26A N23B 0.92 2.3 2.793(6) 113.2 . N26B H26B Cl14 0.92 2.26 3.132(5) 157.4 . N26C H26C Cl21 0.92 2.26 3.124(5) 155.3 . N26C H26D Cl17 0.92 2.25 3.089(5) 150.9 1_655 N30 H30A Cl9 0.91 2.27 3.148(5) 161.3 3_676 N30 H30B Cl7 0.91 2.21 3.119(5) 173.1 2_656 N30 H30C Cl4 0.91 2.25 3.155(5) 171 1_455 N33A H33A Cl9 0.92 2.17 3.075(5) 168.9 3_676 N33A H33B N33B 0.92 2.34 2.994(6) 127.6 . N33A H33B Cl6 0.92 2.51 3.145(4) 126.3 3_666 N36B H36A N36A 0.92 2.13 2.843(7) 133.3 . N36B H36A N33B 0.92 2.33 2.821(6) 113.1 . N36B H36B Cl20 0.92 2.28 3.084(5) 145 . N36C H36C Cl12 0.92 2.22 3.109(6) 163.4 4_576 N36C H36D Cl7 0.92 2.33 3.161(5) 151 . N40 H40A Cl11 0.91 2.42 3.283(6) 157.5 3_776 N40 H40B Cl10 0.91 2.13 3.029(5) 172.3 2_756 N40 H40C Cl18 0.91 2.66 3.141(5) 113.6 3_666 N43A H43A Cl11 0.92 2.1 2.997(5) 166.4 3_776 N43A H43B N43B 0.92 2.29 2.955(7) 129.3 . N43A H43B Cl13 0.92 2.59 3.181(5) 122.7 3_776 N46B H46A N46A 0.92 2.14 2.853(7) 133.8 . N46B H46A N43B 0.92 2.36 2.835(6) 112 . N46B H46B Cl4 0.92 2.31 3.152(5) 152 . N46C H46C Cl14 0.92 2.25 3.139(5) 162.8 4_576 N46C H46D Cl10 0.92 2.29 3.133(5) 153 . N50 H50A Cl1 0.91 2.2 3.112(5) 178.5 . N50 H50B Cl3 0.91 2.26 3.165(5) 170.2 3_666 N50 H50C Cl5 0.91 2.26 3.154(5) 168.4 . N53A H53A Cl5 0.92 2.15 3.063(5) 169.8 . N53A H53B N53B 0.92 2.42 3.053(6) 126 . N53A H53B Cl8 0.92 2.51 3.191(4) 131.1 . N56B H56A N56A 0.92 2.18 2.883(7) 132.4 . N56B H56A N53B 0.92 2.29 2.786(6) 113 . N56B H56B Cl21 0.92 2.46 3.170(5) 134.5 3_666 N56B H56B O2 0.92 2.51 3.150(6) 127.3 . N56C H56C Cl20 0.92 2.23 3.074(5) 152.1 3_666 N56C H56D Cl18 0.92 2.21 3.067(5) 154.6 . N60 H60A Cl8 0.91 2.31 3.206(5) 167.5 3_666 N60 H60B O12 0.91 1.9 2.783(10) 161.9 3_766 N60 H60B O12' 0.91 1.98 2.855(10) 159.6 3_766 N60 H60C O2 0.91 1.94 2.785(6) 154.4 1_655 N63A H63A Cl8 0.92 2.18 3.098(5) 178.5 3_666 N63A H63B N63B 0.92 2.39 3.003(6) 124.2 . N63A H63B Cl5 0.92 2.51 3.194(4) 131.1 3_666 N66B H66A N66A 0.92 2.13 2.824(6) 131.3 . N66B H66A N63B 0.92 2.33 2.814(6) 112.3 . N66B H66B Cl3 0.92 2.29 3.123(5) 150.3 3_666 N66C H66C Cl4 0.92 2.27 3.160(5) 161.7 3_766 N66C H66D Cl2 0.92 2.3 3.115(4) 147.7 . N16A H16E Cl2 0.83(4) 2.64(6) 3.328(5) 142(7) 1_565 N13B H13F N13C 0.84(4) 2.23(6) 2.904(7) 138(7) . N13C H13G Cl26 0.81(4) 2.33(5) 3.029(11) 145(7) . N13C H13G Cl25 0.81(4) 2.44(4) 3.231(5) 165(7) . N26A H26E Cl18 0.83(4) 2.67(5) 3.389(5) 146(7) 1_665 N23B H23F N23C 0.84(4) 2.32(6) 2.929(6) 130(7) . N23C H23G O7 0.82(4) 2.51(6) 3.204(7) 142(7) 3_666 N36A H36E Cl10 0.83(4) 2.74(6) 3.334(5) 130(6) 2_756 N33B H33F N33C 0.84(4) 2.31(6) 2.918(7) 130(7) . N33C H33G O1 0.82(4) 2.59(6) 3.280(7) 143(7) 3_666 N46A H46E Cl7 0.85(4) 2.75(6) 3.372(5) 132(6) 2_756 N43B H43F N43C 0.84(4) 2.25(6) 2.882(6) 132(7) . N43C H43G Cl19 0.83(4) 2.82(6) 3.474(5) 137(6) 3_666 N56A H56E O2 0.82(4) 2.37(5) 3.147(6) 158(7) . N53B H53F N53C 0.85(4) 2.25(6) 2.939(6) 138(7) . N66A H66E Cl1 0.81(4) 2.72(6) 3.372(5) 139(7) . N63B H63F N63C 0.83(4) 2.30(6) 2.923(7) 131(7) . N63C H63G O4 0.81(4) 2.32(4) 3.114(8) 164(7) . #===END #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_PLAT306_gk204 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 RESPONSE: Water molecule H atoms not located. ; _chemical_name_common 6((CH3)(NH2)sar).24HCl.14(H2O) # Attachment 'CuL4rev.cif' data_gk165 _database_code_depnum_ccdc_archive 'CCDC 738801' #TrackingRef 'CuL4rev.cif' _audit_creation_date 2009-06-29T18:38:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C28 H61 Cl2 Cu N7 O8' _chemical_formula_moiety 'C28 H61 Cu N7, 2(Cl O4)' _chemical_formula_weight 758.28 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.803(3) _cell_length_b 17.759(4) _cell_length_c 27.012(10) _cell_angle_alpha 91.86(2) _cell_angle_beta 99.60(2) _cell_angle_gamma 119.65(2) _cell_volume 3586(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9187 _cell_measurement_theta_min 2.8806 _cell_measurement_theta_max 66.0207 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.70 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0456610651 _diffrn_orient_matrix_ub_12 -0.0226688768 _diffrn_orient_matrix_ub_13 0.0453882387 _diffrn_orient_matrix_ub_21 -0.0663668707 _diffrn_orient_matrix_ub_22 -0.0928942749 _diffrn_orient_matrix_ub_23 -0.0277195121 _diffrn_orient_matrix_ub_31 0.0637959203 _diffrn_orient_matrix_ub_32 -0.0308170348 _diffrn_orient_matrix_ub_33 0.0243134025 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_number 38793 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 66.04 _diffrn_reflns_theta_full 66.04 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 12163 _reflns_number_gt 7178 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal appeared to be a partial merohedral twin. ADDSYM finds a pseudo C2/c cell a=53.27(2) b=8.803(3) c=15.434(9) beta=97.71(2). Refinement in this setting resulted in R~.24. Refinment in the triclinic cell with the twin law of (1 0 -2 -1 0 -1 0 -1) gave a twin fraction of 0.37 and a lower residual, R=0.18. The two largest residual peaks are 1.09 and 1.16 Angstroms from the Cu atoms. ; _diffrn_reflns_twin_matrix ; 1.00 0.00 0.00 -2.00 -1.00 0.00 -1.00 0.00 -1.00 ; _refine_ls_twin_fraction 0.37 _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' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12163 _refine_ls_number_parameters 788 _refine_ls_number_restraints 488 _refine_ls_R_factor_all 0.2142 _refine_ls_R_factor_gt 0.184 _refine_ls_wR_factor_ref 0.4259 _refine_ls_wR_factor_gt 0.3883 _refine_ls_goodness_of_fit_ref 1.892 _refine_ls_restrained_S_all 1.978 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.008 _refine_diff_density_max 2.864 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.216 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 Cu 0.53826(16) 0.39933(7) 0.33358(5) 0.0851(4) Uani 1 1 d . . . Cu2 Cu 0.42070(17) 0.10084(7) 0.66692(5) 0.0864(4) Uani 1 1 d . . . N10 N 0.2341(13) 0.2040(5) 0.1865(3) 0.159(5) Uani 1 1 d D . . H10 H 0.2832 0.1749 0.1767 0.191 Uiso 1 1 calc R . . C11 C 0.3187(12) 0.2684(5) 0.2338(4) 0.103(3) Uani 1 1 d DU B . C12 C 0.0697(17) 0.1921(8) 0.1580(4) 0.201(3) Uani 1 1 d DU . . H12A H 0.0924 0.2495 0.1482 0.241 Uiso 1 1 calc R . . H12B H -0.016 0.1749 0.1807 0.241 Uiso 1 1 calc R . . C13 C -0.018(2) 0.1285(6) 0.1121(4) 0.181(5) Uani 1 1 d DU . . H13A H 0.046 0.1573 0.0852 0.217 Uiso 1 1 calc R . . H13B H -0.14 0.1189 0.1021 0.217 Uiso 1 1 calc R . . C14 C -0.035(2) 0.0423(6) 0.1102(5) 0.201(3) Uani 1 1 d DU . . H14A H -0.0496 0.0222 0.1438 0.241 Uiso 1 1 calc R . . H14B H 0.0767 0.0476 0.1036 0.241 Uiso 1 1 calc R . . C15 C -0.188(2) -0.0253(6) 0.0709(5) 0.215(7) Uani 1 1 d DU . . H15A H -0.2991 -0.0439 0.0836 0.258 Uiso 1 1 calc R . . H15B H -0.1968 0.0028 0.0403 0.258 Uiso 1 1 calc R . . C16 C -0.1843(18) -0.1044(6) 0.0552(4) 0.179(6) Uani 1 1 d DU . . H16A H -0.1687 -0.1312 0.0859 0.215 Uiso 1 1 calc R . . H16B H -0.0785 -0.0868 0.0401 0.215 Uiso 1 1 calc R . . C17 C -0.3458(19) -0.1720(7) 0.0183(5) 0.205(6) Uani 1 1 d DU . . H17A H -0.3623 -0.1448 -0.0119 0.246 Uiso 1 1 calc R . . H17B H -0.4511 -0.1899 0.0338 0.246 Uiso 1 1 calc R . . C18 C -0.3441(18) -0.2526(6) 0.0013(4) 0.170(5) Uani 1 1 d DU . . H18A H -0.2431 -0.2354 -0.016 0.204 Uiso 1 1 calc R . . H18B H -0.3217 -0.2785 0.0315 0.204 Uiso 1 1 calc R . . C19 C -0.5110(18) -0.3205(6) -0.0334(5) 0.185(6) Uani 1 1 d DU . . H19A H -0.5324 -0.2948 -0.0639 0.222 Uiso 1 1 calc R . . H19B H -0.6121 -0.337 -0.0163 0.222 Uiso 1 1 calc R . . C110 C -0.5106(19) -0.4018(6) -0.0500(4) 0.179(6) Uani 1 1 d DU . . H11A H -0.4966 -0.4294 -0.0196 0.214 Uiso 1 1 calc R . . H11B H -0.4048 -0.3848 -0.0651 0.214 Uiso 1 1 calc R . . C111 C -0.6738(17) -0.4686(6) -0.0875(4) 0.151(5) Uani 1 1 d DU . . H11C H -0.6831 -0.4427 -0.119 0.182 Uiso 1 1 calc R . . H11D H -0.7807 -0.4828 -0.0736 0.182 Uiso 1 1 calc R . . C112 C -0.6752(19) -0.5530(7) -0.1007(5) 0.201(3) Uani 1 1 d DU . . H11E H -0.5758 -0.5397 -0.1181 0.241 Uiso 1 1 calc R . . H11F H -0.653 -0.5755 -0.0689 0.241 Uiso 1 1 calc R . . C113 C -0.8432(19) -0.6217(6) -0.1333(5) 0.190(6) Uani 1 1 d DU . . H11G H -0.8702 -0.5969 -0.1635 0.228 Uiso 1 1 calc R . . H11H H -0.9404 -0.6378 -0.1146 0.228 Uiso 1 1 calc R . . C114 C -0.847(2) -0.7056(8) -0.1513(5) 0.215(7) Uani 1 1 d DU . . H11I H -0.9669 -0.748 -0.171 0.322 Uiso 1 1 calc R . . H11J H -0.818 -0.7305 -0.1219 0.322 Uiso 1 1 calc R . . H11K H -0.7594 -0.6919 -0.1727 0.322 Uiso 1 1 calc R . . C12A C 0.1859(15) 0.2541(5) 0.2644(4) 0.106(4) Uani 1 1 d . . . H12C H 0.1197 0.2829 0.2503 0.128 Uiso 0.5 1 calc PR A 1 H12D H 0.099 0.1905 0.2601 0.128 Uiso 0.5 1 calc PR A 1 H12I H 0.0723 0.2426 0.2446 0.128 Uiso 0.5 1 d PR A 2 H12J H 0.1644 0.2042 0.282 0.128 Uiso 0.5 1 d PR A 2 N13A N 0.2527(18) 0.2850(9) 0.3188(5) 0.080(4) Uiso 0.5 1 d P B 1 H13C H 0.2578 0.2397 0.3338 0.096 Uiso 0.5 1 calc PR B 1 N18A N 0.274(3) 0.3409(12) 0.3023(7) 0.116(6) Uiso 0.5 1 d P B 2 H18C H 0.2508 0.3811 0.2867 0.139 Uiso 0.5 1 calc PR B 2 C14A C 0.1680(15) 0.3105(5) 0.3460(4) 0.106(4) Uani 1 1 d . . . H14C H 0.0666 0.2574 0.3541 0.128 Uiso 0.5 1 calc PR B 1 H14D H 0.1168 0.3397 0.3242 0.128 Uiso 0.5 1 calc PR B 1 H14I H 0.0607 0.3138 0.3356 0.128 Uiso 0.5 1 d PR B 2 H14J H 0.1308 0.251 0.3524 0.128 Uiso 0.5 1 d PR B 2 C15A C 0.2706(12) 0.3683(7) 0.3927(4) 0.124(4) Uani 1 1 d . B . H15C H 0.201 0.391 0.4061 0.148 Uiso 0.5 1 calc PR C 1 H15D H 0.3012 0.3367 0.4183 0.148 Uiso 0.5 1 calc PR C 1 H15I H 0.2202 0.4049 0.3978 0.148 Uiso 0.5 1 d PR C 2 H15J H 0.2513 0.3324 0.4199 0.148 Uiso 0.5 1 d PR C 2 N16A N 0.4293(14) 0.4384(7) 0.3815(4) 0.057(3) Uiso 0.5 1 d P B 1 H16C H 0.3978 0.4758 0.3656 0.068 Uiso 0.5 1 calc PR B 1 N19A N 0.449(2) 0.4370(10) 0.3988(6) 0.090(5) Uiso 0.5 1 d P B 2 H19C H 0.422 0.4758 0.3828 0.108 Uiso 0.5 1 calc PR B 2 C17A C 0.5735(14) 0.4942(6) 0.4348(3) 0.093(3) Uani 1 1 d . . . H17C H 0.551 0.5409 0.4458 0.112 Uiso 0.5 1 calc PR B 1 H17D H 0.5495 0.4546 0.4611 0.112 Uiso 0.5 1 calc PR B 1 H17I H 0.5641 0.4696 0.4664 0.112 Uiso 0.5 1 d PR B 2 H17J H 0.5377 0.5377 0.4366 0.112 Uiso 0.5 1 d PR B 2 C12B C 0.4596(13) 0.2552(6) 0.2542(4) 0.124(4) Uani 1 1 d U . . H12E H 0.5172 0.2515 0.2264 0.149 Uiso 0.5 1 calc PR B 1 H12F H 0.4087 0.198 0.2671 0.149 Uiso 0.5 1 calc PR B 1 H12K H 0.5503 0.2744 0.2339 0.149 Uiso 0.5 1 d PR B 2 H12L H 0.405 0.1923 0.2526 0.149 Uiso 0.5 1 d PR B 2 N13B N 0.5958(16) 0.3209(7) 0.2943(4) 0.068(3) Uiso 0.5 1 d PU B 1 H13D H 0.6827 0.359 0.2777 0.081 Uiso 0.5 1 calc PR B 1 N18B N 0.544(2) 0.2848(9) 0.3143(5) 0.089(4) Uiso 0.5 1 d P B 2 H18D H 0.463 0.2419 0.3304 0.106 Uiso 0.5 1 calc PR B 2 C14B C 0.6933(10) 0.2920(5) 0.3318(4) 0.119(3) Uani 1 1 d . . . H14E H 0.7718 0.2796 0.315 0.143 Uiso 0.5 1 calc PR B 1 H14F H 0.6049 0.2365 0.3419 0.143 Uiso 0.5 1 calc PR B 1 H14K H 0.7686 0.3065 0.3071 0.143 Uiso 0.5 1 d PR B 2 H14L H 0.6609 0.2334 0.339 0.143 Uiso 0.5 1 d PR B 2 C15B C 0.8058(9) 0.3559(5) 0.3791(5) 0.109(4) Uani 1 1 d . B . H15E H 0.8453 0.3275 0.405 0.131 Uiso 0.5 1 calc PR D 1 H15F H 0.9128 0.4066 0.3714 0.131 Uiso 0.5 1 calc PR D 1 H15K H 0.9305 0.3733 0.3821 0.131 Uiso 0.5 1 d PR D 2 H15L H 0.7663 0.3248 0.4075 0.131 Uiso 0.5 1 d PR D 2 N16B N 0.7036(16) 0.3814(8) 0.3956(5) 0.070(3) Uiso 0.5 1 d P B 1 H16D H 0.6304 0.3395 0.4138 0.084 Uiso 0.5 1 calc PR B 1 N19B N 0.768(3) 0.4152(15) 0.3868(8) 0.143(8) Uiso 0.5 1 d P B 2 H19D H 0.8518 0.4551 0.37 0.172 Uiso 0.5 1 calc PR B 2 C17B C 0.8289(12) 0.4748(7) 0.4328(4) 0.115(4) Uani 1 1 d . . . H17E H 0.8497 0.462 0.4679 0.138 Uiso 0.5 1 calc PR B 1 H17F H 0.9465 0.5053 0.4231 0.138 Uiso 0.5 1 calc PR B 1 H17K H 0.9581 0.5081 0.4437 0.138 Uiso 0.5 1 d PR B 2 H17L H 0.7817 0.4327 0.4562 0.138 Uiso 0.5 1 d PR B 2 C12C C 0.403(2) 0.3644(6) 0.2175(4) 0.137(6) Uani 1 1 d U . . H12G H 0.4473 0.3656 0.186 0.164 Uiso 0.5 1 calc PR B 1 H12H H 0.3111 0.3817 0.2112 0.164 Uiso 0.5 1 calc PR B 1 H12M H 0.3265 0.3668 0.188 0.164 Uiso 0.5 1 d PR B 2 H12N H 0.5162 0.379 0.2089 0.164 Uiso 0.5 1 d PR B 2 N18C N 0.551(2) 0.4249(10) 0.2587(6) 0.096(5) Uiso 0.5 1 d P B 1 H18E H 0.6477 0.4209 0.2529 0.115 Uiso 0.5 1 calc PR B 1 N13C N 0.4392(16) 0.4297(7) 0.2642(4) 0.064(3) Uiso 0.5 1 d PU B 2 H13E H 0.341 0.4359 0.2657 0.077 Uiso 0.5 1 calc PR B 2 C14C C 0.5964(15) 0.5132(5) 0.2502(4) 0.103(4) Uani 1 1 d . . . H14G H 0.6704 0.5315 0.2242 0.123 Uiso 0.5 1 calc PR B 1 H14H H 0.4855 0.5142 0.237 0.123 Uiso 0.5 1 calc PR B 1 H14M H 0.6723 0.4954 0.2375 0.123 Uiso 0.5 1 d PR B 2 H14N H 0.5557 0.5394 0.2242 0.123 Uiso 0.5 1 d PR B 2 C15C C 0.6934(15) 0.5745(5) 0.2961(3) 0.098(4) Uani 1 1 d . B . H15G H 0.6165 0.5942 0.3078 0.118 Uiso 0.5 1 calc PR E 1 H15H H 0.8004 0.6263 0.2893 0.118 Uiso 0.5 1 calc PR E 1 H15M H 0.8204 0.5985 0.2982 0.118 Uiso 0.5 1 d PR E 2 H15N H 0.6701 0.6224 0.2938 0.118 Uiso 0.5 1 d PR E 2 N16C N 0.7485(16) 0.5323(7) 0.3361(4) 0.066(3) Uiso 0.5 1 d P B 1 H16E H 0.8503 0.5325 0.3306 0.079 Uiso 0.5 1 calc PR B 1 N19C N 0.663(2) 0.5455(9) 0.3385(5) 0.083(4) Uiso 0.5 1 d P B 2 H19E H 0.5698 0.5537 0.3432 0.1 Uiso 0.5 1 calc PR B 2 C17C C 0.7950(13) 0.5885(5) 0.3875(3) 0.090(3) Uani 1 1 d . . . H17G H 0.7223 0.6171 0.3851 0.108 Uiso 0.5 1 calc PR B 1 H17H H 0.9224 0.6351 0.3942 0.108 Uiso 0.5 1 calc PR B 1 H17M H 0.7913 0.6408 0.3967 0.108 Uiso 0.5 1 d PR B 2 H17N H 0.914 0.6069 0.3821 0.108 Uiso 0.5 1 d PR B 2 C11' C 0.7612(9) 0.5343(5) 0.4330(4) 0.087(2) Uani 1 1 d . B . C10' C 0.8783(13) 0.5992(6) 0.4798(3) 0.100(3) Uani 1 1 d . . . H10A H 0.8415 0.6425 0.4838 0.151 Uiso 1 1 calc R B . H10B H 1.0033 0.6288 0.4764 0.151 Uiso 1 1 calc R . . H10C H 0.866 0.5683 0.5097 0.151 Uiso 1 1 calc R . . N20 N 0.6601(15) 0.2906(6) 0.8161(4) 0.191(5) Uani 1 1 d DU . . H20 H 0.7725 0.3081 0.8293 0.229 Uiso 1 1 calc R . . C21 C 0.570(2) 0.2282(6) 0.7685(4) 0.144(5) Uani 1 1 d DU G . C22 C 0.5715(18) 0.3222(9) 0.8401(4) 0.201(3) Uani 1 1 d DU . . H22A H 0.4577 0.2728 0.8455 0.241 Uiso 1 1 calc R . . H22B H 0.5434 0.3598 0.8188 0.241 Uiso 1 1 calc R . . C23 C 0.690(3) 0.3745(7) 0.8907(4) 0.229(8) Uani 1 1 d DU . . H23A H 0.6114 0.3669 0.9147 0.275 Uiso 1 1 calc R . . H23B H 0.7629 0.3484 0.9035 0.275 Uiso 1 1 calc R . . C24 C 0.809(3) 0.4669(7) 0.8918(4) 0.201(3) Uani 1 1 d DU . . H24A H 0.7611 0.486 0.8621 0.241 Uiso 1 1 calc R . . H24B H 0.9259 0.4759 0.8875 0.241 Uiso 1 1 calc R . . C25 C 0.840(2) 0.5253(6) 0.9377(4) 0.170(5) Uani 1 1 d DU . . H25A H 0.7268 0.5233 0.9392 0.204 Uiso 1 1 calc R . . H25B H 0.8711 0.5013 0.9678 0.204 Uiso 1 1 calc R . . C26 C 0.980(2) 0.6166(7) 0.9414(4) 0.207(7) Uani 1 1 d DU . . H26A H 0.9466 0.6407 0.9117 0.248 Uiso 1 1 calc R . . H26B H 1.0918 0.6182 0.9386 0.248 Uiso 1 1 calc R . . C27 C 1.018(2) 0.6756(6) 0.9870(4) 0.182(6) Uani 1 1 d DU . . H27A H 0.9107 0.6806 0.9868 0.218 Uiso 1 1 calc R . . H27B H 1.0314 0.6464 1.0167 0.218 Uiso 1 1 calc R . . C28 C 1.174(2) 0.7649(7) 0.9958(5) 0.229(7) Uani 1 1 d DU . . H28A H 1.1778 0.7912 0.964 0.275 Uiso 1 1 calc R . . H28B H 1.2841 0.7622 1.0054 0.275 Uiso 1 1 calc R . . C29 C 1.169(2) 0.8221(7) 1.0364(5) 0.194(6) Uani 1 1 d DU . . H29A H 1.0704 0.8333 1.0238 0.233 Uiso 1 1 calc R . . H29B H 1.1399 0.79 1.0659 0.233 Uiso 1 1 calc R . . C210 C 1.3319(19) 0.9056(7) 1.0535(5) 0.236(6) Uani 1 1 d DU . . H21A H 1.3792 0.9292 1.0232 0.283 Uiso 1 1 calc R . . H21B H 1.4204 0.8943 1.0744 0.283 Uiso 1 1 calc R . . C211 C 1.3247(19) 0.9748(7) 1.0828(6) 0.207(7) Uani 1 1 d DU . . H21C H 1.2749 0.9516 1.1128 0.249 Uiso 1 1 calc R . . H21D H 1.241 0.9888 1.0617 0.249 Uiso 1 1 calc R . . C212 C 1.498(2) 1.0567(7) 1.1003(5) 0.201(3) Uani 1 1 d DU . . H21E H 1.532 1.0889 1.0711 0.241 Uiso 1 1 calc R . . H21F H 1.591 1.0419 1.1132 0.241 Uiso 1 1 calc R . . C213 C 1.496(2) 1.1148(7) 1.1409(5) 0.206(7) Uani 1 1 d DU . . H21G H 1.3852 1.1175 1.1315 0.248 Uiso 1 1 calc R . . H21H H 1.492 1.0887 1.1728 0.248 Uiso 1 1 calc R . . C214 C 1.651(3) 1.2047(8) 1.1501(5) 0.224(9) Uani 1 1 d DU . . H21I H 1.6287 1.2422 1.1715 0.336 Uiso 1 1 calc R . . H21J H 1.6697 1.2274 1.1177 0.336 Uiso 1 1 calc R . . H21K H 1.758 1.2043 1.1671 0.336 Uiso 1 1 calc R . . C22A C 0.4352(16) 0.2396(6) 0.7373(5) 0.135(5) Uani 1 1 d . . . H22C H 0.4946 0.2951 0.7229 0.163 Uiso 0.5 1 calc PR F 1 H22D H 0.3592 0.2446 0.7589 0.163 Uiso 0.5 1 calc PR F 1 H22I H 0.4759 0.3016 0.7421 0.163 Uiso 0.5 1 d PR F 2 H22J H 0.3268 0.2101 0.7505 0.163 Uiso 0.5 1 d PR F 2 N28A N 0.322(2) 0.1690(12) 0.6964(7) 0.110(6) Uiso 0.5 1 d P G 1 H28C H 0.2406 0.1276 0.713 0.132 Uiso 0.5 1 calc PR G 1 N23A N 0.3929(19) 0.2158(9) 0.6803(5) 0.082(4) Uiso 0.5 1 d PU G 2 H23C H 0.4684 0.262 0.6649 0.099 Uiso 0.5 1 calc PR G 2 C24A C 0.2054(9) 0.1846(5) 0.6587(4) 0.139(3) Uani 1 1 d U . . H24C H 0.2705 0.2464 0.6526 0.167 Uiso 0.5 1 calc PR G 1 H24D H 0.1006 0.1753 0.6723 0.167 Uiso 0.5 1 calc PR G 1 H24I H 0.1971 0.2359 0.652 0.167 Uiso 0.5 1 d PR G 2 H24J H 0.1271 0.1552 0.6817 0.167 Uiso 0.5 1 d PR G 2 C25A C 0.1428(15) 0.1278(6) 0.6105(5) 0.132(5) Uani 1 1 d U G . H25C H 0.0274 0.0748 0.6113 0.158 Uiso 0.5 1 calc PR H 1 H25D H 0.1199 0.1588 0.583 0.158 Uiso 0.5 1 calc PR H 1 H25I H 0.015 0.104 0.5998 0.158 Uiso 0.5 1 d PR H 2 H25J H 0.2 0.1606 0.5845 0.158 Uiso 0.5 1 d PR H 2 N29A N 0.246(2) 0.1047(10) 0.5999(6) 0.101(5) Uiso 0.5 1 d PD G 1 H29C H 0.3216 0.1486 0.5833 0.121 Uiso 0.5 1 calc PR G 1 N26A N 0.1885(18) 0.0576(8) 0.6099(5) 0.075(4) Uiso 0.5 1 d PD G 2 H26C H 0.0999 0.0141 0.6237 0.09 Uiso 0.5 1 calc PR G 2 C27A C 0.1638(13) 0.0158(7) 0.5623(4) 0.104(4) Uani 1 1 d . . . H27C H 0.0404 -0.0238 0.5666 0.125 Uiso 0.5 1 calc PR G 1 H27D H 0.155 0.0299 0.5271 0.125 Uiso 0.5 1 calc PR G 1 H27I H 0.2073 0.0584 0.5389 0.125 Uiso 0.5 1 d PR G 2 H27J H 0.0386 -0.0258 0.5482 0.125 Uiso 0.5 1 d PR G 2 C22B C 0.721(2) 0.2530(6) 0.7418(4) 0.139(6) Uani 1 1 d . . . H22E H 0.7287 0.298 0.72 0.167 Uiso 0.5 1 calc PR G 1 H22F H 0.8348 0.278 0.767 0.167 Uiso 0.5 1 calc PR G 1 H22K H 0.7914 0.2316 0.761 0.167 Uiso 0.5 1 d PR G 2 H22L H 0.7954 0.3161 0.7451 0.167 Uiso 0.5 1 d PR G 2 N23B N 0.692(2) 0.1798(10) 0.7125(6) 0.092(4) Uiso 0.5 1 d P G 1 H23D H 0.725 0.146 0.7321 0.111 Uiso 0.5 1 calc PR G 1 N28B N 0.691(2) 0.2173(11) 0.6825(6) 0.102(5) Uiso 0.5 1 d P G 2 H28D H 0.6771 0.2582 0.6646 0.123 Uiso 0.5 1 calc PR G 2 C24B C 0.8015(12) 0.2107(6) 0.6666(5) 0.112(4) Uani 1 1 d U . . H24E H 0.8139 0.2673 0.659 0.135 Uiso 0.5 1 calc PR G 1 H24F H 0.9235 0.2211 0.6793 0.135 Uiso 0.5 1 calc PR G 1 H24K H 0.8697 0.1946 0.6915 0.135 Uiso 0.5 1 d PR G 2 H24L H 0.883 0.2686 0.6594 0.135 Uiso 0.5 1 d PR G 2 C25B C 0.7291(16) 0.1543(7) 0.6217(5) 0.129(5) Uani 1 1 d U G . H25E H 0.7806 0.1872 0.5941 0.155 Uiso 0.5 1 calc PR I 1 H25F H 0.7622 0.1086 0.6249 0.155 Uiso 0.5 1 calc PR I 1 H25K H 0.7186 0.1849 0.5934 0.155 Uiso 0.5 1 d PR I 2 H25L H 0.8181 0.1386 0.618 0.155 Uiso 0.5 1 d PR I 2 N26B N 0.5448(19) 0.1147(9) 0.6090(5) 0.083(4) Uiso 0.5 1 d PU G 1 H26D H 0.522 0.152 0.5899 0.099 Uiso 0.5 1 calc PR G 1 N29B N 0.5525(17) 0.0673(9) 0.6196(5) 0.074(3) Uiso 0.5 1 d P G 2 H29D H 0.5837 0.0303 0.6361 0.089 Uiso 0.5 1 calc PR G 2 C27B C 0.4613(13) 0.0248(7) 0.5711(3) 0.097(3) Uani 1 1 d . . . H27E H 0.4809 0.0394 0.5368 0.116 Uiso 0.5 1 calc PR G 1 H27F H 0.5263 -0.0058 0.5827 0.116 Uiso 0.5 1 calc PR G 1 H27K H 0.5128 -0.0085 0.5602 0.116 Uiso 0.5 1 d PR G 2 H27L H 0.4714 0.0655 0.5469 0.116 Uiso 0.5 1 d PR G 2 C22C C 0.492(2) 0.1405(6) 0.7832(4) 0.144(6) Uani 1 1 d U . . H22G H 0.3668 0.1199 0.7861 0.173 Uiso 0.5 1 calc PR G 1 H22H H 0.5594 0.1424 0.8169 0.173 Uiso 0.5 1 calc PR G 1 H22M H 0.4367 0.1391 0.8117 0.173 Uiso 0.5 1 d PR G 2 H22N H 0.582 0.1246 0.7932 0.173 Uiso 0.5 1 d PR G 2 N28C N 0.493(2) 0.0744(10) 0.7439(6) 0.093(4) Uiso 0.5 1 d P G 1 H28E H 0.6031 0.077 0.7494 0.112 Uiso 0.5 1 calc PR G 1 N23C N 0.3358(17) 0.0660(8) 0.7390(5) 0.070(3) Uiso 0.5 1 d PU G 2 H23E H 0.224 0.0592 0.739 0.084 Uiso 0.5 1 calc PR G 2 C24C C 0.3457(17) -0.0129(5) 0.7509(3) 0.106(4) Uani 1 1 d U . . H24G H 0.3888 -0.0356 0.7797 0.128 Uiso 0.5 1 calc PR G 1 H24H H 0.2448 -0.0076 0.7584 0.128 Uiso 0.5 1 calc PR G 1 H24M H 0.4694 0.0042 0.764 0.128 Uiso 0.5 1 d PR G 2 H24N H 0.2776 -0.0391 0.7766 0.128 Uiso 0.5 1 d PR G 2 C25C C 0.286(2) -0.0733(5) 0.7036(4) 0.128(5) Uani 1 1 d . G . H25G H 0.3069 -0.1219 0.7117 0.154 Uiso 0.5 1 calc PR J 1 H25H H 0.1556 -0.0988 0.6922 0.154 Uiso 0.5 1 calc PR J 1 H25M H 0.3641 -0.0968 0.7016 0.154 Uiso 0.5 1 d PR J 2 H25N H 0.1704 -0.1216 0.7061 0.154 Uiso 0.5 1 d PR J 2 N26C N 0.3671(17) -0.0382(8) 0.6628(4) 0.065(3) Uiso 0.5 1 d P G 1 H26E H 0.4727 -0.0392 0.665 0.078 Uiso 0.5 1 calc PR G 1 N29C N 0.267(2) -0.0413(11) 0.6584(6) 0.099(5) Uiso 0.5 1 d P G 2 H29E H 0.1537 -0.0492 0.6567 0.119 Uiso 0.5 1 calc PR G 2 C27C C 0.2375(17) -0.0877(6) 0.6127(3) 0.103(4) Uani 1 1 d . . . H27G H 0.247 -0.1397 0.6041 0.124 Uiso 0.5 1 calc PR G 1 H27H H 0.1144 -0.109 0.6176 0.124 Uiso 0.5 1 calc PR G 1 H27M H 0.1186 -0.1389 0.6037 0.124 Uiso 0.5 1 d PR G 2 H27N H 0.322 -0.1082 0.6173 0.124 Uiso 0.5 1 d PR G 2 C21' C 0.2654(15) -0.0359(6) 0.5679(3) 0.097(3) Uani 1 1 d . G . C20' C 0.187(2) -0.1003(7) 0.5199(4) 0.147(7) Uani 1 1 d . . . H20A H 0.0603 -0.1412 0.5183 0.22 Uiso 1 1 calc R G . H20B H 0.2506 -0.1328 0.5198 0.22 Uiso 1 1 calc R . . H20C H 0.2008 -0.0686 0.4904 0.22 Uiso 1 1 calc R . . Cl1 Cl 0.6569(6) 0.3670(2) 0.58373(19) 0.199(2) Uani 1 1 d D . . O11 O 0.5422(8) 0.3633(6) 0.6157(4) 0.220(4) Uani 1 1 d DU . . O12 O 0.6995(11) 0.4279(6) 0.5528(4) 0.312(5) Uani 1 1 d DU . . O13 O 0.8302(11) 0.3917(8) 0.6202(4) 0.258(8) Uani 1 1 d DU . . O14 O 0.612(2) 0.2839(6) 0.5625(6) 0.411(19) Uani 1 1 d DU . . Cl2 Cl 0.3077(5) 0.1310(2) 0.41489(18) 0.180(2) Uani 1 1 d D . . O21 O 0.2734(17) 0.0614(7) 0.4414(5) 0.317(6) Uani 1 1 d DU . . O22 O 0.1641(14) 0.1189(8) 0.3761(4) 0.205(6) Uani 1 1 d DU . . O23 O 0.4604(11) 0.1469(8) 0.3982(6) 0.359(10) Uani 1 1 d DU . . O24 O 0.341(3) 0.2055(9) 0.4464(7) 0.58(2) Uani 1 1 d DU . . Cl3 Cl 0.8681(5) 1.01982(18) 0.74787(13) 0.1295(11) Uani 1 1 d DU . . O31 O 0.9481(16) 0.9752(8) 0.7290(7) 0.280(8) Uani 1 1 d DU . . O32 O 0.951(2) 1.1010(7) 0.7446(5) 0.303(7) Uani 1 1 d DU . . O33 O 0.791(3) 1.0167(13) 0.7897(4) 0.357(13) Uani 1 1 d DU . . O34 O 0.7267(17) 1.0096(12) 0.7073(6) 0.344(9) Uani 1 1 d DU . . Cl4 Cl 0.0472(4) 0.4782(2) 0.25254(12) 0.1205(11) Uani 1 1 d D . . O41 O -0.002(3) 0.3875(9) 0.2535(8) 0.363(14) Uani 1 1 d DU . . O42 O -0.0867(19) 0.4771(12) 0.2156(6) 0.348(10) Uani 1 1 d DU . . O43 O 0.2093(10) 0.5196(9) 0.2464(6) 0.261(7) Uani 1 1 d DU . . O44 O 0.0252(18) 0.5057(11) 0.2945(4) 0.257(8) Uani 1 1 d DU . . 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 Cu1 0.0825(7) 0.0517(5) 0.1038(8) 0.0028(5) 0.0174(7) 0.0224(5) Cu2 0.0818(7) 0.0473(5) 0.1095(9) 0.0079(6) 0.0179(7) 0.0184(5) N10 0.150(9) 0.109(6) 0.137(7) -0.071(5) 0.008(7) 0.018(6) C11 0.066(4) 0.060(4) 0.158(8) -0.020(5) 0.027(5) 0.015(3) C12 0.227(5) 0.237(3) 0.121(3) -0.012(3) 0.022(4) 0.110(3) C13 0.146(10) 0.215(5) 0.133(8) -0.010(6) -0.014(8) 0.071(7) C14 0.227(5) 0.237(3) 0.121(3) -0.012(3) 0.022(4) 0.110(3) C15 0.215(12) 0.196(5) 0.207(12) -0.009(7) -0.023(9) 0.107(6) C16 0.197(10) 0.195(6) 0.121(8) 0.010(6) -0.025(8) 0.101(6) C17 0.191(10) 0.195(6) 0.198(12) -0.007(6) -0.032(9) 0.100(6) C18 0.178(10) 0.210(6) 0.110(8) -0.002(6) -0.002(7) 0.100(6) C19 0.185(10) 0.200(6) 0.136(10) 0.003(6) 0.000(8) 0.084(6) C110 0.182(10) 0.205(6) 0.116(9) -0.002(6) -0.002(8) 0.085(7) C111 0.136(9) 0.162(5) 0.106(7) 0.048(5) 0.012(6) 0.041(5) C112 0.227(5) 0.237(3) 0.121(3) -0.012(3) 0.022(4) 0.110(3) C113 0.221(10) 0.145(5) 0.185(11) 0.060(6) -0.008(8) 0.093(6) C114 0.224(12) 0.244(7) 0.167(12) -0.036(8) -0.076(10) 0.151(8) C12A 0.104(7) 0.056(4) 0.116(7) 0.012(5) 0.024(6) 0.008(5) C14A 0.122(7) 0.045(4) 0.136(7) 0.026(4) 0.054(6) 0.021(4) C15A 0.106(5) 0.113(6) 0.170(8) 0.018(6) 0.096(5) 0.049(5) C17A 0.132(6) 0.093(5) 0.058(4) 0.016(4) 0.024(4) 0.058(5) C12B 0.095(5) 0.108(5) 0.171(8) -0.029(6) 0.058(5) 0.046(4) C14B 0.122(3) 0.115(4) 0.213(9) 0.069(5) 0.098(5) 0.106(3) C15B 0.052(3) 0.085(4) 0.214(11) 0.013(5) 0.018(5) 0.055(3) C17B 0.050(4) 0.109(7) 0.142(8) 0.005(6) 0.035(5) 0.004(5) C12C 0.167(11) 0.067(5) 0.108(7) -0.001(5) 0.006(8) 0.016(7) C14C 0.115(7) 0.056(4) 0.102(6) 0.021(4) 0.012(6) 0.020(4) C15C 0.112(7) 0.057(4) 0.093(6) 0.014(4) 0.005(5) 0.024(4) C17C 0.089(5) 0.071(4) 0.103(6) -0.003(4) 0.035(4) 0.031(4) C11' 0.083(3) 0.123(4) 0.100(6) 0.008(4) 0.018(4) 0.086(3) C10' 0.086(5) 0.114(6) 0.078(5) -0.025(5) -0.018(4) 0.047(5) N20 0.257(9) 0.099(5) 0.225(11) -0.032(6) 0.007(10) 0.112(5) C21 0.199(10) 0.071(5) 0.143(9) -0.026(5) -0.024(8) 0.074(5) C22 0.227(5) 0.237(3) 0.121(3) -0.012(3) 0.022(4) 0.110(3) C23 0.254(15) 0.237(6) 0.159(8) -0.056(7) 0.050(9) 0.100(10) C24 0.227(5) 0.237(3) 0.121(3) -0.012(3) 0.022(4) 0.110(3) C25 0.216(10) 0.196(6) 0.131(7) 0.019(5) 0.074(8) 0.119(7) C26 0.212(13) 0.233(6) 0.126(8) 0.001(6) 0.075(9) 0.068(8) C27 0.225(11) 0.193(6) 0.149(8) 0.031(6) 0.085(9) 0.108(7) C28 0.235(13) 0.232(7) 0.174(11) -0.016(6) 0.081(10) 0.075(8) C29 0.236(12) 0.199(6) 0.150(9) 0.033(6) 0.085(9) 0.099(7) C210 0.250(11) 0.253(6) 0.161(9) -0.028(7) 0.122(8) 0.076(7) C211 0.194(11) 0.225(7) 0.201(13) -0.009(7) 0.040(10) 0.107(6) C212 0.227(5) 0.237(3) 0.121(3) -0.012(3) 0.022(4) 0.110(3) C213 0.243(13) 0.201(8) 0.177(11) 0.000(7) 0.037(10) 0.118(7) C214 0.252(15) 0.250(8) 0.111(8) -0.010(8) 0.087(10) 0.071(10) C22A 0.095(7) 0.050(4) 0.220(14) -0.031(6) -0.004(8) 0.020(4) C24A 0.094(2) 0.121(3) 0.210(10) 0.028(5) 0.049(4) 0.055(2) C25A 0.122(6) 0.088(5) 0.201(12) -0.008(6) 0.007(8) 0.073(4) C27A 0.065(5) 0.104(6) 0.126(8) 0.015(6) 0.011(5) 0.033(5) C22B 0.187(13) 0.051(5) 0.099(7) 0.006(5) 0.031(8) 0.001(7) C24B 0.046(4) 0.063(4) 0.205(11) 0.032(6) 0.030(5) 0.009(3) C25B 0.087(6) 0.067(5) 0.204(11) 0.021(7) 0.036(7) 0.015(5) C27B 0.078(5) 0.116(6) 0.094(5) 0.047(5) 0.035(4) 0.041(4) C22C 0.206(12) 0.066(5) 0.113(7) -0.008(5) 0.012(8) 0.040(7) C24C 0.164(9) 0.052(4) 0.073(5) 0.004(4) 0.019(6) 0.034(5) C25C 0.229(12) 0.048(4) 0.078(5) 0.011(4) 0.016(7) 0.053(5) C27C 0.127(8) 0.064(5) 0.060(4) 0.002(4) 0.006(5) 0.009(5) C21' 0.149(7) 0.085(5) 0.045(4) -0.006(4) -0.008(4) 0.061(5) C20' 0.226(15) 0.122(8) 0.075(6) 0.031(6) 0.032(8) 0.074(9) Cl1 0.188(3) 0.146(2) 0.280(4) 0.127(3) 0.110(3) 0.074(2) O11 0.125(3) 0.233(6) 0.426(12) 0.195(7) 0.175(5) 0.138(4) O12 0.258(4) 0.405(8) 0.550(12) 0.369(8) 0.318(6) 0.286(4) O13 0.128(9) 0.270(13) 0.298(14) 0.122(12) 0.037(10) 0.042(10) O14 0.39(3) 0.269(19) 0.38(3) -0.028(19) -0.10(2) 0.08(2) Cl2 0.106(2) 0.137(2) 0.228(4) 0.085(3) 0.008(2) 0.016(2) O21 0.205(9) 0.437(11) 0.427(12) 0.364(9) 0.174(8) 0.201(8) O22 0.189(9) 0.245(9) 0.184(8) 0.126(7) 0.032(8) 0.109(8) O23 0.072(5) 0.314(11) 0.66(2) 0.314(13) 0.043(10) 0.070(7) O24 0.46(3) 0.44(3) 0.46(2) -0.22(2) -0.27(2) 0.07(3) Cl3 0.168(2) 0.0934(12) 0.148(2) 0.0483(14) 0.0488(19) 0.0756(13) O31 0.216(7) 0.254(8) 0.47(2) 0.081(11) 0.074(12) 0.193(6) O32 0.443(13) 0.176(7) 0.255(12) -0.082(7) -0.180(11) 0.211(7) O33 0.313(18) 0.59(2) 0.169(8) 0.190(12) 0.121(10) 0.198(18) O34 0.284(7) 0.548(15) 0.35(2) 0.005(15) -0.014(12) 0.351(7) Cl4 0.1115(17) 0.1187(17) 0.1292(19) 0.0499(15) 0.0388(15) 0.0510(14) O41 0.36(2) 0.296(17) 0.42(3) 0.006(18) -0.07(2) 0.199(16) O42 0.303(11) 0.511(19) 0.37(2) 0.042(18) 0.028(16) 0.323(11) O43 0.094(3) 0.292(12) 0.403(17) 0.083(11) 0.100(6) 0.087(5) O44 0.246(11) 0.410(18) 0.149(8) 0.048(10) 0.107(8) 0.172(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N13B 2.026(14) . ? Cu1 N16A 2.023(13) . ? Cu1 N18A 2.026(19) . ? Cu1 N18C 2.096(16) . ? Cu1 N18B 2.111(17) . ? Cu1 N13C 2.134(12) . ? Cu1 N16C 2.152(11) . ? Cu1 N16B 2.170(14) . ? Cu1 N19B 2.16(3) . ? Cu1 N19A 2.252(18) . ? Cu1 N19C 2.251(14) . ? Cu1 N13A 2.272(12) . ? Cu2 N28A 2.01(2) . ? Cu2 N26B 2.007(16) . ? Cu2 N29B 2.113(15) . ? Cu2 N26A 2.112(13) . ? Cu2 N29C 2.175(17) . ? Cu2 N23B 2.187(15) . ? Cu2 N29A 2.200(18) . ? Cu2 N23C 2.200(13) . ? Cu2 N23A 2.198(17) . ? Cu2 N28C 2.206(16) . ? Cu2 N28B 2.201(16) . ? Cu2 N26C 2.268(13) . ? N10 C12 1.431(14) . ? N10 C11 1.495(12) . ? N10 H10 0.88 . ? C11 C12B 1.402(16) . ? C11 C12A 1.468(16) . ? C11 C12C 1.599(14) . ? C12 C13 1.459(12) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.458(14) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.491(13) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.473(14) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.489(12) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.497(14) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.485(12) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C110 1.499(14) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C110 C111 1.500(12) . ? C110 H11A 0.99 . ? C110 H11B 0.99 . ? C111 C112 1.522(14) . ? C111 H11C 0.99 . ? C111 H11D 0.99 . ? C112 C113 1.471(13) . ? C112 H11E 0.99 . ? C112 H11F 0.99 . ? C113 C114 1.534(15) . ? C113 H11G 0.99 . ? C113 H11H 0.99 . ? C114 H11I 0.98 . ? C114 H11J 0.98 . ? C114 H11K 0.98 . ? C12A N13A 1.466(16) . ? C12A N18A 1.57(2) . ? C12A H12C 0.99 . ? C12A H12D 0.99 . ? C12A H12I 0.97 . ? C12A H12J 0.97 . ? N13A C14A 1.34(2) . ? N13A H13C 0.93 . ? N18A C14A 1.57(2) . ? N18A H18C 0.93 . ? C14A C15A 1.441(13) . ? C14A H14C 0.99 . ? C14A H14D 0.99 . ? C14A H14I 0.97 . ? C14A H14J 0.97 . ? C15A N19A 1.410(17) . ? C15A N16A 1.427(14) . ? C15A H15C 0.99 . ? C15A H15D 0.99 . ? C15A H15I 0.97 . ? C15A H15J 0.97 . ? N16A C17A 1.648(12) . ? N16A H16C 0.93 . ? N19A C17A 1.287(16) . ? N19A H19C 0.93 . ? C17A C11' 1.450(13) . ? C17A H17C 0.99 . ? C17A H17D 0.99 . ? C17A H17I 0.97 . ? C17A H17J 0.97 . ? C12B N13B 1.440(14) . ? C12B N18B 1.620(18) . ? C12B H12E 0.99 . ? C12B H12F 0.99 . ? C12B H12K 0.97 . ? C12B H12L 0.97 . ? N13B C14B 1.485(17) . ? N13B H13D 0.93 . ? N18B C14B 1.259(19) . ? N18B H18D 0.93 . ? C14B C15B 1.508(14) . ? C14B H14E 0.99 . ? C14B H14F 0.99 . ? C14B H14K 0.97 . ? C14B H14L 0.97 . ? C15B N19B 1.27(3) . ? C15B N16B 1.317(18) . ? C15B H15E 0.99 . ? C15B H15F 0.99 . ? C15B H15K 0.97 . ? C15B H15L 0.97 . ? N16B C17B 1.640(15) . ? N16B H16D 0.93 . ? N19B C17B 1.44(2) . ? N19B H19D 0.93 . ? C17B C11' 1.448(16) . ? C17B H17E 0.99 . ? C17B H17F 0.99 . ? C17B H17K 0.97 . ? C17B H17L 0.97 . ? C12C N18C 1.464(18) . ? C12C N13C 1.563(16) . ? C12C H12G 0.99 . ? C12C H12H 0.99 . ? C12C H12M 0.97 . ? C12C H12N 0.97 . ? N18C C14C 1.450(19) . ? N18C H18E 0.93 . ? N13C C14C 1.561(14) . ? N13C H13E 0.93 . ? C14C C15C 1.447(12) . ? C14C H14G 0.99 . ? C14C H14H 0.99 . ? C14C H14M 0.97 . ? C14C H14N 0.97 . ? C15C N19C 1.285(17) . ? C15C N16C 1.482(17) . ? C15C H15G 0.99 . ? C15C H15H 0.99 . ? C15C H15M 0.97 . ? C15C H15N 0.97 . ? N16C C17C 1.553(14) . ? N16C H16E 0.93 . ? N19C C17C 1.493(16) . ? N19C H19E 0.93 . ? C17C C11' 1.562(13) . ? C17C H17G 0.99 . ? C17C H17H 0.99 . ? C17C H17M 0.97 . ? C17C H17N 0.97 . ? C11' C10' 1.512(11) . ? C10' H10A 0.98 . ? C10' H10B 0.98 . ? C10' H10C 0.98 . ? N20 C22 1.386(15) . ? N20 C21 1.486(12) . ? N20 H20 0.88 . ? C21 C22A 1.44(2) . ? C21 C22C 1.458(15) . ? C21 C22B 1.49(2) . ? C22 C23 1.515(13) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C24 1.442(13) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 C25 1.485(13) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 C26 1.457(13) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.468(13) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.473(13) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.489(15) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C210 1.449(13) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C210 C211 1.475(15) . ? C210 H21A 0.99 . ? C210 H21B 0.99 . ? C211 C212 1.480(14) . ? C211 H21C 0.99 . ? C211 H21D 0.99 . ? C212 C213 1.492(15) . ? C212 H21E 0.99 . ? C212 H21F 0.99 . ? C213 C214 1.477(14) . ? C213 H21G 0.99 . ? C213 H21H 0.99 . ? C214 H21I 0.98 . ? C214 H21J 0.98 . ? C214 H21K 0.98 . ? C22A N28A 1.447(19) . ? C22A N23A 1.517(19) . ? C22A H22C 0.99 . ? C22A H22D 0.99 . ? C22A H22I 0.97 . ? C22A H22J 0.97 . ? N28A C24A 1.46(2) . ? N28A H28C 0.93 . ? N23A C24A 1.458(17) . ? N23A H23C 0.93 . ? C24A C25A 1.464(16) . ? C24A H24C 0.99 . ? C24A H24D 0.99 . ? C24A H24I 0.97 . ? C24A H24J 0.97 . ? C25A N29A 1.23(2) . ? C25A N26A 1.49(2) . ? C25A H25C 0.99 . ? C25A H25D 0.99 . ? C25A H25I 0.97 . ? C25A H25J 0.97 . ? N29A C27A 1.604(19) . ? N29A H29C 0.93 . ? N26A C27A 1.392(17) . ? N26A H26C 0.93 . ? C27A C21' 1.562(18) . ? C27A H27C 0.99 . ? C27A H27D 0.99 . ? C27A H27I 0.97 . ? C27A H27J 0.97 . ? C22B N23B 1.39(2) . ? C22B N28B 1.63(2) . ? C22B H22E 0.99 . ? C22B H22F 0.99 . ? C22B H22K 0.97 . ? C22B H22L 0.97 . ? N23B C24B 1.64(2) . ? N23B H23D 0.93 . ? N28B C24B 1.18(2) . ? N28B H28D 0.93 . ? C24B C25B 1.383(17) . ? C24B H24E 0.99 . ? C24B H24F 0.99 . ? C24B H24K 0.97 . ? C24B H24L 0.97 . ? C25B N26B 1.384(19) . ? C25B N29B 1.547(16) . ? C25B H25E 0.99 . ? C25B H25F 0.99 . ? C25B H25K 0.97 . ? C25B H25L 0.97 . ? N26B C27B 1.618(17) . ? N26B H26D 0.93 . ? N29B C27B 1.383(15) . ? N29B H29D 0.93 . ? C27B C21' 1.499(14) . ? C27B H27E 0.99 . ? C27B H27F 0.99 . ? C27B H27K 0.97 . ? C27B H27L 0.97 . ? C22C N28C 1.57(2) . ? C22C N23C 1.616(15) . ? C22C H22G 0.99 . ? C22C H22H 0.99 . ? C22C H22M 0.97 . ? C22C H22N 0.97 . ? N28C C24C 1.497(17) . ? N28C H28E 0.93 . ? N23C C24C 1.490(18) . ? N23C H23E 0.93 . ? C24C C25C 1.480(12) . ? C24C H24G 0.99 . ? C24C H24H 0.99 . ? C24C H24M 0.97 . ? C24C H24N 0.97 . ? C25C N29C 1.38(2) . ? C25C N26C 1.406(17) . ? C25C H25G 0.99 . ? C25C H25H 0.99 . ? C25C H25M 0.97 . ? C25C H25N 0.97 . ? N26C C27C 1.523(14) . ? N26C H26E 0.93 . ? N29C C27C 1.373(19) . ? N29C H29E 0.93 . ? C27C C21' 1.524(12) . ? C27C H27G 0.99 . ? C27C H27H 0.99 . ? C27C H27M 0.97 . ? C27C H27N 0.97 . ? C21' C20' 1.514(13) . ? C20' H20A 0.98 . ? C20' H20B 0.98 . ? C20' H20C 0.98 . ? Cl1 O12 1.330(9) . ? Cl1 O14 1.399(10) . ? Cl1 O11 1.415(9) . ? Cl1 O13 1.517(10) . ? Cl2 O21 1.376(10) . ? Cl2 O23 1.387(12) . ? Cl2 O22 1.421(10) . ? Cl2 O24 1.420(14) . ? Cl3 O32 1.268(12) . ? Cl3 O33 1.400(16) . ? Cl3 O31 1.425(15) . ? Cl3 O34 1.447(14) . ? Cl4 O43 1.286(8) . ? Cl4 O44 1.302(12) . ? Cl4 O42 1.404(14) . ? Cl4 O41 1.448(15) . ? 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 N13B Cu1 N16A 160.2(5) . . ? N18A Cu1 N18C 80.0(7) . . ? N18A Cu1 N18B 92.0(7) . . ? N18C Cu1 N18B 88.3(7) . . ? N13B Cu1 N13C 90.1(5) . . ? N16A Cu1 N13C 100.1(5) . . ? N13B Cu1 N16C 107.8(5) . . ? N16A Cu1 N16C 90.7(5) . . ? N13C Cu1 N16C 80.1(4) . . ? N13B Cu1 N16B 81.3(5) . . ? N16A Cu1 N16B 92.2(5) . . ? N13C Cu1 N16B 164.4(5) . . ? N16C Cu1 N16B 90.2(5) . . ? N18A Cu1 N19B 154.4(8) . . ? N18C Cu1 N19B 121.6(8) . . ? N18B Cu1 N19B 76.4(8) . . ? N18A Cu1 N19A 81.7(7) . . ? N18C Cu1 N19A 137.6(7) . . ? N18B Cu1 N19A 130.4(6) . . ? N19B Cu1 N19A 88.6(8) . . ? N18A Cu1 N19C 109.6(7) . . ? N18C Cu1 N19C 75.5(6) . . ? N18B Cu1 N19C 149.8(6) . . ? N19B Cu1 N19C 90.4(7) . . ? N19A Cu1 N19C 75.2(6) . . ? N13B Cu1 N13A 86.8(5) . . ? N16A Cu1 N13A 78.0(5) . . ? N13C Cu1 N13A 81.9(5) . . ? N16C Cu1 N13A 156.7(6) . . ? N16B Cu1 N13A 110.3(5) . . ? N28A Cu2 N29B 158.8(7) . . ? N26B Cu2 N26A 84.9(6) . . ? N28A Cu2 N29C 118.9(8) . . ? N29B Cu2 N29C 78.4(7) . . ? N26B Cu2 N23B 84.3(6) . . ? N26A Cu2 N23B 162.2(6) . . ? N28A Cu2 N29A 77.7(7) . . ? N29B Cu2 N29A 90.2(7) . . ? N29C Cu2 N29A 92.0(6) . . ? N26B Cu2 N23C 161.5(7) . . ? N26A Cu2 N23C 107.8(5) . . ? N23B Cu2 N23C 86.3(5) . . ? N26B Cu2 N23A 108.9(6) . . ? N26A Cu2 N23A 83.6(5) . . ? N23B Cu2 N23A 86.5(6) . . ? N23C Cu2 N23A 86.3(6) . . ? N28A Cu2 N28C 88.8(7) . . ? N29B Cu2 N28C 107.8(7) . . ? N29C Cu2 N28C 78.1(6) . . ? N29A Cu2 N28C 156.9(7) . . ? N28A Cu2 N28B 91.0(7) . . ? N29B Cu2 N28B 77.4(6) . . ? N29C Cu2 N28B 145.4(8) . . ? N29A Cu2 N28B 112.3(7) . . ? N28C Cu2 N28B 86.2(6) . . ? N26B Cu2 N26C 87.3(6) . . ? N26A Cu2 N26C 89.2(5) . . ? N23B Cu2 N26C 104.4(6) . . ? N23C Cu2 N26C 79.6(5) . . ? N23A Cu2 N26C 161.5(5) . . ? C12 N10 C11 116.9(10) . . ? C12 N10 H10 121.6 . . ? C11 N10 H10 121.5 . . ? C12B C11 C12A 118.0(10) . . ? C12B C11 N10 101.0(9) . . ? C12A C11 N10 110.7(7) . . ? C12B C11 C12C 108.0(9) . . ? C12A C11 C12C 110.5(10) . . ? N10 C11 C12C 107.9(9) . . ? N10 C12 C13 118.1(13) . . ? N10 C12 H12A 107.9 . . ? C13 C12 H12A 107.8 . . ? N10 C12 H12B 107.8 . . ? C13 C12 H12B 107.7 . . ? H12A C12 H12B 107.1 . . ? C12 C13 C14 122.4(11) . . ? C12 C13 H13A 106.7 . . ? C14 C13 H13A 106.7 . . ? C12 C13 H13B 106.8 . . ? C14 C13 H13B 106.7 . . ? H13A C13 H13B 106.6 . . ? C13 C14 C15 114.4(12) . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C14 117.8(13) . . ? C16 C15 H15A 107.9 . . ? C14 C15 H15A 107.9 . . ? C16 C15 H15B 107.9 . . ? C14 C15 H15B 107.8 . . ? H15A C15 H15B 107.2 . . ? C15 C16 C17 115.3(12) . . ? C15 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C16 C17 C18 116.3(12) . . ? C16 C17 H17A 108.2 . . ? C18 C17 H17A 108.2 . . ? C16 C17 H17B 108.2 . . ? C18 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C19 C18 C17 114.8(12) . . ? C19 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? C19 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? C18 C19 C110 114.9(12) . . ? C18 C19 H19A 108.6 . . ? C110 C19 H19A 108.6 . . ? C18 C19 H19B 108.5 . . ? C110 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C110 C111 115.4(12) . . ? C19 C110 H11A 108.4 . . ? C111 C110 H11A 108.4 . . ? C19 C110 H11B 108.4 . . ? C111 C110 H11B 108.4 . . ? H11A C110 H11B 107.5 . . ? C110 C111 C112 114.2(11) . . ? C110 C111 H11C 108.7 . . ? C112 C111 H11C 108.7 . . ? C110 C111 H11D 108.7 . . ? C112 C111 H11D 108.7 . . ? H11C C111 H11D 107.6 . . ? C113 C112 C111 114.0(12) . . ? C113 C112 H11E 108.7 . . ? C111 C112 H11E 108.8 . . ? C113 C112 H11F 108.7 . . ? C111 C112 H11F 108.7 . . ? H11E C112 H11F 107.6 . . ? C112 C113 C114 116.4(13) . . ? C112 C113 H11G 108.2 . . ? C114 C113 H11G 108.2 . . ? C112 C113 H11H 108.2 . . ? C114 C113 H11H 108.1 . . ? H11G C113 H11H 107.4 . . ? C113 C114 H11I 109.5 . . ? C113 C114 H11J 109.5 . . ? H11I C114 H11J 109.5 . . ? C113 C114 H11K 109.4 . . ? H11I C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? N13A C12A C11 117.2(10) . . ? C11 C12A N18A 105.0(10) . . ? N13A C12A H12C 107.9 . . ? C11 C12A H12C 108 . . ? N13A C12A H12D 108.1 . . ? C11 C12A H12D 108 . . ? H12C C12A H12D 107.2 . . ? C11 C12A H12I 113.6 . . ? N18A C12A H12I 110 . . ? C11 C12A H12J 108.5 . . ? N18A C12A H12J 111.7 . . ? H12I C12A H12J 108.1 . . ? C14A N13A C12A 121.9(13) . . ? C14A N13A Cu1 105.0(8) . . ? C12A N13A Cu1 110.1(8) . . ? C14A N13A H13C 106.3 . . ? C12A N13A H13C 106.2 . . ? Cu1 N13A H13C 106.3 . . ? C12A N18A C14A 102.6(11) . . ? C12A N18A Cu1 118.3(14) . . ? C14A N18A Cu1 108.0(10) . . ? C12A N18A H18C 109.2 . . ? C14A N18A H18C 109.2 . . ? Cu1 N18A H18C 109.2 . . ? N13A C14A C15A 117.6(11) . . ? C15A C14A N18A 110.9(9) . . ? N13A C14A H14C 107.9 . . ? C15A C14A H14C 107.9 . . ? N13A C14A H14D 107.9 . . ? C15A C14A H14D 107.9 . . ? H14C C14A H14D 107.2 . . ? C15A C14A H14I 108.6 . . ? N18A C14A H14I 106.2 . . ? C15A C14A H14J 108.6 . . ? N18A C14A H14J 114.8 . . ? H14I C14A H14J 107.5 . . ? N19A C15A C14A 123.7(11) . . ? N16A C15A C14A 107.2(9) . . ? N19A C15A H15C 108.7 . . ? N16A C15A H15C 110.3 . . ? C14A C15A H15C 110.3 . . ? N16A C15A H15D 110.3 . . ? C14A C15A H15D 110.3 . . ? H15C C15A H15D 108.5 . . ? C14A C15A H15I 107.4 . . ? N19A C15A H15J 113.2 . . ? C14A C15A H15J 107.4 . . ? H15I C15A H15J 107 . . ? C15A N16A C17A 109.6(9) . . ? C15A N16A Cu1 113.5(8) . . ? C17A N16A Cu1 112.0(8) . . ? C15A N16A H16C 107.1 . . ? C17A N16A H16C 107.1 . . ? Cu1 N16A H16C 107.1 . . ? C17A N19A C15A 137.7(15) . . ? C17A N19A Cu1 116.4(12) . . ? C15A N19A Cu1 102.4(9) . . ? C17A N19A H19C 96 . . ? C15A N19A H19C 95.9 . . ? Cu1 N19A H19C 96 . . ? N19A C17A C11' 122.0(12) . . ? C11' C17A N16A 116.2(8) . . ? N19A C17A H17C 113.4 . . ? C11' C17A H17C 108.2 . . ? N16A C17A H17C 108.3 . . ? C11' C17A H17D 108.2 . . ? N16A C17A H17D 108.2 . . ? H17C C17A H17D 107.4 . . ? N19A C17A H17I 109.5 . . ? C11' C17A H17I 104.8 . . ? N19A C17A H17J 101.3 . . ? C11' C17A H17J 111.3 . . ? H17I C17A H17J 107.3 . . ? C11 C12B N13B 116.1(10) . . ? C11 C12B N18B 117.8(11) . . ? C11 C12B H12E 108.3 . . ? N13B C12B H12E 108.3 . . ? C11 C12B H12F 108.2 . . ? N13B C12B H12F 108.2 . . ? H12E C12B H12F 107.4 . . ? C11 C12B H12K 112.5 . . ? N18B C12B H12K 112.7 . . ? C11 C12B H12L 104.7 . . ? N18B C12B H12L 100.4 . . ? H12K C12B H12L 107.1 . . ? C12B N13B C14B 116.7(11) . . ? C12B N13B Cu1 119.2(9) . . ? C14B N13B Cu1 107.2(7) . . ? C12B N13B H13D 103.9 . . ? C14B N13B H13D 103.9 . . ? Cu1 N13B H13D 103.9 . . ? C14B N18B C12B 119.2(14) . . ? C14B N18B Cu1 112.6(9) . . ? C12B N18B Cu1 106.5(10) . . ? C14B N18B H18D 105.8 . . ? C12B N18B H18D 105.9 . . ? Cu1 N18B H18D 105.8 . . ? N18B C14B C15B 117.2(10) . . ? N13B C14B C15B 115.5(8) . . ? N13B C14B H14E 108.4 . . ? C15B C14B H14E 108.4 . . ? N13B C14B H14F 108.4 . . ? C15B C14B H14F 108.4 . . ? H14E C14B H14F 107.5 . . ? N18B C14B H14K 112.7 . . ? C15B C14B H14K 106.7 . . ? N18B C14B H14L 103 . . ? C15B C14B H14L 109.2 . . ? H14K C14B H14L 107.8 . . ? N19B C15B C14B 114.3(13) . . ? N16B C15B C14B 106.4(8) . . ? N19B C15B H15E 127.1 . . ? N16B C15B H15E 110.5 . . ? C14B C15B H15E 110.5 . . ? N16B C15B H15F 110.4 . . ? C14B C15B H15F 110.4 . . ? H15E C15B H15F 108.7 . . ? N19B C15B H15K 118.2 . . ? C14B C15B H15K 110.4 . . ? C14B C15B H15L 106.5 . . ? H15K C15B H15L 107.2 . . ? C15B N16B C17B 109.7(9) . . ? C15B N16B Cu1 111.5(9) . . ? C17B N16B Cu1 108.2(8) . . ? C17B N16B H15L 109.9 . . ? C15B N16B H16D 109.1 . . ? C17B N16B H16D 109.2 . . ? Cu1 N16B H16D 109.1 . . ? C15B N19B C17B 126(2) . . ? C15B N19B Cu1 114.2(13) . . ? C17B N19B Cu1 117.1(18) . . ? C15B N19B H19D 95 . . ? C17B N19B H19D 94.9 . . ? Cu1 N19B H19D 95 . . ? C11' C17B N19B 116.1(14) . . ? C11' C17B N16B 116.9(9) . . ? C11' C17B H17E 108.1 . . ? N16B C17B H17E 108 . . ? C11' C17B H17F 108.1 . . ? N16B C17B H17F 108.1 . . ? H17E C17B H17F 107.3 . . ? C11' C17B H17K 108.9 . . ? N19B C17B H17K 113.2 . . ? C11' C17B H17L 110.8 . . ? H17K C17B H17L 108 . . ? N18C C12C C11 108.1(11) . . ? N13C C12C C11 108.2(9) . . ? N18C C12C H12G 110.1 . . ? C11 C12C H12G 110.1 . . ? N18C C12C H12H 110 . . ? C11 C12C H12H 110 . . ? H12G C12C H12H 108.4 . . ? N13C C12C H12M 112.4 . . ? C11 C12C H12M 111.5 . . ? N13C C12C H12N 108.7 . . ? C11 C12C H12N 107.4 . . ? H12M C12C H12N 108.4 . . ? C14C N18C C12C 108.0(13) . . ? C14C N18C Cu1 115.2(10) . . ? C12C N18C Cu1 119.3(10) . . ? C14C N18C H12N 105.2 . . ? C14C N18C H18E 104.2 . . ? C12C N18C H18E 104.2 . . ? Cu1 N18C H18E 104.2 . . ? C12C N18C H14M 107.8 . . ? C14C N13C C12C 98.0(9) . . ? C14C N13C Cu1 108.3(7) . . ? C12C N13C Cu1 112.4(9) . . ? C14C N13C H13E 112.4 . . ? C12C N13C H13E 112.5 . . ? Cu1 N13C H13E 112.4 . . ? C15C C14C N18C 111.8(10) . . ? C15C C14C N13C 107.4(8) . . ? C15C C14C H14G 109.2 . . ? N18C C14C H14G 109.3 . . ? C15C C14C H14H 109.3 . . ? N18C C14C H14H 109.3 . . ? H14G C14C H14H 107.9 . . ? C15C C14C H14M 110.3 . . ? N13C C14C H14M 107.1 . . ? C15C C14C H14N 110.7 . . ? N13C C14C H14N 112.6 . . ? H14M C14C H14N 108.6 . . ? N19C C15C C14C 117.8(9) . . ? C14C C15C N16C 110.0(9) . . ? C14C C15C H15G 109.6 . . ? N16C C15C H15G 109.6 . . ? C14C C15C H15H 109.7 . . ? N16C C15C H15H 109.7 . . ? H15G C15C H15H 108.2 . . ? N19C C15C H15M 105.7 . . ? C14C C15C H15M 108.6 . . ? N19C C15C H15N 108.3 . . ? C14C C15C H15N 108.4 . . ? N16C C15C H15N 138.3 . . ? H15M C15C H15N 107.6 . . ? C15C N16C C17C 107.1(10) . . ? C15C N16C Cu1 110.1(7) . . ? C17C N16C Cu1 112.4(7) . . ? C15C N16C H16E 109 . . ? C17C N16C H16E 109.1 . . ? Cu1 N16C H16E 109.1 . . ? C15C N19C C17C 122.8(11) . . ? C15C N19C Cu1 113.5(9) . . ? C17C N19C Cu1 110.0(9) . . ? C15C N19C H19E 102.5 . . ? C17C N19C H19E 102.4 . . ? Cu1 N19C H19E 102.5 . . ? N19C C17C C11' 116.7(8) . . ? N16C C17C C11' 113.2(8) . . ? N16C C17C H17G 109 . . ? C11' C17C H17G 109 . . ? N16C C17C H17H 108.9 . . ? C11' C17C H17H 108.9 . . ? H17G C17C H17H 107.8 . . ? N19C C17C H17M 105.7 . . ? C11' C17C H17M 108.1 . . ? N19C C17C H17N 109.2 . . ? C11' C17C H17N 109.3 . . ? H17M C17C H17N 107.6 . . ? C17A C11' C17B 115.2(8) . . ? C17A C11' C10' 111.1(8) . . ? C17B C11' C10' 103.0(8) . . ? C17A C11' C17C 108.4(7) . . ? C17B C11' C17C 113.0(8) . . ? C10' C11' C17C 105.8(7) . . ? C11' C10' H10A 109.5 . . ? C11' C10' H10B 109.5 . . ? H10A C10' H10B 109.5 . . ? C11' C10' H10C 109.5 . . ? H10A C10' H10C 109.5 . . ? H10B C10' H10C 109.5 . . ? C22 N20 C21 121.6(11) . . ? C22 N20 H20 119.2 . . ? C21 N20 H20 119.2 . . ? C22A C21 C22C 110.6(12) . . ? C22A C21 C22B 108.7(12) . . ? C22C C21 C22B 115.3(14) . . ? C22A C21 N20 113.1(11) . . ? C22C C21 N20 106.9(10) . . ? C22B C21 N20 102.1(10) . . ? N20 C22 C23 109.0(13) . . ? N20 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? N20 C22 H22B 109.8 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 C23 C22 117.6(11) . . ? C24 C23 H23A 108 . . ? C22 C23 H23A 107.9 . . ? C24 C23 H23B 107.8 . . ? C22 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? C23 C24 C25 117.3(12) . . ? C23 C24 H24A 107.9 . . ? C25 C24 H24A 107.9 . . ? C23 C24 H24B 108.1 . . ? C25 C24 H24B 108 . . ? H24A C24 H24B 107.2 . . ? C26 C25 C24 116.6(11) . . ? C26 C25 H25A 108.2 . . ? C24 C25 H25A 108.2 . . ? C26 C25 H25B 108.1 . . ? C24 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? C25 C26 C27 118.0(11) . . ? C25 C26 H26A 107.8 . . ? C27 C26 H26A 107.7 . . ? C25 C26 H26B 107.9 . . ? C27 C26 H26B 107.9 . . ? H26A C26 H26B 107.2 . . ? C28 C27 C26 119.9(12) . . ? C28 C27 H27A 107.5 . . ? C26 C27 H27A 107.5 . . ? C28 C27 H27B 107.2 . . ? C26 C27 H27B 107.2 . . ? H27A C27 H27B 106.9 . . ? C27 C28 C29 112.7(12) . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C210 C29 C28 115.6(12) . . ? C210 C29 H29A 108.4 . . ? C28 C29 H29A 108.5 . . ? C210 C29 H29B 108.4 . . ? C28 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C210 C211 118.7(13) . . ? C29 C210 H21A 107.6 . . ? C211 C210 H21A 107.6 . . ? C29 C210 H21B 107.7 . . ? C211 C210 H21B 107.6 . . ? H21A C210 H21B 107.1 . . ? C210 C211 C212 115.2(13) . . ? C210 C211 H21C 108.5 . . ? C212 C211 H21C 108.4 . . ? C210 C211 H21D 108.5 . . ? C212 C211 H21D 108.5 . . ? H21C C211 H21D 107.5 . . ? C211 C212 C213 113.4(12) . . ? C211 C212 H21E 108.8 . . ? C213 C212 H21E 108.8 . . ? C211 C212 H21F 108.9 . . ? C213 C212 H21F 109 . . ? H21E C212 H21F 107.7 . . ? C214 C213 C212 114.0(13) . . ? C214 C213 H21G 108.8 . . ? C212 C213 H21G 108.8 . . ? C214 C213 H21H 108.8 . . ? C212 C213 H21H 108.7 . . ? H21G C213 H21H 107.7 . . ? C213 C214 H21I 109.5 . . ? C213 C214 H21J 109.5 . . ? H21I C214 H21J 109.5 . . ? C213 C214 H21K 109.5 . . ? H21I C214 H21K 109.5 . . ? H21J C214 H21K 109.5 . . ? C21 C22A N28A 113.5(13) . . ? C21 C22A N23A 119.7(13) . . ? C21 C22A H22C 108.9 . . ? N28A C22A H22C 108.9 . . ? C21 C22A H22D 108.8 . . ? N28A C22A H22D 108.9 . . ? H22C C22A H22D 107.7 . . ? C21 C22A H22I 106.8 . . ? N23A C22A H22I 104.3 . . ? C21 C22A H22J 108.1 . . ? N23A C22A H22J 110.3 . . ? H22I C22A H22J 106.8 . . ? C24A N28A C22A 115.5(16) . . ? C24A N28A Cu2 113.6(11) . . ? C22A N28A Cu2 119.5(13) . . ? C24A N28A H28C 101.4 . . ? C22A N28A H28C 101.4 . . ? Cu2 N28A H28C 101.4 . . ? C24A N23A C22A 111.3(12) . . ? C24A N23A Cu2 104.2(8) . . ? C22A N23A Cu2 106.4(10) . . ? C24A N23A H23C 111.5 . . ? C22A N23A H23C 111.6 . . ? Cu2 N23A H23C 111.5 . . ? N28A C24A C25A 113.0(11) . . ? N23A C24A C25A 112.0(10) . . ? N28A C24A H24C 109 . . ? C25A C24A H24C 109 . . ? N28A C24A H24D 109 . . ? C25A C24A H24D 109 . . ? H24C C24A H24D 107.8 . . ? N23A C24A H24I 106.6 . . ? C25A C24A H24I 107.7 . . ? N23A C24A H24J 113.1 . . ? C25A C24A H24J 109.9 . . ? H24I C24A H24J 107.4 . . ? N29A C25A C24A 115.3(12) . . ? C24A C25A N26A 115.9(11) . . ? N29A C25A H25C 108.5 . . ? C24A C25A H25C 108.4 . . ? N29A C25A H25D 108.4 . . ? C24A C25A H25D 108.4 . . ? H25C C25A H25D 107.5 . . ? C24A C25A H25I 108.4 . . ? N26A C25A H25I 111.4 . . ? C24A C25A H25J 110.9 . . ? N26A C25A H25J 101.8 . . ? H25I C25A H25J 108 . . ? C25A N29A C27A 118.4(13) . . ? C25A N29A Cu2 113.3(13) . . ? C27A N29A Cu2 108.0(11) . . ? C25A N29A H29C 105.3 . . ? C27A N29A H29C 105.3 . . ? Cu2 N29A H29C 105.3 . . ? C27A N26A C25A 115.9(12) . . ? C27A N26A Cu2 123.0(11) . . ? C25A N26A Cu2 106.9(8) . . ? C27A N26A H26C 102.7 . . ? C25A N26A H26C 102.7 . . ? Cu2 N26A H26C 102.7 . . ? N26A C27A C21' 108.3(10) . . ? C21' C27A N29A 117.8(10) . . ? C21' C27A H27C 107.8 . . ? N29A C27A H27C 107.8 . . ? C21' C27A H27D 107.8 . . ? N29A C27A H27D 107.9 . . ? H27C C27A H27D 107.2 . . ? N26A C27A H27I 110.1 . . ? C21' C27A H27I 111.1 . . ? N26A C27A H27J 111.9 . . ? C21' C27A H27J 107.8 . . ? H27I C27A H27J 107.7 . . ? N23B C22B C21 109.6(10) . . ? C21 C22B N28B 123.0(12) . . ? N23B C22B H22E 109.8 . . ? C21 C22B H22E 109.7 . . ? N23B C22B H22F 109.7 . . ? C21 C22B H22F 109.8 . . ? H22E C22B H22F 108.2 . . ? C21 C22B H22K 103.7 . . ? N28B C22B H22K 105.6 . . ? C21 C22B H22L 110.6 . . ? N28B C22B H22L 105.9 . . ? H22K C22B H22L 107.1 . . ? C22B N23B C24B 109.3(11) . . ? C22B N23B Cu2 114.0(13) . . ? C24B N23B Cu2 98.9(8) . . ? C22B N23B H23D 111.3 . . ? C24B N23B H23D 111.3 . . ? Cu2 N23B H23D 111.3 . . ? C24B N28B Cu2 116.6(12) . . ? C22B N28B Cu2 103.4(10) . . ? C24B N28B H28D 104.4 . . ? C22B N28B H28D 104.3 . . ? Cu2 N28B H28D 104.4 . . ? N28B C24B C25B 111.3(12) . . ? C25B C24B N23B 117.2(9) . . ? C25B C24B H24E 108 . . ? N23B C24B H24E 108 . . ? C25B C24B H24F 108 . . ? N23B C24B H24F 108 . . ? H24E C24B H24F 107.2 . . ? N28B C24B H24K 112.3 . . ? C25B C24B H24K 112 . . ? N28B C24B H24L 105.4 . . ? C25B C24B H24L 107.9 . . ? H24K C24B H24L 107.5 . . ? N26B C25B C24B 112.3(13) . . ? C24B C25B N29B 116.8(11) . . ? N26B C25B H25E 109.2 . . ? C24B C25B H25E 109.1 . . ? N26B C25B H25F 109.2 . . ? C24B C25B H25F 109.2 . . ? C24B C25B H25K 110.3 . . ? N29B C25B H25K 111.1 . . ? C24B C25B H25L 104.4 . . ? N29B C25B H25L 106.4 . . ? H25K C25B H25L 107.2 . . ? C25B N26B C27B 110.1(13) . . ? C25B N26B Cu2 116.2(11) . . ? C27B N26B Cu2 113.2(8) . . ? C25B N26B H26D 105.5 . . ? C27B N26B H26D 105.5 . . ? Cu2 N26B H26D 105.5 . . ? C27B N29B C25B 114.3(11) . . ? C27B N29B Cu2 119.0(10) . . ? C25B N29B Cu2 103.6(9) . . ? C27B N29B H29D 106.4 . . ? C25B N29B H29D 106.4 . . ? Cu2 N29B H29D 106.4 . . ? N29B C27B C21' 112.8(9) . . ? C21' C27B N26B 113.7(10) . . ? C21' C27B H27E 108.8 . . ? N26B C27B H27E 108.8 . . ? C21' C27B H27F 108.8 . . ? N26B C27B H27F 108.8 . . ? H27E C27B H27F 107.7 . . ? N29B C27B H27K 108.7 . . ? C21' C27B H27K 108.9 . . ? N29B C27B H27L 112.1 . . ? C21' C27B H27L 106.7 . . ? H27K C27B H27L 107.4 . . ? C21 C22C N28C 111.7(12) . . ? C21 C22C N23C 113.4(10) . . ? C21 C22C H22G 109.3 . . ? N28C C22C H22G 109.3 . . ? C21 C22C H22H 109.3 . . ? N28C C22C H22H 109.2 . . ? H22G C22C H22H 107.9 . . ? C21 C22C H22M 108.8 . . ? N23C C22C H22M 106.5 . . ? C21 C22C H22N 111.1 . . ? N23C C22C H22N 108.3 . . ? H22M C22C H22N 108.6 . . ? C24C N28C C22C 104.2(12) . . ? C24C N28C Cu2 108.0(9) . . ? C22C N28C Cu2 108.6(11) . . ? C24C N28C H22N 107.4 . . ? C24C N28C H28E 111.9 . . ? C22C N28C H28E 111.9 . . ? Cu2 N28C H28E 111.9 . . ? C22C N28C H24M 110.1 . . ? C24C N23C C22C 102.1(10) . . ? C24C N23C Cu2 108.6(9) . . ? C22C N23C Cu2 106.9(8) . . ? C24C N23C H23E 112.9 . . ? C22C N23C H23E 112.8 . . ? Cu2 N23C H23E 112.9 . . ? C25C C24C N23C 109.3(9) . . ? C25C C24C N28C 108.1(10) . . ? C25C C24C H24G 110.1 . . ? N28C C24C H24G 110 . . ? C25C C24C H24H 110 . . ? N28C C24C H24H 110.1 . . ? H24G C24C H24H 108.4 . . ? C25C C24C H24M 106.3 . . ? N23C C24C H24M 109.2 . . ? C25C C24C H24N 113.7 . . ? N23C C24C H24N 109.6 . . ? N28C C24C H24N 138.1 . . ? H24M C24C H24N 108.6 . . ? N29C C25C C24C 117.2(11) . . ? N26C C25C C24C 117.2(8) . . ? N26C C25C H25G 108 . . ? C24C C25C H25G 108 . . ? N26C C25C H25H 108 . . ? C24C C25C H25H 108 . . ? H25G C25C H25H 107.2 . . ? N29C C25C H25M 107 . . ? C24C C25C H25M 111.9 . . ? N29C C25C H25N 108.4 . . ? C24C C25C H25N 104.5 . . ? H25M C25C H25N 107.4 . . ? C25C N26C C27C 110.2(10) . . ? C25C N26C Cu2 106.4(9) . . ? C27C N26C Cu2 107.2(8) . . ? C25C N26C H26E 111 . . ? C27C N26C H26E 110.9 . . ? Cu2 N26C H26E 111 . . ? C27C N29C C25C 121.4(16) . . ? C27C N29C Cu2 119.0(11) . . ? C25C N29C Cu2 112.2(9) . . ? C27C N29C H29E 99.2 . . ? C25C N29C H29E 99.1 . . ? Cu2 N29C H29E 99.2 . . ? N29C C27C C21' 115.2(11) . . ? C21' C27C N26C 115.7(8) . . ? C21' C27C H27G 108.4 . . ? N26C C27C H27G 108.4 . . ? C21' C27C H27H 108.3 . . ? N26C C27C H27H 108.3 . . ? H27G C27C H27H 107.4 . . ? N29C C27C H27M 112.6 . . ? C21' C27C H27M 107.3 . . ? N29C C27C H27N 105.6 . . ? C21' C27C H27N 108.5 . . ? H27M C27C H27N 107.2 . . ? C27B C21' C20' 109.5(10) . . ? C27B C21' C27C 109.9(9) . . ? C20' C21' C27C 107.9(8) . . ? C27B C21' C27A 110.3(8) . . ? C20' C21' C27A 105.0(10) . . ? C27C C21' C27A 114.1(10) . . ? C21' C20' H20A 109.5 . . ? C21' C20' H20B 109.5 . . ? H20A C20' H20B 109.5 . . ? C21' C20' H20C 109.4 . . ? H20A C20' H20C 109.5 . . ? H20B C20' H20C 109.5 . . ? O12 Cl1 O14 116.1(8) . . ? O12 Cl1 O11 116.7(7) . . ? O14 Cl1 O11 112.3(7) . . ? O12 Cl1 O13 105.7(6) . . ? O14 Cl1 O13 99.3(9) . . ? O11 Cl1 O13 103.8(7) . . ? O21 Cl2 O23 102.8(9) . . ? O21 Cl2 O22 115.7(7) . . ? O23 Cl2 O22 114.6(8) . . ? O21 Cl2 O24 111.8(10) . . ? O23 Cl2 O24 110.5(10) . . ? O22 Cl2 O24 101.7(10) . . ? O32 Cl3 O33 102.2(12) . . ? O32 Cl3 O31 112.8(11) . . ? O33 Cl3 O31 135.3(12) . . ? O32 Cl3 O34 88.7(10) . . ? O33 Cl3 O34 100.4(11) . . ? O31 Cl3 O34 107.1(10) . . ? O43 Cl4 O44 114.0(9) . . ? O43 Cl4 O42 118.4(10) . . ? O44 Cl4 O42 103.3(10) . . ? O43 Cl4 O41 106.9(11) . . ? O44 Cl4 O41 108.0(11) . . ? O42 Cl4 O41 105.6(10) . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_gk165a _database_code_depnum_ccdc_archive 'CCDC 738802' _audit_creation_date 2009-06-11T18:55:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H62 Cu N7, 3(Cl O4), 2(H2 O)' _chemical_formula_sum 'C28 H66 Cl3 Cu N7 O14' _chemical_formula_weight 894.77 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5910(10) _cell_length_b 8.6340(10) _cell_length_c 31.316(5) _cell_angle_alpha 95.803(10) _cell_angle_beta 91.411(10) _cell_angle_gamma 119.620(10) _cell_volume 2001.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 950 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.95 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type ; PX1 beamline 3BM at the Australian Synchrotron ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.766 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator diamond _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_unetI/netI 0.0801 _diffrn_reflns_number 29344 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.908 _diffrn_measured_fraction_theta_max 0.905 _reflns_number_total 6666 _reflns_number_gt 6468 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1328P)^2^+5.6985P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6666 _refine_ls_number_parameters 569 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2467 _refine_ls_wR_factor_gt 0.2458 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.175 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 Cu 0.22844(8) 0.39883(8) 0.643206(19) 0.0420(3) Uani 1 1 d . . . N0 N 0.3032(5) 0.4757(6) 0.79354(13) 0.0360(9) Uani 1 1 d . . . H0A H 0.1934 0.4512 0.8028 0.043 Uiso 1 1 calc R . . H0B H 0.382 0.5956 0.8023 0.043 Uiso 1 1 calc R . . C1 C 0.2838(6) 0.4486(7) 0.74506(15) 0.0361(10) Uani 1 1 d . B . C2 C 0.3658(6) 0.3696(7) 0.81687(16) 0.0388(10) Uani 1 1 d . . . H2A H 0.2819 0.2395 0.8085 0.047 Uiso 1 1 calc R . . H2B H 0.4862 0.3968 0.8084 0.047 Uiso 1 1 calc R . . C3 C 0.3748(8) 0.4144(8) 0.86434(17) 0.0472(12) Uani 1 1 d . . . H3A H 0.2619 0.4105 0.872 0.057 Uiso 1 1 calc R . . H3B H 0.4751 0.5381 0.8733 0.057 Uiso 1 1 calc R . . C4 C 0.4023(8) 0.2844(9) 0.88852(18) 0.0508(13) Uani 1 1 d . . . H4A H 0.3938 0.3118 0.9196 0.061 Uiso 1 1 calc R . . H4B H 0.3027 0.1612 0.8787 0.061 Uiso 1 1 calc R . . C5 C 0.5784(7) 0.2869(7) 0.88341(16) 0.0402(11) Uani 1 1 d . . . H5A H 0.6789 0.4065 0.8955 0.048 Uiso 1 1 calc R . . H5B H 0.5923 0.2677 0.8524 0.048 Uiso 1 1 calc R . . C6 C 0.5891(7) 0.1434(7) 0.90574(16) 0.0410(11) Uani 1 1 d . . . H6A H 0.5634 0.1567 0.9361 0.049 Uiso 1 1 calc R . . H6B H 0.4936 0.0241 0.8919 0.049 Uiso 1 1 calc R . . C7 C 0.7653(7) 0.1472(7) 0.90515(16) 0.0417(11) Uani 1 1 d . . . H7A H 0.8602 0.2628 0.9209 0.05 Uiso 1 1 calc R . . H7B H 0.7955 0.1415 0.8749 0.05 Uiso 1 1 calc R . . C8 C 0.7656(7) -0.0045(7) 0.92503(16) 0.0422(11) Uani 1 1 d . . . H8A H 0.7333 0.0002 0.9551 0.051 Uiso 1 1 calc R . . H8B H 0.6717 -0.12 0.909 0.051 Uiso 1 1 calc R . . C9 C 0.9407(7) -0.0008(7) 0.92522(16) 0.0423(11) Uani 1 1 d . . . H9A H 1.0339 0.1141 0.9416 0.051 Uiso 1 1 calc R . . H9B H 0.9738 -0.0029 0.8952 0.051 Uiso 1 1 calc R . . C10 C 0.9430(6) -0.1540(7) 0.94440(17) 0.0418(11) Uani 1 1 d . . . H10A H 0.9117 -0.1512 0.9746 0.05 Uiso 1 1 calc R . . H10B H 0.8492 -0.2691 0.9282 0.05 Uiso 1 1 calc R . . C11 C 1.1204(7) -0.1490(7) 0.94386(17) 0.0439(12) Uani 1 1 d . . . H11A H 1.214 -0.0323 0.9594 0.053 Uiso 1 1 calc R . . H11B H 1.1501 -0.1533 0.9136 0.053 Uiso 1 1 calc R . . C12 C 1.1306(6) -0.2976(7) 0.96341(17) 0.0422(11) Uani 1 1 d . . . H12A H 1.0999 -0.295 0.9936 0.051 Uiso 1 1 calc R . . H12B H 1.0396 -0.4148 0.9475 0.051 Uiso 1 1 calc R . . C13 C 1.3108(7) -0.2837(8) 0.96263(18) 0.0473(12) Uani 1 1 d . . . H13A H 1.4012 -0.167 0.9789 0.057 Uiso 1 1 calc R . . H13B H 1.3421 -0.2838 0.9324 0.057 Uiso 1 1 calc R . . C14 C 1.3235(8) -0.4305(8) 0.9811(2) 0.0505(13) Uani 1 1 d . . . H14A H 1.2904 -0.4336 1.0109 0.076 Uiso 1 1 calc R . . H14B H 1.447 -0.408 0.9807 0.076 Uiso 1 1 calc R . . H14C H 1.2415 -0.546 0.9639 0.076 Uiso 1 1 calc R . . C2A C 0.2107(6) 0.5690(7) 0.73268(16) 0.0379(10) Uani 1 1 d . . . H2A1 H 0.0821 0.5118 0.7381 0.045 Uiso 0.5 1 calc PR A 1 H2A2 H 0.275 0.6851 0.7517 0.045 Uiso 0.5 1 calc PR A 1 H2D1 H 0.1227 0.5648 0.753 0.045 Uiso 0.5 1 d PR A 2 H2D2 H 0.3114 0.6944 0.7354 0.045 Uiso 0.5 1 d PR A 2 N3A N 0.2273(12) 0.6036(12) 0.6890(3) 0.0332(16) Uani 0.5 1 d P B 1 H3A1 H 0.3409 0.7037 0.6891 0.04 Uiso 0.5 1 calc PR B 1 N3D N 0.1214(11) 0.5148(12) 0.6871(3) 0.0372(19) Uani 0.5 1 d P B 2 H3D H 0.0037 0.4252 0.6891 0.045 Uiso 0.5 1 calc PR B 2 C4A C 0.1088(8) 0.6527(8) 0.67084(19) 0.0483(13) Uani 1 1 d . . . H4A1 H 0.1544 0.7814 0.6809 0.058 Uiso 0.5 1 calc PR B 1 H4A2 H -0.0095 0.5836 0.6824 0.058 Uiso 0.5 1 calc PR B 1 H4D1 H 0.2205 0.768 0.6801 0.058 Uiso 0.5 1 d PR B 2 H4D2 H 0.0077 0.6613 0.683 0.058 Uiso 0.5 1 d PR B 2 C4A' C 0.0804(6) 0.6256(7) 0.62343(17) 0.0411(11) Uani 1 1 d . B . H4A3 H -0.031 0.6262 0.6149 0.049 Uiso 0.5 1 calc PR C 1 H4A4 H 0.1818 0.7272 0.612 0.049 Uiso 0.5 1 calc PR C 1 H4D3 H -0.0482 0.5391 0.6149 0.049 Uiso 0.5 1 d PR C 2 H4D4 H 0.1081 0.7411 0.6135 0.049 Uiso 0.5 1 d PR C 2 N3A' N 0.0669(12) 0.4641(12) 0.6047(3) 0.045(2) Uani 0.5 1 d P B 1 H3A' H -0.052 0.3739 0.6049 0.054 Uiso 0.5 1 calc PR B 1 N3D' N 0.1848(10) 0.5586(10) 0.6017(2) 0.0306(15) Uani 0.5 1 d P B 2 H3D' H 0.2968 0.6582 0.5998 0.037 Uiso 0.5 1 calc PR B 2 C2A' C 0.1124(8) 0.4741(9) 0.55718(19) 0.0518(13) Uani 1 1 d . . . H2A3 H 0.0032 0.4444 0.5389 0.062 Uiso 0.5 1 calc PR B 1 H2A4 H 0.2045 0.5993 0.5543 0.062 Uiso 0.5 1 calc PR B 1 H2D3 H 0.1451 0.5683 0.5381 0.062 Uiso 0.5 1 d PR B 2 H2D4 H -0.0203 0.4046 0.5563 0.062 Uiso 0.5 1 d PR B 2 C2B C 0.4730(6) 0.5094(7) 0.73004(15) 0.0369(10) Uani 1 1 d . . . H2B1 H 0.5451 0.6423 0.7348 0.044 Uiso 0.5 1 calc PR B 1 H2B2 H 0.5337 0.4621 0.7475 0.044 Uiso 0.5 1 calc PR B 1 H2E1 H 0.5621 0.618 0.7492 0.044 Uiso 0.5 1 d PR B 2 H2E2 H 0.5032 0.4137 0.7324 0.044 Uiso 0.5 1 d PR B 2 N3B N 0.4648(10) 0.4476(15) 0.6853(3) 0.0335(18) Uani 0.5 1 d P B 1 H3B1 H 0.4533 0.3346 0.6851 0.04 Uiso 0.5 1 calc PR B 1 N3E N 0.4844(10) 0.5490(14) 0.6848(3) 0.0315(18) Uani 0.5 1 d P B 2 H3E H 0.5125 0.6684 0.6868 0.038 Uiso 0.5 1 calc PR B 2 C4B C 0.6198(5) 0.5440(9) 0.66362(17) 0.0488(14) Uani 1 1 d . . . H4B1 H 0.707 0.5056 0.6712 0.059 Uiso 0.5 1 calc PR B 1 H4B2 H 0.6748 0.673 0.6748 0.059 Uiso 0.5 1 calc PR B 1 H4E1 H 0.6302 0.4412 0.6716 0.059 Uiso 0.5 1 d PR B 2 H4E2 H 0.7348 0.6549 0.6736 0.059 Uiso 0.5 1 d PR B 2 C4B' C 0.5945(5) 0.5255(7) 0.61642(16) 0.0380(11) Uani 1 1 d . B . H4B3 H 0.6983 0.6282 0.606 0.046 Uiso 0.5 1 calc PR D 1 H4B4 H 0.5924 0.4142 0.6041 0.046 Uiso 0.5 1 calc PR D 1 H4E3 H 0.6246 0.6441 0.608 0.046 Uiso 0.5 1 d PR D 2 H4E4 H 0.6807 0.4926 0.6039 0.046 Uiso 0.5 1 d PR D 2 N3B' N 0.4332(12) 0.5189(14) 0.6013(3) 0.0432(19) Uani 0.5 1 d P B 1 H3B' H 0.4586 0.6368 0.6012 0.052 Uiso 0.5 1 calc PR B 1 N3E' N 0.4165(9) 0.3977(12) 0.5975(2) 0.0323(16) Uani 0.5 1 d P B 2 H3E' H 0.4064 0.2848 0.5954 0.039 Uiso 0.5 1 calc PR B 2 C2B' C 0.3813(7) 0.4267(9) 0.55396(18) 0.0522(14) Uani 1 1 d . . . H2B3 H 0.4541 0.5155 0.5347 0.063 Uiso 0.5 1 calc PR B 1 H2B4 H 0.4103 0.3288 0.5506 0.063 Uiso 0.5 1 calc PR B 1 H2E3 H 0.4316 0.3728 0.5331 0.063 Uiso 0.5 1 d PR B 2 H2E4 H 0.445 0.5578 0.5527 0.063 Uiso 0.5 1 d PR B 2 C2C C 0.1515(6) 0.2495(7) 0.73032(17) 0.0410(11) Uani 1 1 d . . . H2C1 H 0.2151 0.181 0.7327 0.049 Uiso 0.5 1 calc PR B 1 H2C2 H 0.0544 0.2059 0.75 0.049 Uiso 0.5 1 calc PR B 1 H2F1 H 0.028 0.2241 0.735 0.049 Uiso 0.5 1 calc PR B 2 H2F2 H 0.179 0.1758 0.748 0.049 Uiso 0.5 1 calc PR B 2 N3C N 0.0746(11) 0.2140(10) 0.6881(3) 0.0342(17) Uani 0.5 1 d P B 1 H3C H -0.0269 0.2256 0.6906 0.041 Uiso 0.5 1 calc PR B 1 N3F N 0.1604(10) 0.1950(10) 0.6819(2) 0.0311(16) Uani 0.5 1 d P B 2 H3F H 0.2541 0.1702 0.6813 0.037 Uiso 0.5 1 calc PR B 2 C4C C 0.0076(7) 0.0350(6) 0.66566(19) 0.0457(12) Uani 1 1 d . . . H4C1 H -0.1117 -0.0444 0.6755 0.055 Uiso 0.5 1 calc PR B 1 H4C2 H 0.0888 -0.0086 0.6747 0.055 Uiso 0.5 1 calc PR B 1 H4F1 H -0.0997 0.034 0.6768 0.055 Uiso 0.5 1 calc PR B 2 H4F2 H 0.0147 -0.0669 0.6755 0.055 Uiso 0.5 1 calc PR B 2 C4C' C -0.0110(7) 0.0125(6) 0.61845(19) 0.0472(13) Uani 1 1 d . B . H4C3 H -0.0121 -0.0995 0.6073 0.057 Uiso 0.5 1 calc PR E 1 H4C4 H -0.1273 0.0003 0.6085 0.057 Uiso 0.5 1 calc PR E 1 H4F3 H 0.0703 -0.031 0.6081 0.057 Uiso 0.5 1 calc PR E 2 H4F4 H -0.1354 -0.0839 0.6088 0.057 Uiso 0.5 1 calc PR E 2 N3C' N 0.1261(12) 0.1549(12) 0.6018(3) 0.044(2) Uani 0.5 1 d P B 1 H3C' H 0.2197 0.1301 0.6001 0.053 Uiso 0.5 1 calc PR B 1 N3F' N 0.0244(10) 0.1642(10) 0.5973(3) 0.0328(16) Uani 0.5 1 d P B 2 H3F' H -0.0801 0.1714 0.597 0.039 Uiso 0.5 1 calc PR B 2 C2C' C 0.0699(8) 0.1628(8) 0.55421(18) 0.0507(13) Uani 1 1 d . . . H2C3 H 0.0842 0.0743 0.5345 0.061 Uiso 0.5 1 calc PR B 1 H2C4 H -0.0586 0.1284 0.5517 0.061 Uiso 0.5 1 calc PR B 1 H2F3 H -0.0422 0.0948 0.5349 0.061 Uiso 0.5 1 calc PR B 2 H2F4 H 0.138 0.0981 0.5505 0.061 Uiso 0.5 1 calc PR B 2 C1' C 0.1817(6) 0.3492(7) 0.54026(17) 0.0439(12) Uani 1 1 d . B . C0' C 0.1605(7) 0.3276(8) 0.49133(18) 0.0487(13) Uani 1 1 d . . . H0'1 H 0.2068 0.2503 0.4796 0.073 Uiso 1 1 calc R B . H0'2 H 0.228 0.4457 0.4814 0.073 Uiso 1 1 calc R . . H0'3 H 0.033 0.2729 0.4814 0.073 Uiso 1 1 calc R . . Cl1 Cl -0.03710(18) -0.18051(17) 0.79341(4) 0.0504(4) Uani 1 1 d . . . O11 O -0.0726(7) -0.2279(7) 0.74904(15) 0.0754(14) Uani 1 1 d . . . O12 O 0.1420(7) -0.1308(9) 0.8056(2) 0.100(2) Uani 1 1 d . . . O13 O -0.1564(7) -0.3286(6) 0.81441(18) 0.0755(14) Uani 1 1 d . . . O14 O -0.0655(7) -0.0326(6) 0.80575(16) 0.0721(13) Uani 1 1 d . . . Cl2 Cl 0.59978(17) 0.10883(19) 0.72279(6) 0.0456(5) Uani 0.878(5) 1 d P F 1 O21 O 0.6101(7) -0.0478(7) 0.7115(2) 0.0526(13) Uani 0.878(5) 1 d P F 1 O22 O 0.6097(9) 0.1451(8) 0.7687(2) 0.0800(18) Uani 0.878(5) 1 d P F 1 O23 O 0.4346(6) 0.0846(7) 0.7047(2) 0.0753(18) Uani 0.878(5) 1 d P F 1 O24 O 0.7460(5) 0.2569(6) 0.70673(18) 0.0575(13) Uani 0.878(5) 1 d P F 1 Cl2' Cl 0.5967(18) 0.1194(19) 0.6909(5) 0.069(5) Uiso 0.122(5) 1 d PD F 2 O22' O 0.748(3) 0.231(4) 0.6680(9) 0.056(8) Uiso 0.122(5) 1 d PD F 2 O21' O 0.433(3) 0.083(5) 0.6663(12) 0.095(11) Uiso 0.122(5) 1 d PD F 2 O23' O 0.591(5) -0.049(3) 0.6937(12) 0.060(15) Uiso 0.122(5) 1 d PD F 2 O24' O 0.608(5) 0.214(5) 0.7322(8) 0.095(11) Uiso 0.122(5) 1 d PD F 2 Cl3 Cl 0.5333(3) 0.0046(4) 0.57465(9) 0.0947(7) Uani 1 1 d D . . O31 O 0.5477(15) -0.0996(15) 0.5369(4) 0.145(4) Uani 0.878(5) 1 d P F 1 O32 O 0.5475(9) -0.0917(10) 0.6082(3) 0.103(3) Uani 0.878(5) 1 d P F 1 O33 O 0.3738(9) -0.0017(10) 0.5722(3) 0.099(2) Uani 0.878(5) 1 d P F 1 O34 O 0.6628(10) 0.1757(11) 0.5784(5) 0.159(6) Uani 0.878(5) 1 d P F 1 O31' O 0.437(5) 0.038(5) 0.6116(9) 0.078(12) Uiso 0.122(5) 1 d PD F 2 O32' O 0.697(3) 0.172(3) 0.5750(13) 0.077(10) Uiso 0.122(5) 1 d PD F 2 O33' O 0.545(3) -0.143(2) 0.5763(8) 0.030(6) Uiso 0.122(5) 1 d PD F 2 O34' O 0.413(4) -0.012(5) 0.5373(8) 0.077(10) Uiso 0.122(5) 1 d PD F 2 O1 O 0.5512(7) 0.8373(6) 0.81453(15) 0.0687(12) Uani 1 1 d . . . O2 O -0.0331(6) 0.4110(7) 0.81613(16) 0.0659(12) 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 Cu1 0.0351(4) 0.0367(4) 0.0517(4) 0.0109(3) 0.0049(2) 0.0150(3) N0 0.0273(18) 0.035(2) 0.050(2) 0.0185(17) 0.0128(15) 0.0161(16) C1 0.021(2) 0.036(3) 0.049(3) 0.0162(19) 0.0091(17) 0.0105(18) C2 0.035(2) 0.031(3) 0.054(3) 0.012(2) 0.0022(19) 0.019(2) C3 0.050(3) 0.048(3) 0.054(3) 0.018(2) 0.012(2) 0.030(3) C4 0.063(3) 0.056(3) 0.051(3) 0.024(2) 0.019(2) 0.040(3) C5 0.041(2) 0.030(2) 0.049(3) 0.0143(19) 0.0025(19) 0.015(2) C6 0.042(3) 0.030(2) 0.048(3) 0.0132(19) 0.006(2) 0.014(2) C7 0.038(2) 0.034(3) 0.047(3) 0.012(2) 0.0003(19) 0.012(2) C8 0.040(3) 0.037(3) 0.049(3) 0.012(2) 0.003(2) 0.017(2) C9 0.036(2) 0.036(3) 0.048(3) 0.013(2) 0.0017(19) 0.012(2) C10 0.034(2) 0.034(3) 0.057(3) 0.014(2) 0.003(2) 0.015(2) C11 0.041(3) 0.037(3) 0.055(3) 0.016(2) 0.007(2) 0.019(2) C12 0.036(2) 0.029(2) 0.058(3) 0.014(2) 0.003(2) 0.012(2) C13 0.041(3) 0.041(3) 0.060(3) 0.013(2) 0.007(2) 0.019(2) C14 0.050(3) 0.041(3) 0.070(4) 0.014(2) 0.006(2) 0.029(3) C2A 0.026(2) 0.034(3) 0.055(3) 0.018(2) 0.0094(18) 0.0138(19) N3A 0.024(4) 0.024(4) 0.056(5) 0.020(3) 0.005(3) 0.013(4) N3D 0.013(4) 0.030(4) 0.058(5) 0.024(3) 0.008(3) -0.001(4) C4A 0.050(3) 0.042(3) 0.068(3) 0.007(2) -0.001(2) 0.035(3) C4A' 0.026(2) 0.036(3) 0.068(3) 0.019(2) 0.005(2) 0.018(2) N3A' 0.024(4) 0.029(4) 0.067(6) 0.011(4) 0.005(3) 0.002(4) N3D' 0.022(4) 0.015(3) 0.049(4) 0.009(3) 0.001(3) 0.004(3) C2A' 0.053(3) 0.051(3) 0.058(3) 0.005(2) -0.006(2) 0.031(3) C2B 0.023(2) 0.037(3) 0.050(3) 0.016(2) 0.0105(17) 0.0124(18) N3B 0.019(4) 0.028(5) 0.052(5) 0.011(4) 0.010(3) 0.008(4) N3E 0.025(4) 0.021(4) 0.047(4) 0.012(4) 0.011(3) 0.008(4) C4B 0.0068(17) 0.071(4) 0.058(3) 0.020(3) 0.0045(17) 0.009(2) C4B' 0.0120(18) 0.038(3) 0.056(3) 0.010(2) 0.0064(17) 0.0054(17) N3B' 0.048(5) 0.031(5) 0.054(5) 0.011(4) -0.007(4) 0.022(4) N3E' 0.022(3) 0.025(4) 0.047(4) 0.010(3) -0.001(3) 0.008(3) C2B' 0.031(3) 0.058(4) 0.056(3) 0.014(2) -0.003(2) 0.013(2) C2C 0.027(2) 0.035(3) 0.059(3) 0.018(2) 0.0105(19) 0.0116(19) N3C 0.018(4) 0.024(4) 0.058(5) 0.012(3) 0.005(3) 0.007(3) N3F 0.011(3) 0.029(4) 0.050(4) 0.007(3) 0.003(3) 0.007(3) C4C 0.036(2) 0.014(2) 0.078(4) 0.017(2) 0.016(2) 0.0034(19) C4C' 0.032(2) 0.014(2) 0.081(4) 0.008(2) -0.010(2) 0.0004(18) N3C' 0.026(4) 0.041(5) 0.060(5) 0.009(4) 0.002(3) 0.012(4) N3F' 0.015(3) 0.026(4) 0.059(5) 0.010(3) 0.004(3) 0.011(3) C2C' 0.047(3) 0.038(3) 0.058(3) 0.006(2) 0.002(2) 0.015(2) C1' 0.027(2) 0.043(3) 0.054(3) 0.006(2) -0.002(2) 0.012(2) C0' 0.033(2) 0.049(3) 0.055(3) 0.006(2) -0.003(2) 0.014(2) Cl1 0.0493(7) 0.0327(7) 0.0528(7) 0.0068(5) 0.0070(5) 0.0078(5) O11 0.066(3) 0.078(3) 0.057(3) -0.001(2) 0.011(2) 0.019(3) O12 0.047(3) 0.092(4) 0.130(5) -0.010(4) -0.015(3) 0.017(3) O13 0.077(3) 0.049(3) 0.097(4) 0.031(2) 0.033(3) 0.024(2) O14 0.088(3) 0.046(3) 0.078(3) 0.017(2) 0.028(2) 0.027(2) Cl2 0.0278(7) 0.0278(8) 0.0828(12) 0.0173(6) 0.0169(6) 0.0127(6) O21 0.045(3) 0.043(3) 0.081(4) 0.017(2) 0.015(3) 0.028(2) O22 0.084(4) 0.055(3) 0.089(4) 0.012(3) 0.033(3) 0.025(3) O23 0.022(2) 0.044(3) 0.163(6) 0.026(3) 0.016(3) 0.0164(19) O24 0.0223(19) 0.038(3) 0.107(4) 0.029(2) 0.013(2) 0.0074(18) Cl3 0.0533(10) 0.0959(17) 0.1227(18) 0.0366(13) 0.0110(10) 0.0240(10) O31 0.145(9) 0.118(7) 0.193(11) 0.034(7) 0.067(7) 0.078(7) O32 0.060(4) 0.062(4) 0.181(8) 0.038(4) -0.008(4) 0.023(3) O33 0.072(4) 0.082(5) 0.169(7) 0.066(5) 0.039(4) 0.048(4) O34 0.061(4) 0.072(5) 0.383(17) 0.083(7) 0.085(7) 0.051(4) O1 0.089(3) 0.040(2) 0.070(3) 0.0063(19) 0.006(2) 0.027(2) O2 0.053(2) 0.076(3) 0.091(3) 0.049(2) 0.040(2) 0.042(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3F 2.088(8) . ? Cu1 N3D 2.105(9) . ? Cu1 N3C' 2.109(9) . ? Cu1 N3B' 2.116(9) . ? Cu1 N3A' 2.127(10) . ? Cu1 N3D' 2.141(8) . ? Cu1 N3A 2.165(8) . ? Cu1 N3C 2.174(8) . ? Cu1 N3E' 2.188(8) . ? Cu1 N3E 2.216(8) . ? Cu1 N3B 2.225(9) . ? Cu1 N3F' 2.240(8) . ? N0 C1 1.505(6) . ? N0 C2 1.505(6) . ? N0 H0A 0.92 . ? N0 H0B 0.92 . ? C1 C2A 1.530(7) . ? C1 C2C 1.530(7) . ? C1 C2B 1.544(6) . ? C2 C3 1.488(7) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.521(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.515(8) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.522(7) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.499(7) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.507(7) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.489(7) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.516(8) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.503(7) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.515(7) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.494(7) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.495(8) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C2A N3A 1.426(9) . ? C2A N3D 1.516(10) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C2A H2D1 0.99 . ? C2A H2D2 0.99 . ? N3A C4A 1.410(9) . ? N3A H3A1 0.93 . ? N3D C4A 1.392(10) . ? N3D H3D 0.93 . ? C4A C4A' 1.474(8) . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? C4A H4D1 0.99 . ? C4A H4D2 0.99 . ? C4A' N3A' 1.403(11) . ? C4A' N3D' 1.436(9) . ? C4A' H4A3 0.99 . ? C4A' H4A4 0.99 . ? C4A' H4D3 0.99 . ? C4A' H4D4 0.99 . ? N3A' C2A' 1.549(11) . ? N3A' H3A' 0.93 . ? N3D' C2A' 1.471(9) . ? N3D' H3D' 0.93 . ? C2A' C1' 1.527(8) . ? C2A' H2A3 0.99 . ? C2A' H2A4 0.99 . ? C2A' H2D3 0.99 . ? C2A' H2D4 0.99 . ? C2B N3B 1.436(10) . ? C2B N3E 1.485(9) . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C2B H2E1 0.99 . ? C2B H2E2 0.99 . ? N3B C4B 1.410(9) . ? N3B H3B1 0.93 . ? N3E C4B 1.370(9) . ? N3E H3E 0.93 . ? C4B C4B' 1.469(7) . ? C4B H4B1 0.99 . ? C4B H4B2 0.99 . ? C4B H4E1 0.99 . ? C4B H4E2 0.99 . ? C4B' N3B' 1.426(10) . ? C4B' N3E' 1.436(8) . ? C4B' H4B3 0.99 . ? C4B' H4B4 0.99 . ? C4B' H4E3 0.99 . ? C4B' H4E4 0.99 . ? N3B' C2B' 1.552(11) . ? N3B' H3B' 0.93 . ? N3E' C2B' 1.461(9) . ? N3E' H3E' 0.93 . ? C2B' C1' 1.531(7) . ? C2B' H2B3 0.99 . ? C2B' H2B4 0.99 . ? C2B' H2E3 0.99 . ? C2B' H2E4 0.99 . ? C2C N3C 1.399(10) . ? C2C N3F 1.556(9) . ? C2C H2C1 0.99 . ? C2C H2C2 0.99 . ? C2C H2F1 0.99 . ? C2C H2F2 0.99 . ? N3C C4C 1.447(10) . ? N3C H3C 0.93 . ? N3F C4C 1.387(9) . ? N3F H3F 0.93 . ? C4C C4C' 1.466(8) . ? C4C H4C1 0.99 . ? C4C H4C2 0.99 . ? C4C H4F1 0.99 . ? C4C H4F2 0.99 . ? C4C' N3C' 1.378(10) . ? C4C' N3F' 1.427(10) . ? C4C' H4C3 0.99 . ? C4C' H4C4 0.99 . ? C4C' H4F3 0.99 . ? C4C' H4F4 0.99 . ? N3C' C2C' 1.574(11) . ? N3C' H3C' 0.93 . ? N3F' C2C' 1.416(10) . ? N3F' H3F' 0.93 . ? C2C' C1' 1.529(8) . ? C2C' H2C3 0.99 . ? C2C' H2C4 0.99 . ? C2C' H2F3 0.99 . ? C2C' H2F4 0.99 . ? C1' C0' 1.520(7) . ? C0' H0'1 0.98 . ? C0' H0'2 0.98 . ? C0' H0'3 0.98 . ? Cl1 O11 1.390(5) . ? Cl1 O12 1.408(6) . ? Cl1 O13 1.423(5) . ? Cl1 O14 1.432(5) . ? Cl2 O21 1.409(5) . ? Cl2 O23 1.421(5) . ? Cl2 O24 1.428(4) . ? Cl2 O22 1.431(6) . ? Cl2' O24' 1.432(16) . ? Cl2' O23' 1.438(17) . ? Cl2' O22' 1.443(16) . ? Cl2' O21' 1.460(17) . ? Cl3 O34 1.329(9) . ? Cl3 O33' 1.338(14) . ? Cl3 O33 1.344(7) . ? Cl3 O32' 1.432(16) . ? Cl3 O32 1.443(8) . ? Cl3 O31 1.456(11) . ? Cl3 O34' 1.490(15) . ? Cl3 O31' 1.523(16) . ? 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 N3F Cu1 N3D 88.7(3) . . ? N3C' Cu1 N3B' 88.2(4) . . ? N3C' Cu1 N3A' 88.2(4) . . ? N3B' Cu1 N3A' 88.0(3) . . ? N3F Cu1 N3D' 157.2(3) . . ? N3D Cu1 N3D' 81.4(3) . . ? N3C' Cu1 N3A 158.4(4) . . ? N3B' Cu1 N3A 110.1(4) . . ? N3A' Cu1 N3A 81.5(3) . . ? N3C' Cu1 N3C 81.1(3) . . ? N3B' Cu1 N3C 156.6(4) . . ? N3A' Cu1 N3C 112.2(3) . . ? N3A Cu1 N3C 85.4(3) . . ? N3F Cu1 N3E' 110.3(3) . . ? N3D Cu1 N3E' 156.0(4) . . ? N3D' Cu1 N3E' 85.4(3) . . ? N3F Cu1 N3E 86.0(3) . . ? N3D Cu1 N3E 87.4(3) . . ? N3D' Cu1 N3E 113.8(3) . . ? N3E' Cu1 N3E 79.7(3) . . ? N3C' Cu1 N3B 110.6(4) . . ? N3B' Cu1 N3B 80.2(3) . . ? N3A' Cu1 N3B 157.3(4) . . ? N3A Cu1 N3B 84.4(3) . . ? N3C Cu1 N3B 84.1(3) . . ? N3F Cu1 N3F' 80.6(3) . . ? N3D Cu1 N3F' 115.0(3) . . ? N3D' Cu1 N3F' 85.0(3) . . ? N3E' Cu1 N3F' 83.5(3) . . ? N3E Cu1 N3F' 153.4(4) . . ? C1 N0 C2 119.0(4) . . ? C1 N0 H0A 107.6 . . ? C2 N0 H0A 107.6 . . ? C1 N0 H0B 107.6 . . ? C2 N0 H0B 107.6 . . ? H0A N0 H0B 107 . . ? N0 C1 C2A 104.8(4) . . ? N0 C1 C2C 107.7(4) . . ? C2A C1 C2C 112.1(4) . . ? N0 C1 C2B 107.0(4) . . ? C2A C1 C2B 112.0(4) . . ? C2C C1 C2B 112.6(4) . . ? C3 C2 N0 110.7(4) . . ? C3 C2 H2A 109.5 . . ? N0 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? N0 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 111.7(5) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 115.8(5) . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? C3 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 112.4(4) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 115.5(4) . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 113.5(4) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 114.0(4) . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 114.9(4) . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C9 114.1(4) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 116.2(4) . . ? C10 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? C10 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C11 113.7(4) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 114.7(5) . . ? C12 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? C12 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3A C2A C1 114.6(5) . . ? N3D C2A C1 112.8(5) . . ? N3A C2A H2A1 108.6 . . ? C1 C2A H2A1 108.6 . . ? N3A C2A H2A2 108.6 . . ? C1 C2A H2A2 108.6 . . ? H2A1 C2A H2A2 107.6 . . ? N3D C2A H2D1 109.1 . . ? C1 C2A H2D1 109.3 . . ? N3D C2A H2D2 108.9 . . ? C1 C2A H2D2 108.7 . . ? H2D1 C2A H2D2 107.9 . . ? C4A N3A C2A 117.3(7) . . ? C4A N3A Cu1 107.4(5) . . ? C2A N3A Cu1 116.2(5) . . ? C4A N3A H3A1 104.8 . . ? C2A N3A H3A1 104.8 . . ? Cu1 N3A H3A1 104.8 . . ? C4A N3D C2A 112.7(7) . . ? C4A N3D Cu1 111.3(5) . . ? C2A N3D Cu1 115.1(5) . . ? C4A N3D H3D 105.6 . . ? C2A N3D H3D 105.6 . . ? Cu1 N3D H3D 105.6 . . ? N3D C4A C4A' 112.8(6) . . ? N3A C4A C4A' 116.7(5) . . ? N3A C4A H4A1 108.1 . . ? C4A' C4A H4A1 108.1 . . ? N3A C4A H4A2 108.1 . . ? C4A' C4A H4A2 108.1 . . ? H4A1 C4A H4A2 107.3 . . ? N3D C4A H4D1 109.1 . . ? N3D C4A H4D2 109.1 . . ? H4D1 C4A H4D2 107.8 . . ? N3A' C4A' C4A 113.1(5) . . ? N3D' C4A' C4A 114.8(5) . . ? N3A' C4A' H4A3 109 . . ? C4A C4A' H4A3 109 . . ? N3A' C4A' H4A4 109 . . ? C4A C4A' H4A4 109 . . ? H4A3 C4A' H4A4 107.8 . . ? N3D' C4A' H4D3 108.1 . . ? C4A C4A' H4D3 108.5 . . ? N3D' C4A' H4D4 109.1 . . ? C4A C4A' H4D4 108.6 . . ? H4D3 C4A' H4D4 107.5 . . ? C4A' N3A' C2A' 110.9(7) . . ? C4A' N3A' Cu1 109.6(5) . . ? C2A' N3A' Cu1 113.3(5) . . ? C4A' N3A' H3A' 107.6 . . ? C2A' N3A' H3A' 107.6 . . ? Cu1 N3A' H3A' 107.6 . . ? C4A' N3D' C2A' 113.7(6) . . ? C4A' N3D' Cu1 107.5(5) . . ? C2A' N3D' Cu1 116.2(5) . . ? C4A' N3D' H3D' 106.2 . . ? C2A' N3D' H3D' 106.2 . . ? Cu1 N3D' H3D' 106.2 . . ? N3D' C2A' C1' 112.5(5) . . ? C1' C2A' N3A' 114.5(6) . . ? C1' C2A' H2A3 108.6 . . ? N3A' C2A' H2A3 108.6 . . ? C1' C2A' H2A4 108.6 . . ? N3A' C2A' H2A4 108.6 . . ? H2A3 C2A' H2A4 107.6 . . ? N3D' C2A' H2D3 109.6 . . ? C1' C2A' H2D3 109 . . ? N3D' C2A' H2D4 108.6 . . ? C1' C2A' H2D4 109.2 . . ? H2D3 C2A' H2D4 107.8 . . ? N3B C2B C1 111.6(5) . . ? N3E C2B C1 111.9(5) . . ? N3B C2B H2B1 109.3 . . ? C1 C2B H2B1 109.3 . . ? N3B C2B H2B2 109.3 . . ? C1 C2B H2B2 109.3 . . ? H2B1 C2B H2B2 108 . . ? N3E C2B H2E1 109.5 . . ? C1 C2B H2E1 109.1 . . ? N3E C2B H2E2 109 . . ? C1 C2B H2E2 109.3 . . ? H2E1 C2B H2E2 107.9 . . ? C4B N3B C2B 117.0(7) . . ? C4B N3B Cu1 107.8(5) . . ? C2B N3B Cu1 117.2(5) . . ? C4B N3B H3B1 104.4 . . ? C2B N3B H3B1 104.4 . . ? Cu1 N3B H3B1 104.4 . . ? C4B N3E C2B 116.4(7) . . ? C4B N3E Cu1 109.8(5) . . ? C2B N3E Cu1 115.3(5) . . ? C4B N3E H3E 104.6 . . ? C2B N3E H3E 104.6 . . ? Cu1 N3E H3E 104.6 . . ? N3E C4B C4B' 114.8(5) . . ? N3B C4B C4B' 116.8(5) . . ? N3B C4B H4B1 108.1 . . ? C4B' C4B H4B1 108.1 . . ? N3B C4B H4B2 108.1 . . ? C4B' C4B H4B2 108.1 . . ? H4B1 C4B H4B2 107.3 . . ? N3E C4B H4E1 108.3 . . ? C4B' C4B H4E1 108.3 . . ? N3E C4B H4E2 109 . . ? C4B' C4B H4E2 108.6 . . ? H4E1 C4B H4E2 107.6 . . ? N3B' C4B' C4B 113.2(5) . . ? N3E' C4B' C4B 115.6(4) . . ? N3B' C4B' H4B3 108.9 . . ? C4B C4B' H4B3 108.9 . . ? N3B' C4B' H4B4 108.9 . . ? C4B C4B' H4B4 108.9 . . ? H4B3 C4B' H4B4 107.7 . . ? N3E' C4B' H4E3 107.5 . . ? C4B C4B' H4E3 108.2 . . ? N3E' C4B' H4E4 109 . . ? C4B C4B' H4E4 108.7 . . ? H4E3 C4B' H4E4 107.5 . . ? C4B' N3B' C2B' 108.6(7) . . ? C4B' N3B' Cu1 111.3(5) . . ? C2B' N3B' Cu1 114.4(5) . . ? C4B' N3B' H3B' 107.4 . . ? C2B' N3B' H3B' 107.4 . . ? Cu1 N3B' H3B' 107.4 . . ? C4B' N3E' C2B' 113.2(6) . . ? C4B' N3E' Cu1 107.2(5) . . ? C2B' N3E' Cu1 114.7(5) . . ? C4B' N3E' H3E' 107.1 . . ? C2B' N3E' H3E' 107.1 . . ? Cu1 N3E' H3E' 107.1 . . ? N3E' C2B' C1' 113.9(5) . . ? C1' C2B' N3B' 112.5(5) . . ? C1' C2B' H2B3 109.1 . . ? N3B' C2B' H2B3 109.1 . . ? C1' C2B' H2B4 109.1 . . ? N3B' C2B' H2B4 109.1 . . ? H2B3 C2B' H2B4 107.8 . . ? N3E' C2B' H2E3 109.4 . . ? C1' C2B' H2E3 108.8 . . ? N3E' C2B' H2E4 108.2 . . ? C1' C2B' H2E4 108.7 . . ? H2E3 C2B' H2E4 107.7 . . ? N3C C2C C1 113.9(5) . . ? C1 C2C N3F 112.1(4) . . ? N3C C2C H2C1 108.8 . . ? C1 C2C H2C1 108.8 . . ? N3C C2C H2C2 108.8 . . ? C1 C2C H2C2 108.8 . . ? H2C1 C2C H2C2 107.7 . . ? C1 C2C H2F1 109.2 . . ? N3F C2C H2F1 109.2 . . ? C1 C2C H2F2 109.2 . . ? N3F C2C H2F2 109.2 . . ? H2F1 C2C H2F2 107.9 . . ? C2C N3C C4C 117.4(7) . . ? C2C N3C Cu1 117.6(5) . . ? C4C N3C Cu1 106.3(5) . . ? C2C N3C H3C 104.7 . . ? C4C N3C H3C 104.7 . . ? Cu1 N3C H3C 104.7 . . ? C4C N3F C2C 111.4(6) . . ? C4C N3F Cu1 113.4(5) . . ? C2C N3F Cu1 114.7(5) . . ? C4C N3F H3F 105.5 . . ? C2C N3F H3F 105.5 . . ? Cu1 N3F H3F 105.5 . . ? N3F C4C C4C' 111.0(5) . . ? N3C C4C C4C' 117.6(5) . . ? N3C C4C H4C1 107.9 . . ? C4C' C4C H4C1 107.9 . . ? N3C C4C H4C2 107.9 . . ? C4C' C4C H4C2 107.9 . . ? H4C1 C4C H4C2 107.2 . . ? N3F C4C H4F1 109.4 . . ? C4C' C4C H4F1 109.4 . . ? N3F C4C H4F2 109.4 . . ? C4C' C4C H4F2 109.4 . . ? H4F1 C4C H4F2 108 . . ? N3C' C4C' C4C 112.3(5) . . ? N3F' C4C' C4C 118.5(5) . . ? N3C' C4C' H4C3 109.1 . . ? C4C C4C' H4C3 109.1 . . ? N3C' C4C' H4C4 109.1 . . ? C4C C4C' H4C4 109.1 . . ? H4C3 C4C' H4C4 107.9 . . ? N3F' C4C' H4F3 107.7 . . ? C4C C4C' H4F3 107.7 . . ? N3F' C4C' H4F4 107.7 . . ? C4C C4C' H4F4 107.7 . . ? H4F3 C4C' H4F4 107.1 . . ? C4C' N3C' C2C' 110.8(6) . . ? C4C' N3C' Cu1 112.5(6) . . ? C2C' N3C' Cu1 114.6(6) . . ? C4C' N3C' H3C' 106 . . ? C2C' N3C' H3C' 106 . . ? Cu1 N3C' H3C' 106 . . ? C2C' N3F' C4C' 117.7(6) . . ? C2C' N3F' Cu1 114.9(5) . . ? C4C' N3F' Cu1 103.7(5) . . ? C2C' N3F' H3F' 106.6 . . ? C4C' N3F' H3F' 106.6 . . ? Cu1 N3F' H3F' 106.6 . . ? N3F' C2C' C1' 114.4(5) . . ? C1' C2C' N3C' 112.6(5) . . ? C1' C2C' H2C3 109.1 . . ? N3C' C2C' H2C3 109.1 . . ? C1' C2C' H2C4 109.1 . . ? N3C' C2C' H2C4 109.1 . . ? H2C3 C2C' H2C4 107.8 . . ? N3F' C2C' H2F3 108.7 . . ? C1' C2C' H2F3 108.7 . . ? N3F' C2C' H2F4 108.7 . . ? C1' C2C' H2F4 108.7 . . ? H2F3 C2C' H2F4 107.6 . . ? C0' C1' C2A' 107.7(5) . . ? C0' C1' C2C' 107.6(4) . . ? C2A' C1' C2C' 111.0(5) . . ? C0' C1' C2B' 107.4(4) . . ? C2A' C1' C2B' 112.3(5) . . ? C2C' C1' C2B' 110.6(5) . . ? C1' C0' H0'1 109.5 . . ? C1' C0' H0'2 109.5 . . ? H0'1 C0' H0'2 109.5 . . ? C1' C0' H0'3 109.5 . . ? H0'1 C0' H0'3 109.5 . . ? H0'2 C0' H0'3 109.5 . . ? O11 Cl1 O12 110.0(4) . . ? O11 Cl1 O13 109.5(3) . . ? O12 Cl1 O13 109.8(4) . . ? O11 Cl1 O14 109.1(3) . . ? O12 Cl1 O14 109.6(4) . . ? O13 Cl1 O14 108.8(3) . . ? O21 Cl2 O23 109.8(4) . . ? O21 Cl2 O24 109.3(3) . . ? O23 Cl2 O24 109.5(3) . . ? O21 Cl2 O22 109.6(4) . . ? O23 Cl2 O22 109.3(4) . . ? O24 Cl2 O22 109.3(3) . . ? O24' Cl2' O23' 112.7(16) . . ? O24' Cl2' O22' 109.6(15) . . ? O23' Cl2' O22' 109.2(15) . . ? O24' Cl2' O21' 108.3(15) . . ? O23' Cl2' O21' 108.4(15) . . ? O22' Cl2' O21' 108.5(15) . . ? O34 Cl3 O33 108.5(5) . . ? O33' Cl3 O32' 117.7(15) . . ? O34 Cl3 O32 113.9(7) . . ? O33 Cl3 O32 112.0(5) . . ? O34 Cl3 O31 111.4(7) . . ? O33 Cl3 O31 110.6(7) . . ? O32 Cl3 O31 100.3(7) . . ? O33' Cl3 O34' 112.9(13) . . ? O32' Cl3 O34' 107.1(14) . . ? O33' Cl3 O31' 112.7(13) . . ? O32' Cl3 O31' 104.8(14) . . ? O34' Cl3 O31' 99.9(13) . . ? 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 N0 H0A O2 0.92 1.87 2.783(5) 173.8 . N0 H0B O1 0.92 1.85 2.768(6) 173.9 . N3A H3A1 O21 0.93 2.27 3.169(11) 162.4 1_565 N3D H3D O22' 0.93 2.03 2.91(3) 157.4 1_455 N3A' H3A' O34 0.93 2.25 3.135(12) 157.6 1_455 N3D' H3D' O33' 0.93 2.18 3.08(2) 163.6 1_565 N3B H3B1 O23 0.93 2.23 3.139(13) 163.9 . N3E H3E O23' 0.93 2.18 3.10(2) 177 1_565 N3B' H3B' O32 0.93 2.06 2.982(13) 170.9 1_565 N3E' H3E' O31' 0.93 2.37 3.27(3) 161.5 . N3C H3C O24 0.93 2.16 3.085(11) 171.5 1_455 N3F H3F O21' 0.93 2.06 2.98(3) 166.9 . N3C' H3C' O33 0.93 2.27 3.147(13) 156.8 . N3F' H3F' O32' 0.93 2.02 2.91(4) 160.9 1_455 #===END _publ_section_references ; Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_gk203 _database_code_depnum_ccdc_archive 'CCDC 738803' _audit_creation_date 2009-08-03T11:48:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H63 N7 Zn, 2(Cl O4)' _chemical_formula_sum 'C29 H63 Cl2 N7 O8 Zn' _chemical_formula_weight 774.13 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7770(10) _cell_length_b 8.8680(10) _cell_length_c 27.515(3) _cell_angle_alpha 93.830(3) _cell_angle_beta 94.964(3) _cell_angle_gamma 117.163(3) _cell_volume 1884.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9336 _cell_measurement_theta_min 2.927 _cell_measurement_theta_max 19.292 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.848 _diffrn_measurement_device_type ; Bruker 6000 CCD detector on beamline 15 at Advanced Photon Source, Argonne, Illinois, USA ; _diffrn_measurement_method '\p and \w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator diamond _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_number 28352 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 17.18 _diffrn_reflns_theta_full 17.18 _diffrn_measured_fraction_theta_full 0.958 _diffrn_measured_fraction_theta_max 0.958 _reflns_number_total 6365 _reflns_number_gt 6184 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_expression ? _refine_ls_extinction_coef 0 _refine_ls_number_reflns 6365 _refine_ls_number_parameters 467 _refine_ls_number_restraints 225 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.1170 _refine_ls_wR_factor_ref 0.3452 _refine_ls_wR_factor_gt 0.343 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 2.037 _refine_diff_density_min -1.431 _refine_diff_density_rms 0.239 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn1 Zn 0.62642(5) 0.80418(5) 0.836751(15) 0.03476(14) Uani 1 1 d . . . N0 N 0.4834(11) 0.3961(11) 0.7027(3) 0.0553(18) Uiso 0.5 1 d PDU A 1 H0 H 0.5362 0.3324 0.7041 0.066 Uiso 0.5 1 calc PR A 1 N0' N 0.3704(19) 0.407(2) 0.6897(6) 0.113(4) Uiso 0.5 1 d PDU A 2 H0' H 0.2582 0.3395 0.6861 0.135 Uiso 0.5 1 calc PR A 2 C1 C 0.5087(10) 0.5266(9) 0.7425(3) 0.0877(17) Uani 1 1 d U . . C2 C 0.3616(17) 0.3807(18) 0.6598(5) 0.075(3) Uiso 0.5 1 d PDU A 1 H2A H 0.386 0.4962 0.6519 0.09 Uiso 0.5 1 calc PR A 1 H2B H 0.2422 0.3235 0.6682 0.09 Uiso 0.5 1 calc PR A 1 C2' C 0.490(2) 0.449(2) 0.6526(6) 0.099(3) Uiso 0.5 1 d PDU A 2 H2'A H 0.6031 0.4568 0.6654 0.118 Uiso 0.5 1 calc PR A 2 H2'B H 0.5079 0.5539 0.6382 0.118 Uiso 0.5 1 calc PR A 2 C3 C 0.3751(10) 0.2802(9) 0.6154(3) 0.0930(18) Uani 1 1 d DU . . H3A H 0.4906 0.3465 0.6051 0.112 Uiso 0.5 1 calc PR A 1 H3B H 0.2887 0.2717 0.5882 0.112 Uiso 0.5 1 calc PR A 1 H3G H 0.2576 0.2704 0.6109 0.112 Uiso 0.5 1 d PR A 2 H3H H 0.4201 0.3072 0.5836 0.112 Uiso 0.5 1 d PR A 2 C4 C 0.3490(11) 0.0988(10) 0.6211(3) 0.092(2) Uani 1 1 d U A . H4A H 0.4514 0.1078 0.6419 0.111 Uiso 1 1 calc R . . H4B H 0.2477 0.0405 0.6387 0.111 Uiso 1 1 calc R . . C5 C 0.3217(10) -0.0114(8) 0.5733(2) 0.081(2) Uani 1 1 d U . . H5A H 0.2202 -0.0172 0.5529 0.098 Uiso 1 1 calc R A . H5B H 0.423 0.05 0.556 0.098 Uiso 1 1 calc R . . C6 C 0.2949(10) -0.1905(9) 0.5739(2) 0.084(2) Uani 1 1 d . A . H6A H 0.3924 -0.1875 0.5956 0.101 Uiso 1 1 calc R . . H6B H 0.1883 -0.2563 0.5886 0.101 Uiso 1 1 calc R . . C7 C 0.2808(10) -0.2832(8) 0.5259(2) 0.075(2) Uani 1 1 d . . . H7A H 0.3863 -0.2147 0.511 0.089 Uiso 1 1 calc R A . H7B H 0.1822 -0.2867 0.5045 0.089 Uiso 1 1 calc R . . C8 C 0.2568(9) -0.4663(8) 0.5240(2) 0.0727(19) Uani 1 1 d . A . H8A H 0.3564 -0.4636 0.5447 0.087 Uiso 1 1 calc R . . H8B H 0.152 -0.5355 0.5391 0.087 Uiso 1 1 calc R . . C9 C 0.2407(9) -0.5548(7) 0.4746(2) 0.075(2) Uani 1 1 d . . . H9A H 0.3462 -0.4874 0.4595 0.09 Uiso 1 1 calc R A . H9B H 0.1417 -0.5574 0.4537 0.09 Uiso 1 1 calc R . . C10 C 0.2152(10) -0.7348(8) 0.4745(2) 0.081(2) Uani 1 1 d . A . H10A H 0.1107 -0.8012 0.4901 0.098 Uiso 1 1 calc R . . H10B H 0.3149 -0.7315 0.4952 0.098 Uiso 1 1 calc R . . C11 C 0.1958(8) -0.8293(7) 0.4242(2) 0.0644(16) Uani 1 1 d . . . H11A H 0.0982 -0.83 0.4031 0.077 Uiso 1 1 calc R A . H11B H 0.3018 -0.7654 0.409 0.077 Uiso 1 1 calc R . . C12 C 0.1654(9) -1.0091(8) 0.4251(2) 0.0733(18) Uani 1 1 d U A . H12A H 0.0558 -1.0734 0.4387 0.088 Uiso 1 1 calc R . . H12B H 0.2591 -1.0077 0.4482 0.088 Uiso 1 1 calc R . . C13 C 0.1560(8) -1.1071(8) 0.3765(2) 0.0664(16) Uani 1 1 d U . . H13A H 0.064 -1.1065 0.3532 0.08 Uiso 1 1 calc R A . H13B H 0.2666 -1.0441 0.3633 0.08 Uiso 1 1 calc R . . C14 C 0.1230(10) -1.2833(9) 0.3773(2) 0.0802(18) Uani 1 1 d U A . H14A H 0.0167 -1.3429 0.3928 0.096 Uiso 1 1 calc R . . H14B H 0.2189 -1.2817 0.3995 0.096 Uiso 1 1 calc R . . C15 C 0.1025(9) -1.3894(9) 0.3312(3) 0.082(2) Uani 1 1 d U . . H15A H 0.0364 -1.3653 0.3051 0.123 Uiso 1 1 calc R A . H15B H 0.0409 -1.5103 0.3359 0.123 Uiso 1 1 calc R . . H15C H 0.2166 -1.363 0.3219 0.123 Uiso 1 1 calc R . . C2A C 0.3450(9) 0.4994(8) 0.7667(3) 0.0754(17) Uani 1 1 d U A . H2A1 H 0.2472 0.4702 0.7407 0.091 Uiso 0.5 1 calc PR B 1 H2A2 H 0.3128 0.4031 0.7866 0.091 Uiso 0.5 1 calc PR B 1 H2A5 H 0.2652 0.3753 0.7624 0.091 Uiso 0.5 1 d PR B 2 H2A6 H 0.2865 0.5548 0.7482 0.091 Uiso 0.5 1 d PR B 2 N3A N 0.3765(10) 0.6482(10) 0.7968(4) 0.0518(17) Uani 0.5 1 d PU A 1 H3A1 H 0.3507 0.7166 0.777 0.062 Uiso 0.5 1 calc PR A 1 N3D N 0.3734(10) 0.5678(10) 0.8173(3) 0.050(2) Uani 0.5 1 d P A 2 H3D H 0.3838 0.4865 0.8351 0.06 Uiso 0.5 1 calc PR A 2 C4A C 0.2462(7) 0.5970(7) 0.8370(2) 0.0638(14) Uani 1 1 d U . . H4A1 H 0.1354 0.589 0.8223 0.077 Uiso 0.5 1 calc PR A 1 H4A2 H 0.2229 0.4822 0.8454 0.077 Uiso 0.5 1 calc PR A 1 H4A5 H 0.1525 0.4875 0.8441 0.077 Uiso 0.5 1 d PR A 2 H4A6 H 0.1967 0.6403 0.8111 0.077 Uiso 0.5 1 d PR A 2 C4A' C 0.3058(7) 0.7121(9) 0.8812(3) 0.0779(17) Uani 1 1 d U A . H4A3 H 0.266 0.7993 0.8776 0.094 Uiso 0.5 1 calc PR C 1 H4A4 H 0.2515 0.6479 0.9084 0.094 Uiso 0.5 1 calc PR C 1 H4A7 H 0.2181 0.7518 0.8847 0.094 Uiso 0.5 1 d PR C 2 H4A8 H 0.3054 0.6483 0.9095 0.094 Uiso 0.5 1 d PR C 2 N3A' N 0.4799(10) 0.7931(13) 0.8940(4) 0.060(2) Uani 0.5 1 d PU A 1 H3A' H 0.4954 0.7147 0.9119 0.072 Uiso 0.5 1 calc PR A 1 N3D' N 0.4731(8) 0.8649(10) 0.8865(3) 0.042(2) Uani 0.5 1 d P A 2 H3D' H 0.449 0.9433 0.8712 0.051 Uiso 0.5 1 calc PR A 2 C2A' C 0.5549(6) 0.9496(8) 0.93206(19) 0.0588(14) Uani 1 1 d U . . H2A3 H 0.5341 0.911 0.9649 0.071 Uiso 0.5 1 calc PR A 1 H2A4 H 0.4914 1.0157 0.9257 0.071 Uiso 0.5 1 calc PR A 1 H2A7 H 0.5367 0.866 0.9559 0.071 Uiso 0.5 1 d PR A 2 H2A8 H 0.5009 1.0207 0.9427 0.071 Uiso 0.5 1 d PR A 2 C2B C 0.6347(10) 0.5006(9) 0.7739(3) 0.0869(17) Uani 1 1 d U A . H2B1 H 0.7462 0.5523 0.7605 0.104 Uiso 0.5 1 calc PR D 1 H2B2 H 0.5959 0.3764 0.7726 0.104 Uiso 0.5 1 calc PR D 1 H2B5 H 0.5773 0.4002 0.7918 0.104 Uiso 0.5 1 d PR D 2 H2B6 H 0.7145 0.4819 0.7539 0.104 Uiso 0.5 1 d PR D 2 N3B N 0.6664(12) 0.5793(12) 0.8306(4) 0.069(2) Uani 0.5 1 d PU A 1 H3B1 H 0.5836 0.4974 0.8466 0.083 Uiso 0.5 1 calc PR A 1 N3E N 0.7221(9) 0.6393(10) 0.8071(3) 0.0521(19) Uani 0.5 1 d P A 2 H3E H 0.8108 0.7114 0.7906 0.062 Uiso 0.5 1 calc PR A 2 C4B C 0.8225(7) 0.6079(8) 0.8524(3) 0.0826(16) Uani 1 1 d U . . H4B1 H 0.9086 0.6534 0.8292 0.099 Uiso 0.5 1 calc PR A 1 H4B2 H 0.8167 0.499 0.8611 0.099 Uiso 0.5 1 calc PR A 1 H4B5 H 0.7465 0.4934 0.8614 0.099 Uiso 0.5 1 d PR A 2 H4B6 H 0.9268 0.6049 0.8424 0.099 Uiso 0.5 1 d PR A 2 C4B' C 0.8751(7) 0.7260(8) 0.8954(3) 0.0841(16) Uani 1 1 d U A . H4B3 H 0.9987 0.7622 0.9061 0.101 Uiso 0.5 1 calc PR E 1 H4B4 H 0.8099 0.6647 0.9216 0.101 Uiso 0.5 1 calc PR E 1 H4B7 H 0.8841 0.6683 0.9243 0.101 Uiso 0.5 1 d PR E 2 H4B8 H 0.9914 0.8201 0.8934 0.101 Uiso 0.5 1 d PR E 2 N3B' N 0.8537(9) 0.8863(10) 0.8925(3) 0.0520(17) Uani 0.5 1 d PU A 1 H3B' H 0.9487 0.9648 0.8795 0.062 Uiso 0.5 1 calc PR A 1 N3E' N 0.7707(10) 0.7943(12) 0.9030(3) 0.056(2) Uani 0.5 1 d P A 2 H3E' H 0.687 0.7159 0.9196 0.067 Uiso 0.5 1 calc PR A 2 C2B' C 0.8500(6) 0.9640(8) 0.9384(2) 0.0622(15) Uani 1 1 d U . . H2B3 H 0.9699 1.0385 0.9542 0.075 Uiso 0.5 1 calc PR A 1 H2B4 H 0.7926 0.8747 0.9599 0.075 Uiso 0.5 1 calc PR A 1 H2B7 H 0.8543 0.9375 0.9728 0.075 Uiso 0.5 1 d PR A 2 H2B8 H 0.9704 1.0356 0.9324 0.075 Uiso 0.5 1 d PR A 2 C2C C 0.5928(11) 0.7118(10) 0.7250(2) 0.094(3) Uani 1 1 d U A . H2C1 H 0.4991 0.7378 0.7126 0.112 Uiso 0.5 1 calc PR F 1 H2C2 H 0.6578 0.7112 0.6974 0.112 Uiso 0.5 1 calc PR F 1 H2C5 H 0.5315 0.7059 0.6924 0.112 Uiso 0.5 1 d PR F 2 H2C6 H 0.7156 0.7484 0.7215 0.112 Uiso 0.5 1 d PR F 2 N3C N 0.7201(10) 0.8601(11) 0.7673(3) 0.0541(19) Uani 0.5 1 d PU A 1 H3C H 0.83 0.8685 0.7689 0.065 Uiso 0.5 1 calc PR A 1 N3F N 0.5760(15) 0.8563(12) 0.7630(3) 0.068(3) Uani 0.5 1 d P A 2 H3F H 0.4708 0.8576 0.7569 0.081 Uiso 0.5 1 calc PR A 2 C4C C 0.7259(8) 1.0176(7) 0.75426(18) 0.0610(14) Uani 1 1 d U . . H4C1 H 0.6095 0.9974 0.7403 0.073 Uiso 0.5 1 calc PR A 1 H4C2 H 0.8052 1.0633 0.7294 0.073 Uiso 0.5 1 calc PR A 1 H4C5 H 0.8225 0.9968 0.7456 0.073 Uiso 0.5 1 d PR A 2 H4C6 H 0.6918 1.067 0.7267 0.073 Uiso 0.5 1 d PR A 2 C4C' C 0.7900(9) 1.1444(7) 0.80092(18) 0.0642(15) Uani 1 1 d U A . H4C3 H 0.9147 1.1818 0.81 0.077 Uiso 0.5 1 calc PR G 1 H4C4 H 0.7774 1.2463 0.7936 0.077 Uiso 0.5 1 calc PR G 1 H4C7 H 0.9045 1.24 0.798 0.077 Uiso 0.5 1 d PR G 2 H4C8 H 0.7083 1.192 0.8037 0.077 Uiso 0.5 1 d PR G 2 N3C' N 0.7076(10) 1.0836(8) 0.8398(2) 0.0386(15) Uani 0.5 1 d PU A 1 H3C' H 0.6058 1.0922 0.8352 0.046 Uiso 0.5 1 calc PR A 1 N3F' N 0.8062(10) 1.0716(9) 0.8436(3) 0.0412(19) Uani 0.5 1 d P A 2 H3F' H 0.9164 1.0806 0.8473 0.049 Uiso 0.5 1 calc PR A 2 C2C' C 0.7935(6) 1.1735(6) 0.88990(16) 0.0484(12) Uani 1 1 d U . . H2C3 H 0.7643 1.2679 0.8961 0.058 Uiso 0.5 1 calc PR A 1 H2C4 H 0.9199 1.2259 0.8893 0.058 Uiso 0.5 1 calc PR A 1 H2C7 H 0.7061 1.2132 0.8829 0.058 Uiso 0.5 1 d PR A 2 H2C8 H 0.9074 1.2754 0.8987 0.058 Uiso 0.5 1 d PR A 2 C1' C 0.7530(7) 1.0716(7) 0.93343(17) 0.0546(15) Uani 1 1 d . A . C0' C 0.8119(12) 1.2051(12) 0.9798(2) 0.108(4) Uani 1 1 d . . . H0'1 H 0.7601 1.2813 0.9756 0.162 Uiso 1 1 calc R A . H0'2 H 0.9381 1.272 0.9844 0.162 Uiso 1 1 calc R . . H0'3 H 0.7747 1.1458 1.0088 0.162 Uiso 1 1 calc R . . Cl1 Cl 0.1850(3) 0.9498(2) 0.75673(8) 0.1011(6) Uani 1 1 d D . . O11 O 0.1307(9) 1.0467(9) 0.7299(3) 0.138(3) Uiso 1 1 d D H . O12 O 0.0828(15) 0.8500(16) 0.7892(4) 0.115(4) Uiso 0.5 1 d PD H 1 O13 O 0.3653(16) 1.012(3) 0.7635(8) 0.223(11) Uiso 0.5 1 d PD H 1 O14 O 0.140(3) 0.791(2) 0.7154(8) 0.44(3) Uiso 0.5 1 d PD H 1 O12' O 0.0864(16) 0.925(2) 0.7985(5) 0.144(6) Uiso 0.5 1 d PD H 2 O13' O 0.3627(13) 1.0761(14) 0.7894(4) 0.102(3) Uiso 0.5 1 d PD H 2 O14' O 0.2383(15) 0.8444(14) 0.7328(5) 0.120(4) Uiso 0.5 1 d PD H 2 Cl2 Cl 0.3315(3) 1.2743(4) 0.91972(12) 0.1973(13) Uani 1 1 d D . . O21 O 0.220(3) 1.212(3) 0.8731(6) 0.261(14) Uiso 0.5 1 d PD I 1 O22 O 0.4872(10) 1.4237(11) 0.9180(3) 0.075(2) Uiso 0.5 1 d PD I 1 O23 O 0.2387(15) 1.3876(16) 0.9445(5) 0.138(5) Uiso 0.5 1 d PD I 1 O24 O 0.3123(14) 1.1622(13) 0.9494(4) 0.104(3) Uiso 0.5 1 d PD I 1 O21' O 0.2003(11) 1.2543(12) 0.8853(3) 0.072(2) Uiso 0.5 1 d P I 2 O22' O 0.393(2) 1.278(2) 0.9711(5) 0.177(8) Uiso 0.5 1 d PD I 2 O23' O 0.238(2) 1.0611(16) 0.9114(6) 0.156(6) Uiso 0.5 1 d PD I 2 O24' O 0.4678(15) 1.2892(17) 0.8872(4) 0.117(4) Uiso 0.5 1 d PD I 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 Zn1 0.0357(2) 0.0358(2) 0.0395(3) 0.00522(19) 0.0079(2) 0.02177(18) C1 0.095(3) 0.067(3) 0.081(3) -0.013(2) 0.026(2) 0.021(2) C3 0.122(3) 0.088(3) 0.087(3) 0.023(3) 0.048(3) 0.056(3) C4 0.123(4) 0.084(3) 0.063(3) -0.009(3) 0.019(3) 0.044(3) C5 0.117(4) 0.073(3) 0.042(3) 0.002(2) 0.005(3) 0.036(3) C6 0.109(5) 0.076(4) 0.058(3) 0.009(3) 0.015(3) 0.035(4) C7 0.103(4) 0.055(3) 0.054(3) 0.006(2) 0.011(3) 0.027(3) C8 0.088(4) 0.064(3) 0.061(3) 0.005(3) 0.009(3) 0.032(3) C9 0.102(4) 0.046(3) 0.063(3) -0.001(2) 0.017(3) 0.021(3) C10 0.120(5) 0.065(3) 0.053(3) -0.002(3) 0.006(3) 0.040(3) C11 0.091(3) 0.057(3) 0.044(2) 0.003(2) 0.008(2) 0.034(2) C12 0.090(3) 0.058(3) 0.059(3) 0.004(2) 0.015(3) 0.022(3) C13 0.075(3) 0.064(2) 0.052(2) 0.003(2) 0.007(2) 0.025(2) C14 0.092(3) 0.072(3) 0.063(3) -0.001(2) 0.009(3) 0.028(3) C15 0.090(4) 0.075(3) 0.071(3) -0.004(3) 0.010(3) 0.032(3) C2A 0.079(3) 0.050(2) 0.079(3) -0.017(2) -0.005(3) 0.020(2) N3A 0.040(3) 0.042(3) 0.073(3) -0.004(3) -0.004(3) 0.022(2) N3D 0.043(4) 0.038(4) 0.059(5) -0.008(3) 0.004(3) 0.013(3) C4A 0.040(2) 0.051(2) 0.091(3) 0.007(2) 0.005(2) 0.0143(19) C4A' 0.0366(19) 0.069(3) 0.111(3) -0.016(3) 0.029(2) 0.009(2) N3A' 0.037(3) 0.065(4) 0.075(4) 0.001(3) 0.019(3) 0.020(3) N3D' 0.016(3) 0.040(4) 0.062(4) -0.005(3) 0.015(3) 0.005(3) C2A' 0.046(2) 0.076(3) 0.052(2) 0.004(2) 0.0199(19) 0.024(2) C2B 0.096(3) 0.058(3) 0.110(3) 0.001(3) 0.042(3) 0.035(2) N3B 0.063(3) 0.054(3) 0.103(4) 0.025(3) 0.021(3) 0.034(3) N3E 0.067(3) 0.055(3) 0.066(4) 0.019(3) 0.035(3) 0.049(3) C4B 0.063(2) 0.070(2) 0.139(4) 0.035(3) 0.021(3) 0.0478(18) C4B' 0.054(2) 0.069(2) 0.136(4) 0.037(2) -0.005(3) 0.0350(19) N3B' 0.027(3) 0.051(3) 0.081(4) 0.034(3) 0.010(3) 0.017(2) N3E' 0.046(3) 0.088(5) 0.047(4) 0.017(4) 0.006(3) 0.043(3) C2B' 0.037(2) 0.071(3) 0.063(3) 0.023(2) 0.001(2) 0.010(2) C2C 0.126(5) 0.088(4) 0.041(3) -0.012(3) 0.022(3) 0.028(4) N3C 0.050(3) 0.069(3) 0.052(4) -0.001(3) 0.007(3) 0.036(3) N3F 0.118(7) 0.056(4) 0.029(4) 0.010(3) 0.003(4) 0.040(5) C4C 0.077(3) 0.067(2) 0.0359(19) 0.0076(18) 0.015(2) 0.029(2) C4C' 0.092(3) 0.050(2) 0.039(2) 0.0123(18) 0.008(2) 0.023(2) N3C' 0.060(3) 0.034(2) 0.032(2) 0.003(2) 0.008(2) 0.029(2) N3F' 0.049(4) 0.031(3) 0.040(4) 0.004(3) 0.006(3) 0.015(3) C2C' 0.055(2) 0.042(2) 0.040(2) -0.0053(17) 0.0082(18) 0.0169(18) C1' 0.053(2) 0.063(3) 0.036(2) 0.004(2) 0.0098(19) 0.016(2) C0' 0.106(6) 0.117(6) 0.039(3) -0.017(3) 0.014(3) 0.002(5) Cl1 0.1240(13) 0.0702(8) 0.1214(13) 0.0524(8) 0.0428(11) 0.0459(8) Cl2 0.0739(13) 0.232(2) 0.232(2) 0.1745(17) -0.0015(14) 0.0095(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3A' 2.097(10) . ? Zn1 N3A 2.131(8) . ? Zn1 N3E 2.143(8) . ? Zn1 N3C 2.144(9) . ? Zn1 N3F' 2.150(7) . ? Zn1 N3E' 2.158(8) . ? Zn1 N3F 2.163(8) . ? Zn1 N3B 2.176(11) . ? Zn1 N3D' 2.204(8) . ? Zn1 N3B' 2.204(8) . ? Zn1 N3C' 2.237(7) . ? Zn1 N3D 2.237(7) . ? N0 C1 1.464(12) . ? N0 C2 1.476(16) . ? N0 H0 0.88 . ? N0' C2' 1.47(2) . ? N0' C1 1.737(16) . ? N0' H0' 0.88 . ? C1 C2B 1.455(13) . ? C1 C2A 1.561(11) . ? C1 C2C 1.592(11) . ? C2 C3 1.510(15) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C2' C3 1.594(16) . ? C2' H2'A 0.99 . ? C2' H2'B 0.99 . ? C3 C4 1.539(12) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C3 H3G 0.99 . ? C3 H3H 0.99 . ? C4 C5 1.516(9) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.497(11) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.473(9) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.536(10) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.487(8) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.507(10) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.524(8) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.494(9) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.519(8) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.455(10) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.475(9) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C2A N3A 1.408(11) . ? C2A N3D 1.436(10) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C2A H2A5 0.99 . ? C2A H2A6 0.99 . ? N3A C4A 1.598(11) . ? N3A H3A1 0.93 . ? N3D C4A 1.399(11) . ? N3D H3D 0.93 . ? C4A C4A' 1.425(9) . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? C4A H4A5 0.99 . ? C4A H4A6 0.99 . ? C4A' N3A' 1.359(10) . ? C4A' N3D' 1.461(8) . ? C4A' H4A3 0.99 . ? C4A' H4A4 0.99 . ? C4A' H4A7 0.99 . ? C4A' H4A8 0.99 . ? N3A' C2A' 1.519(11) . ? N3A' H3A' 0.93 . ? N3D' C2A' 1.369(9) . ? N3D' H3D' 0.93 . ? C2A' C1' 1.569(7) . ? C2A' H2A3 0.99 . ? C2A' H2A4 0.99 . ? C2A' H2A7 0.99 . ? C2A' H2A8 0.99 . ? C2B N3E 1.342(10) . ? C2B N3B 1.613(14) . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C2B H2B5 0.99 . ? C2B H2B6 0.99 . ? N3B C4B 1.349(12) . ? N3B H3B1 0.93 . ? N3E C4B 1.578(12) . ? N3E H3E 0.93 . ? C4B C4B' 1.418(11) . ? C4B H4B1 0.99 . ? C4B H4B2 0.99 . ? C4B H4B5 0.99 . ? C4B H4B6 0.99 . ? C4B' N3E' 1.331(12) . ? C4B' N3B' 1.523(11) . ? C4B' H4B3 0.99 . ? C4B' H4B4 0.99 . ? C4B' H4B7 0.99 . ? C4B' H4B8 0.99 . ? N3B' C2B' 1.409(11) . ? N3B' H3B' 0.93 . ? N3E' C2B' 1.559(11) . ? N3E' H3E' 0.93 . ? C2B' C1' 1.547(10) . ? C2B' H2B3 0.99 . ? C2B' H2B4 0.99 . ? C2B' H2B7 0.99 . ? C2B' H2B8 0.99 . ? C2C N3C 1.600(10) . ? C2C N3F 1.667(13) . ? C2C H2C1 0.99 . ? C2C H2C2 0.99 . ? C2C H2C5 0.9899 . ? C2C H2C6 0.99 . ? N3C C4C 1.445(12) . ? N3C H3C 0.93 . ? N3F C4C 1.489(11) . ? N3F H3F 0.93 . ? C4C C4C' 1.528(7) . ? C4C H4C1 0.99 . ? C4C H4C2 0.99 . ? C4C H4C5 0.99 . ? C4C H4C6 0.99 . ? C4C' N3C' 1.347(9) . ? C4C' N3F' 1.405(10) . ? C4C' H4C3 0.99 . ? C4C' H4C4 0.99 . ? C4C' H4C7 0.99 . ? C4C' H4C8 0.99 . ? N3C' C2C' 1.492(8) . ? N3C' H3C' 0.93 . ? N3F' C2C' 1.553(9) . ? N3F' H3F' 0.93 . ? C2C' C1' 1.517(7) . ? C2C' H2C3 0.99 . ? C2C' H2C4 0.99 . ? C2C' H2C7 0.99 . ? C2C' H2C8 0.99 . ? C1' C0' 1.557(9) . ? C0' H0'1 0.98 . ? C0' H0'2 0.98 . ? C0' H0'3 0.98 . ? Cl1 O14' 1.378(12) . ? Cl1 O11 1.381(8) . ? Cl1 O12 1.381(11) . ? Cl1 O13 1.407(13) . ? Cl1 O12' 1.466(12) . ? Cl1 O13' 1.587(10) . ? Cl1 O14 1.621(16) . ? Cl2 O24 1.289(11) . ? Cl2 O21' 1.363(10) . ? Cl2 O22 1.411(8) . ? Cl2 O21 1.450(14) . ? Cl2 O22' 1.462(14) . ? Cl2 O24' 1.519(12) . ? Cl2 O23' 1.671(13) . ? Cl2 O23 1.701(13) . ? 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 N3A' Zn1 N3A 81.9(4) . . ? N3A' Zn1 N3C 158.2(4) . . ? N3A Zn1 N3C 87.5(3) . . ? N3E Zn1 N3F' 114.5(3) . . ? N3E Zn1 N3E' 81.1(4) . . ? N3F' Zn1 N3E' 86.7(3) . . ? N3E Zn1 N3F 89.0(4) . . ? N3F' Zn1 N3F 80.6(3) . . ? N3E' Zn1 N3F 159.0(4) . . ? N3A' Zn1 N3B 109.6(5) . . ? N3A Zn1 N3B 87.0(4) . . ? N3C Zn1 N3B 88.6(4) . . ? N3E Zn1 N3D' 152.1(3) . . ? N3F' Zn1 N3D' 88.9(3) . . ? N3E' Zn1 N3D' 85.4(3) . . ? N3F Zn1 N3D' 110.8(4) . . ? N3A' Zn1 N3B' 88.4(4) . . ? N3A Zn1 N3B' 159.6(4) . . ? N3C Zn1 N3B' 107.1(3) . . ? N3B Zn1 N3B' 79.4(4) . . ? N3A' Zn1 N3C' 88.6(4) . . ? N3A Zn1 N3C' 113.2(3) . . ? N3C Zn1 N3C' 78.1(3) . . ? N3B Zn1 N3C' 154.9(3) . . ? N3D' Zn1 N3C' 71.9(3) . . ? N3B' Zn1 N3C' 84.2(3) . . ? N3E Zn1 N3D 81.9(3) . . ? N3F' Zn1 N3D 157.4(4) . . ? N3E' Zn1 N3D 112.1(4) . . ? N3F Zn1 N3D 84.5(4) . . ? N3D' Zn1 N3D 80.7(3) . . ? C1 N0 C2 114.1(10) . . ? C1 N0 H0 122.9 . . ? C2 N0 H0 122.9 . . ? C2' N0' C1 101.6(10) . . ? C2' N0' H0' 129.2 . . ? C1 N0' H0' 129.2 . . ? C2B C1 C2A 113.9(7) . . ? N0 C1 C2A 116.1(6) . . ? C2B C1 C2C 111.3(6) . . ? N0 C1 C2C 111.1(6) . . ? C2A C1 C2C 108.8(7) . . ? C2B C1 N0' 131.6(9) . . ? C2C C1 N0' 100.5(7) . . ? N0 C2 C3 111.8(11) . . ? N0 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N0 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N0' C2' C3 96.0(11) . . ? N0' C2' H2'A 112.5 . . ? C3 C2' H2'A 112.5 . . ? N0' C2' H2'B 112.5 . . ? C3 C2' H2'B 112.5 . . ? H2'A C2' H2'B 110.1 . . ? C2 C3 C4 117.1(8) . . ? C4 C3 C2' 126.9(10) . . ? C2 C3 H3A 108 . . ? C4 C3 H3A 108 . . ? C2 C3 H3B 108 . . ? C4 C3 H3B 108 . . ? H3A C3 H3B 107.3 . . ? C4 C3 H3G 105.6 . . ? C2' C3 H3G 106 . . ? C4 C3 H3H 105.9 . . ? C2' C3 H3H 105 . . ? H3G C3 H3H 106.1 . . ? C5 C4 C3 115.0(6) . . ? C5 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C6 C5 C4 120.3(6) . . ? C6 C5 H5A 107.3 . . ? C4 C5 H5A 107.3 . . ? C6 C5 H5B 107.3 . . ? C4 C5 H5B 107.3 . . ? H5A C5 H5B 106.9 . . ? C7 C6 C5 116.1(6) . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? C5 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 118.7(6) . . ? C6 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? C6 C7 H7B 107.6 . . ? C8 C7 H7B 107.6 . . ? H7A C7 H7B 107.1 . . ? C9 C8 C7 116.4(6) . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C7 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C10 114.5(6) . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 115.6(5) . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C10 114.5(5) . . ? C12 C11 H11A 108.6 . . ? C10 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 C13 117.2(5) . . ? C11 C12 H12A 108 . . ? C13 C12 H12A 108 . . ? C11 C12 H12B 108 . . ? C13 C12 H12B 108 . . ? H12A C12 H12B 107.2 . . ? C14 C13 C12 117.1(5) . . ? C14 C13 H13A 108 . . ? C12 C13 H13A 108 . . ? C14 C13 H13B 108 . . ? C12 C13 H13B 108 . . ? H13A C13 H13B 107.3 . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14A 107.3 . . ? C15 C14 H14A 107.3 . . ? C13 C14 H14B 107.3 . . ? C15 C14 H14B 107.3 . . ? H14A C14 H14B 106.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3A C2A C1 110.6(6) . . ? N3D C2A C1 116.6(6) . . ? N3A C2A H2A1 109.5 . . ? C1 C2A H2A1 109.5 . . ? N3A C2A H2A2 109.5 . . ? C1 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 108.1 . . ? N3D C2A H2A5 110.3 . . ? C1 C2A H2A5 107.6 . . ? N3D C2A H2A6 106.6 . . ? C1 C2A H2A6 108.2 . . ? H2A5 C2A H2A6 107.3 . . ? C2A N3A C4A 108.9(6) . . ? C2A N3A Zn1 119.8(6) . . ? C4A N3A Zn1 105.5(5) . . ? C2A N3A H3A1 107.3 . . ? C4A N3A H3A1 107.3 . . ? Zn1 N3A H3A1 107.3 . . ? C4A N3D C2A 119.5(7) . . ? C4A N3D Zn1 108.2(5) . . ? C2A N3D Zn1 112.3(5) . . ? C4A N3D H3D 105.2 . . ? C2A N3D H3D 105.2 . . ? Zn1 N3D H3D 105.2 . . ? C4A' C4A N3A 114.9(5) . . ? C4A' C4A H4A1 108.5 . . ? N3A C4A H4A1 108.5 . . ? C4A' C4A H4A2 108.5 . . ? N3A C4A H4A2 108.5 . . ? H4A1 C4A H4A2 107.5 . . ? N3D C4A H4A5 109.5 . . ? C4A' C4A H4A5 107.6 . . ? N3D C4A H4A6 106.6 . . ? C4A' C4A H4A6 110.5 . . ? H4A5 C4A H4A6 107.6 . . ? N3A' C4A' C4A 114.9(7) . . ? C4A C4A' N3D' 119.9(6) . . ? N3A' C4A' H4A3 108.5 . . ? C4A C4A' H4A3 108.5 . . ? N3A' C4A' H4A4 108.5 . . ? C4A C4A' H4A4 108.5 . . ? H4A3 C4A' H4A4 107.5 . . ? C4A C4A' H4A7 106 . . ? N3D' C4A' H4A7 106.6 . . ? C4A C4A' H4A8 109 . . ? N3D' C4A' H4A8 107.7 . . ? H4A7 C4A' H4A8 106.9 . . ? C4A' N3A' C2A' 117.2(8) . . ? C4A' N3A' Zn1 115.7(7) . . ? C2A' N3A' Zn1 116.0(5) . . ? C4A' N3A' H3A' 101.2 . . ? C2A' N3A' H3A' 101.2 . . ? Zn1 N3A' H3A' 101.2 . . ? C2A' N3D' C4A' 120.6(7) . . ? C2A' N3D' Zn1 117.3(5) . . ? C4A' N3D' Zn1 105.5(5) . . ? C2A' N3D' H3D' 103.7 . . ? C4A' N3D' H3D' 103.7 . . ? Zn1 N3D' H3D' 103.7 . . ? N3D' C2A' C1' 114.0(5) . . ? N3A' C2A' C1' 115.3(5) . . ? N3A' C2A' H2A3 108.4 . . ? C1' C2A' H2A3 108.4 . . ? N3A' C2A' H2A4 108.4 . . ? C1' C2A' H2A4 108.4 . . ? H2A3 C2A' H2A4 107.5 . . ? N3D' C2A' H2A7 109.6 . . ? C1' C2A' H2A7 110 . . ? N3D' C2A' H2A8 108.1 . . ? C1' C2A' H2A8 107.3 . . ? H2A7 C2A' H2A8 107.6 . . ? N3E C2B C1 108.3(7) . . ? C1 C2B N3B 114.9(7) . . ? C1 C2B H2B1 108.6 . . ? N3B C2B H2B1 108.6 . . ? C1 C2B H2B2 108.6 . . ? N3B C2B H2B2 108.6 . . ? H2B1 C2B H2B2 107.5 . . ? N3E C2B H2B5 108.2 . . ? C1 C2B H2B5 111.1 . . ? N3E C2B H2B6 110.5 . . ? C1 C2B H2B6 110.2 . . ? H2B5 C2B H2B6 108.5 . . ? C4B N3B C2B 110.7(9) . . ? C4B N3B Zn1 113.4(6) . . ? C2B N3B Zn1 110.7(7) . . ? C4B N3B H3B1 107.2 . . ? C2B N3B H3B1 107.2 . . ? Zn1 N3B H3B1 107.2 . . ? C2B N3B H4B5 108.8 . . ? C2B N3E C4B 113.3(7) . . ? C2B N3E Zn1 126.6(6) . . ? C4B N3E Zn1 105.5(5) . . ? C2B N3E H3E 102.8 . . ? C4B N3E H3E 102.8 . . ? Zn1 N3E H3E 102.8 . . ? N3B C4B C4B' 110.6(7) . . ? C4B' C4B N3E 117.2(6) . . ? N3B C4B H4B1 109.5 . . ? C4B' C4B H4B1 109.5 . . ? N3B C4B H4B2 109.5 . . ? C4B' C4B H4B2 109.5 . . ? H4B1 C4B H4B2 108.1 . . ? C4B' C4B H4B5 107.6 . . ? N3E C4B H4B5 107.5 . . ? C4B' C4B H4B6 107.6 . . ? N3E C4B H4B6 109.4 . . ? H4B5 C4B H4B6 107.1 . . ? N3E' C4B' C4B 114.8(6) . . ? C4B C4B' N3B' 118.0(7) . . ? C4B C4B' H4B3 107.8 . . ? N3B' C4B' H4B3 107.8 . . ? C4B C4B' H4B4 107.8 . . ? N3B' C4B' H4B4 107.8 . . ? H4B3 C4B' H4B4 107.1 . . ? N3E' C4B' H4B7 108.4 . . ? C4B C4B' H4B7 109 . . ? N3E' C4B' H4B8 108 . . ? C4B C4B' H4B8 108.8 . . ? H4B7 C4B' H4B8 107.7 . . ? C2B' N3B' C4B' 113.9(7) . . ? C2B' N3B' Zn1 117.1(5) . . ? C4B' N3B' Zn1 103.8(5) . . ? C2B' N3B' H3B' 107.2 . . ? C4B' N3B' H3B' 107.2 . . ? Zn1 N3B' H3B' 107.2 . . ? C4B' N3E' C2B' 116.3(6) . . ? C4B' N3E' Zn1 114.1(6) . . ? C2B' N3E' Zn1 112.5(6) . . ? C4B' N3E' H3E' 104.1 . . ? C2B' N3E' H3E' 104.1 . . ? Zn1 N3E' H3E' 104.1 . . ? N3B' C2B' C1' 111.9(5) . . ? C1' C2B' N3E' 115.1(5) . . ? N3B' C2B' H2B3 109.2 . . ? C1' C2B' H2B3 109.2 . . ? N3B' C2B' H2B4 109.2 . . ? C1' C2B' H2B4 109.2 . . ? H2B3 C2B' H2B4 107.9 . . ? C1' C2B' H2B7 108.5 . . ? N3E' C2B' H2B7 109 . . ? C1' C2B' H2B8 107.8 . . ? N3E' C2B' H2B8 108.8 . . ? H2B7 C2B' H2B8 107.4 . . ? C1 C2C N3C 113.9(6) . . ? C1 C2C N3F 112.8(6) . . ? C1 C2C H2C1 108.8 . . ? N3C C2C H2C1 108.8 . . ? C1 C2C H2C2 108.8 . . ? N3C C2C H2C2 108.8 . . ? H2C1 C2C H2C2 107.7 . . ? C1 C2C H2C5 108.5 . . ? N3F C2C H2C5 107.5 . . ? C1 C2C H2C6 109.7 . . ? N3F C2C H2C6 110.1 . . ? H2C5 C2C H2C6 108.1 . . ? C4C N3C C2C 107.2(7) . . ? C4C N3C Zn1 111.0(6) . . ? C2C N3C Zn1 109.9(5) . . ? C4C N3C H3C 109.6 . . ? C2C N3C H3C 109.6 . . ? Zn1 N3C H3C 109.6 . . ? C2C N3C H4C5 108.1 . . ? C4C N3F C2C 101.9(7) . . ? C4C N3F Zn1 108.1(5) . . ? C2C N3F Zn1 106.4(6) . . ? C4C N3F H3F 113.2 . . ? C2C N3F H3F 113.2 . . ? Zn1 N3F H3F 113.2 . . ? N3C C4C C4C' 107.7(5) . . ? N3F C4C C4C' 109.4(5) . . ? N3C C4C H4C1 110.2 . . ? C4C' C4C H4C1 110.2 . . ? N3C C4C H4C2 110.2 . . ? C4C' C4C H4C2 110.2 . . ? H4C1 C4C H4C2 108.5 . . ? N3F C4C H4C5 111.1 . . ? C4C' C4C H4C5 108.2 . . ? N3F C4C H4C6 110.1 . . ? C4C' C4C H4C6 110 . . ? H4C5 C4C H4C6 108 . . ? N3C' C4C' C4C 114.9(5) . . ? N3F' C4C' C4C 113.3(6) . . ? N3C' C4C' H4C3 108.6 . . ? C4C C4C' H4C3 108.6 . . ? N3C' C4C' H4C4 108.6 . . ? C4C C4C' H4C4 108.5 . . ? H4C3 C4C' H4C4 107.5 . . ? N3F' C4C' H4C7 107.9 . . ? C4C C4C' H4C7 109.6 . . ? N3F' C4C' H4C8 110.3 . . ? C4C C4C' H4C8 107.8 . . ? H4C7 C4C' H4C8 107.8 . . ? C4C' N3C' C2C' 118.5(6) . . ? C4C' N3C' Zn1 109.4(5) . . ? C2C' N3C' Zn1 110.9(4) . . ? C2C' N3C' H4C8 115.1 . . ? C4C' N3C' H3C' 105.7 . . ? C2C' N3C' H3C' 105.7 . . ? Zn1 N3C' H3C' 105.7 . . ? C4C' N3F' C2C' 111.1(6) . . ? C4C' N3F' Zn1 111.7(4) . . ? C2C' N3F' Zn1 112.8(4) . . ? C4C' N3F' H3F' 107 . . ? C2C' N3F' H3F' 107 . . ? Zn1 N3F' H3F' 107 . . ? N3C' C2C' C1' 118.7(4) . . ? C1' C2C' N3F' 112.6(5) . . ? N3C' C2C' H2C3 107.6 . . ? C1' C2C' H2C3 107.6 . . ? N3F' C2C' H2C3 135.6 . . ? N3C' C2C' H2C4 107.6 . . ? C1' C2C' H2C4 107.6 . . ? H2C3 C2C' H2C4 107.1 . . ? C1' C2C' H2C7 109.6 . . ? N3F' C2C' H2C7 111.2 . . ? C1' C2C' H2C8 108.5 . . ? N3F' C2C' H2C8 107 . . ? H2C7 C2C' H2C8 107.9 . . ? C2C' C1' C2B' 113.1(5) . . ? C2C' C1' C0' 106.0(5) . . ? C2B' C1' C0' 108.8(6) . . ? C2C' C1' C2A' 112.8(4) . . ? C2B' C1' C2A' 108.2(5) . . ? C0' C1' C2A' 107.7(5) . . ? C1' C0' H0'1 109.5 . . ? C1' C0' H0'2 109.5 . . ? H0'1 C0' H0'2 109.5 . . ? C1' C0' H0'3 109.5 . . ? H0'1 C0' H0'3 109.5 . . ? H0'2 C0' H0'3 109.5 . . ? O14' Cl1 O11 119.3(7) . . ? O14' Cl1 O12 103.5(8) . . ? O11 Cl1 O12 119.9(7) . . ? O11 Cl1 O13 114.0(10) . . ? O12 Cl1 O13 121.2(10) . . ? O14' Cl1 O12' 130.6(9) . . ? O11 Cl1 O12' 101.9(8) . . ? O14' Cl1 O13' 98.5(7) . . ? O11 Cl1 O13' 107.9(6) . . ? O12 Cl1 O13' 104.9(6) . . ? O12' Cl1 O13' 93.1(7) . . ? O11 Cl1 O14 100.4(10) . . ? O12 Cl1 O14 94.9(9) . . ? O13 Cl1 O14 97.1(12) . . ? O24 Cl2 O22 124.7(7) . . ? O24 Cl2 O21 116.0(10) . . ? O22 Cl2 O21 113.5(9) . . ? O21' Cl2 O24' 100.6(7) . . ? O22' Cl2 O24' 110.5(9) . . ? O21' Cl2 O23' 84.3(8) . . ? O22' Cl2 O23' 91.3(9) . . ? O24' Cl2 O23' 92.2(8) . . ? O24 Cl2 O23 104.2(8) . . ? O22 Cl2 O23 92.1(6) . . ? O21 Cl2 O23 97.3(11) . . ? 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 N3D H3D O21' 0.93 2.55 3.296(13) 138 1_545 N3A' H3A' O22 0.93 2.57 3.412(15) 151.6 1_545 N3B H3B1 O22 0.93 2.23 3.045(14) 146.5 1_545 N3E H3E O12' 0.93 2.27 3.085(15) 145.8 1_655 N3B' H3B' O21 0.93 2.42 3.31(2) 161.2 1_655 N3C H3C O12 0.93 2.32 3.231(16) 165.5 1_655 N3F H3F O14' 0.93 2.04 2.961(18) 171.2 . N3C' H3C' O13 0.93 2.56 3.292(18) 135.3 . N3F' H3F' O21' 0.93 2.35 3.139(12) 143 1_655 #===END #------------------------------------------------------------------------------ #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_gk204 _database_code_depnum_ccdc_archive 'CCDC 738804' _audit_creation_date 2009-06-11T12:18:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H106 Cl4 N8 O4' _chemical_formula_moiety 'C42 H94 N8, 2(C H4 O),2(H2 O),4(Cl)' _chemical_formula_weight 953.17 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3572(3) _cell_length_b 14.2614(5) _cell_length_c 42.0780(10) _cell_angle_alpha 90 _cell_angle_beta 96.001(3) _cell_angle_gamma 90 _cell_volume 5584.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4095 _cell_measurement_theta_min 2.4276 _cell_measurement_theta_max 27.2271 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.992 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0256795545 _diffrn_orient_matrix_ub_12 0.0468105596 _diffrn_orient_matrix_ub_13 0.00003935 _diffrn_orient_matrix_ub_21 -0.0687214925 _diffrn_orient_matrix_ub_22 0.0164840287 _diffrn_orient_matrix_ub_23 0.0029723724 _diffrn_orient_matrix_ub_31 0.020357049 _diffrn_orient_matrix_ub_32 -0.003078333 _diffrn_orient_matrix_ub_33 0.0166781686 _diffrn_reflns_av_R_equivalents 0.1488 _diffrn_reflns_av_unetI/netI 0.3044 _diffrn_reflns_number 47180 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 9783 _reflns_number_gt 3271 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9783 _refine_ls_number_parameters 564 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1965 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.047 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4607(6) 0.3981(4) 0.18484(14) 0.0299(16) Uani 1 1 d . . . N0 N 0.3324(5) 0.4148(3) 0.16093(11) 0.0287(13) Uani 1 1 d . . . H0A H 0.2567 0.3814 0.1676 0.034 Uiso 1 1 calc R . . H0B H 0.3089 0.4773 0.1619 0.034 Uiso 1 1 calc R . . C11 C 0.3425(6) 0.3907(4) 0.12662(13) 0.0271(16) Uani 1 1 d . . . H11A H 0.3178 0.3238 0.123 0.033 Uiso 1 1 calc R . . H11B H 0.4425 0.4001 0.1216 0.033 Uiso 1 1 calc R . . C12 C 0.2426(6) 0.4505(4) 0.10472(14) 0.0358(17) Uani 1 1 d . . . H12A H 0.26 0.4362 0.0824 0.043 Uiso 1 1 calc R . . H12B H 0.2689 0.517 0.1088 0.043 Uiso 1 1 calc R . . C13 C 0.0803(6) 0.4397(4) 0.10748(14) 0.0357(17) Uani 1 1 d . . . H13A H 0.0526 0.3732 0.1039 0.043 Uiso 1 1 calc R . . H13B H 0.0605 0.4568 0.1294 0.043 Uiso 1 1 calc R . . C14 C -0.0100(6) 0.5001(5) 0.08387(13) 0.0339(16) Uani 1 1 d . . . H14A H 0.0149 0.5666 0.0884 0.041 Uiso 1 1 calc R . . H14B H 0.0158 0.4858 0.0622 0.041 Uiso 1 1 calc R . . C15 C -0.1699(6) 0.4889(4) 0.08386(14) 0.0350(17) Uani 1 1 d . . . H15A H -0.1968 0.5055 0.1053 0.042 Uiso 1 1 calc R . . H15B H -0.1951 0.4222 0.0799 0.042 Uiso 1 1 calc R . . C16 C -0.2568(6) 0.5485(4) 0.05912(14) 0.0339(17) Uani 1 1 d . . . H16A H -0.2342 0.6152 0.0639 0.041 Uiso 1 1 calc R . . H16B H -0.2248 0.5344 0.038 0.041 Uiso 1 1 calc R . . C17 C -0.4158(6) 0.5366(4) 0.05683(15) 0.0374(17) Uani 1 1 d . . . H17A H -0.4486 0.5512 0.0779 0.045 Uiso 1 1 calc R . . H17B H -0.4391 0.4701 0.052 0.045 Uiso 1 1 calc R . . C18 C -0.4991(6) 0.5975(4) 0.03166(15) 0.0405(18) Uani 1 1 d . . . H18A H -0.4746 0.664 0.0363 0.049 Uiso 1 1 calc R . . H18B H -0.467 0.5823 0.0106 0.049 Uiso 1 1 calc R . . C19 C -0.6580(6) 0.5870(4) 0.02948(14) 0.0378(17) Uani 1 1 d . . . H19A H -0.6899 0.6003 0.0507 0.045 Uiso 1 1 calc R . . H19B H -0.6827 0.5209 0.0242 0.045 Uiso 1 1 calc R . . C110 C -0.7421(6) 0.6507(4) 0.00468(14) 0.0398(18) Uani 1 1 d . . . H11C H -0.7165 0.7168 0.0097 0.048 Uiso 1 1 calc R . . H11D H -0.7119 0.6366 -0.0167 0.048 Uiso 1 1 calc R . . C111 C -0.9051(6) 0.6400(4) 0.00321(14) 0.0345(17) Uani 1 1 d . . . H11E H -0.9309 0.5744 -0.0025 0.041 Uiso 1 1 calc R . . H11F H -0.9349 0.6524 0.0247 0.041 Uiso 1 1 calc R . . C112 C -0.9878(6) 0.7043(5) -0.02044(14) 0.0409(18) Uani 1 1 d . . . H11G H -0.9579 0.6924 -0.042 0.049 Uiso 1 1 calc R . . H11H H -0.9634 0.7701 -0.0147 0.049 Uiso 1 1 calc R . . C113 C -1.1502(7) 0.6913(5) -0.02161(16) 0.0492(19) Uani 1 1 d . . . H11I H -1.174 0.6253 -0.0272 0.059 Uiso 1 1 calc R . . H11J H -1.1796 0.7032 0 0.059 Uiso 1 1 calc R . . C114 C -1.2363(7) 0.7549(5) -0.04533(17) 0.070(2) Uani 1 1 d . . . H11K H -1.2163 0.8205 -0.0396 0.104 Uiso 1 1 calc R . . H11L H -1.339 0.7423 -0.0449 0.104 Uiso 1 1 calc R . . H11M H -1.2093 0.7429 -0.0668 0.104 Uiso 1 1 calc R . . C2A C 0.4178(6) 0.4327(4) 0.21682(13) 0.0255(15) Uani 1 1 d . . . H2A1 H 0.435 0.5011 0.2186 0.031 Uiso 1 1 calc R . . H2A2 H 0.3138 0.4215 0.2177 0.031 Uiso 1 1 calc R . . N3A N 0.5007(5) 0.3841(3) 0.24426(13) 0.0265(13) Uani 1 1 d D . . H3A H 0.453(5) 0.337(3) 0.2479(13) 0.032 Uiso 1 1 d D . . C4A C 0.5161(6) 0.4381(4) 0.27368(13) 0.0305(16) Uani 1 1 d . . . H4A1 H 0.4222 0.4407 0.2825 0.037 Uiso 1 1 calc R . . H4A2 H 0.5442 0.5031 0.2689 0.037 Uiso 1 1 calc R . . C4A' C 0.6254(6) 0.3972(4) 0.29808(13) 0.0261(15) Uani 1 1 d . . . H4A3 H 0.6277 0.4338 0.3181 0.031 Uiso 1 1 calc R . . H4A4 H 0.5984 0.3319 0.3027 0.031 Uiso 1 1 calc R . . N3A' N 0.7699(5) 0.3982(3) 0.28660(10) 0.0260(13) Uani 1 1 d . . . H3A1 H 0.7948 0.4595 0.2831 0.031 Uiso 1 1 calc R . . H3A2 H 0.7644 0.3677 0.2672 0.031 Uiso 1 1 calc R . . C2A' C 0.8871(6) 0.3541(4) 0.30844(13) 0.0252(15) Uani 1 1 d . . . H2A3 H 0.8468 0.3023 0.3204 0.03 Uiso 1 1 calc R . . H2A4 H 0.9281 0.4012 0.3241 0.03 Uiso 1 1 calc R . . C2B C 0.4873(6) 0.2901(4) 0.18554(14) 0.0326(17) Uani 1 1 d . . . H2B1 H 0.4124 0.2588 0.1967 0.039 Uiso 1 1 calc R . . H2B2 H 0.4807 0.2657 0.1634 0.039 Uiso 1 1 calc R . . N3B N 0.6331(5) 0.2682(3) 0.20239(11) 0.0271(13) Uani 1 1 d D . . H3B H 0.691(5) 0.261(4) 0.1869(10) 0.032 Uiso 1 1 d D . . C4B C 0.6372(6) 0.1723(4) 0.21742(14) 0.0293(16) Uani 1 1 d . . . H4B1 H 0.5655 0.1686 0.2331 0.035 Uiso 1 1 calc R . . H4B2 H 0.6131 0.1241 0.2008 0.035 Uiso 1 1 calc R . . C4B' C 0.7846(6) 0.1546(4) 0.23384(13) 0.0267(15) Uani 1 1 d . . . H4B3 H 0.7921 0.0887 0.2412 0.032 Uiso 1 1 calc R . . H4B4 H 0.857 0.1648 0.2186 0.032 Uiso 1 1 calc R . . N3B' N 0.8131(5) 0.2178(3) 0.26117(11) 0.0239(12) Uani 1 1 d D . . H3B' H 0.764(5) 0.194(4) 0.2761(9) 0.029 Uiso 1 1 d D . . C2B' C 0.9663(5) 0.2216(4) 0.27428(13) 0.0264(15) Uani 1 1 d . . . H2B3 H 1.0275 0.2103 0.2568 0.032 Uiso 1 1 calc R . . H2B4 H 0.9859 0.1712 0.2903 0.032 Uiso 1 1 calc R . . C2C C 0.5881(6) 0.4527(4) 0.17359(13) 0.0264(16) Uani 1 1 d . . . H2C1 H 0.6252 0.4186 0.1557 0.032 Uiso 1 1 calc R . . H2C2 H 0.5546 0.5151 0.1656 0.032 Uiso 1 1 calc R . . N3C N 0.7017(5) 0.4645(3) 0.19881(11) 0.0319(13) Uani 1 1 d . . . H3C1 H 0.7002 0.4141 0.2124 0.038 Uiso 1 1 calc R . . H3C2 H 0.6825 0.5172 0.2102 0.038 Uiso 1 1 calc R . . C4C C 0.8475(6) 0.4732(4) 0.18934(14) 0.0284(16) Uani 1 1 d . . . H4C1 H 0.8544 0.5314 0.1768 0.034 Uiso 1 1 calc R . . H4C2 H 0.8672 0.4195 0.1755 0.034 Uiso 1 1 calc R . . C4C' C 0.9575(6) 0.4754(4) 0.21770(13) 0.0287(16) Uani 1 1 d . . . H4C3 H 1.0544 0.4822 0.2105 0.034 Uiso 1 1 calc R . . H4C4 H 0.9399 0.53 0.2313 0.034 Uiso 1 1 calc R . . N3C' N 0.9514(5) 0.3881(4) 0.23653(11) 0.0276(14) Uani 1 1 d . . . H3C' H 0.975(6) 0.350(4) 0.2223(12) 0.033 Uiso 1 1 d . . . C2C' C 1.0552(6) 0.3875(4) 0.26553(13) 0.0273(15) Uani 1 1 d . . . H2C3 H 1.0614 0.4509 0.2752 0.033 Uiso 1 1 calc R . . H2C4 H 1.1517 0.3701 0.2598 0.033 Uiso 1 1 calc R . . C1' C 1.0055(6) 0.3161(4) 0.28981(14) 0.0283(15) Uani 1 1 d . . . N1' N 1.1368(4) 0.3005(3) 0.31324(10) 0.0231(12) Uani 1 1 d . . . H1'1 H 1.2018 0.2666 0.303 0.028 Uiso 1 1 calc R . . H1'2 H 1.1776 0.3582 0.318 0.028 Uiso 1 1 calc R . . C11' C 1.1194(6) 0.2525(4) 0.34388(13) 0.0269(16) Uani 1 1 d . . . H11N H 1.0464 0.2024 0.3401 0.032 Uiso 1 1 calc R . . H11O H 1.0844 0.298 0.359 0.032 Uiso 1 1 calc R . . C12' C 1.2615(6) 0.2094(4) 0.35875(13) 0.0319(16) Uani 1 1 d . . . H12C H 1.245 0.1788 0.3792 0.038 Uiso 1 1 calc R . . H12D H 1.2917 0.1603 0.3442 0.038 Uiso 1 1 calc R . . C13' C 1.3824(6) 0.2799(4) 0.36506(13) 0.0308(16) Uani 1 1 d . . . H13C H 1.3485 0.3328 0.3775 0.037 Uiso 1 1 calc R . . H13D H 1.4067 0.3052 0.3444 0.037 Uiso 1 1 calc R . . C14' C 1.5180(6) 0.2388(4) 0.38315(13) 0.0285(16) Uani 1 1 d . . . H14C H 1.4964 0.2184 0.4046 0.034 Uiso 1 1 calc R . . H14D H 1.5482 0.1829 0.3716 0.034 Uiso 1 1 calc R . . C15' C 1.6403(6) 0.3094(4) 0.38665(14) 0.0356(17) Uani 1 1 d . . . H15C H 1.607 0.3663 0.3971 0.043 Uiso 1 1 calc R . . H15D H 1.6631 0.3276 0.3651 0.043 Uiso 1 1 calc R . . C16' C 1.7775(6) 0.2747(4) 0.40573(13) 0.0295(16) Uani 1 1 d . . . H16C H 1.8128 0.2184 0.3952 0.035 Uiso 1 1 calc R . . H16D H 1.7561 0.2565 0.4274 0.035 Uiso 1 1 calc R . . C17' C 1.8945(6) 0.3498(4) 0.40834(14) 0.0358(17) Uani 1 1 d . . . H17C H 1.8582 0.4057 0.4189 0.043 Uiso 1 1 calc R . . H17D H 1.9135 0.3686 0.3865 0.043 Uiso 1 1 calc R . . C18' C 2.0374(6) 0.3187(4) 0.42707(14) 0.0360(17) Uani 1 1 d . . . H18C H 2.0181 0.2982 0.4487 0.043 Uiso 1 1 calc R . . H18D H 2.0754 0.264 0.4161 0.043 Uiso 1 1 calc R . . C19' C 2.1512(6) 0.3949(4) 0.43030(14) 0.0332(17) Uani 1 1 d . . . H19C H 2.1692 0.4163 0.4087 0.04 Uiso 1 1 calc R . . H19D H 2.114 0.4491 0.4416 0.04 Uiso 1 1 calc R . . C10' C 2.2916(6) 0.3638(4) 0.44804(15) 0.0385(17) Uani 1 1 d . . . H10A H 2.2752 0.3474 0.4702 0.046 Uiso 1 1 calc R . . H10B H 2.325 0.3066 0.4377 0.046 Uiso 1 1 calc R . . C1A' C 2.4075(6) 0.4373(4) 0.44889(14) 0.0360(17) Uani 1 1 d . . . H1A1 H 2.3737 0.4942 0.4593 0.043 Uiso 1 1 calc R . . H1A2 H 2.4224 0.4541 0.4267 0.043 Uiso 1 1 calc R . . C1B' C 2.5506(6) 0.4082(4) 0.46629(15) 0.0379(17) Uani 1 1 d . . . H1B1 H 2.5352 0.3895 0.4883 0.046 Uiso 1 1 calc R . . H1B2 H 2.586 0.3525 0.4555 0.046 Uiso 1 1 calc R . . C1C' C 2.6655(6) 0.4831(5) 0.46798(15) 0.0427(18) Uani 1 1 d . . . H1C1 H 2.6814 0.5011 0.4459 0.051 Uiso 1 1 calc R . . H1C2 H 2.6289 0.5392 0.4784 0.051 Uiso 1 1 calc R . . C1D' C 2.8074(6) 0.4568(5) 0.48549(15) 0.056(2) Uani 1 1 d . . . H1D1 H 2.7956 0.4456 0.5081 0.084 Uiso 1 1 calc R . . H1D2 H 2.8763 0.5078 0.4838 0.084 Uiso 1 1 calc R . . H1D3 H 2.8432 0.3996 0.4761 0.084 Uiso 1 1 calc R . . Cl1 Cl 1.21652(17) 0.50308(11) 0.33784(4) 0.0423(5) Uani 1 1 d . . . Cl2 Cl 0.76594(15) 0.11812(10) 0.33023(3) 0.0278(4) Uani 1 1 d . . . Cl3 Cl 0.35533(14) 0.18988(10) 0.27443(3) 0.0247(4) Uani 1 1 d . . . Cl4 Cl 1.10637(16) 0.27211(11) 0.17959(4) 0.0395(5) Uani 1 1 d . . . O1 O 0.8023(5) 0.2268(4) 0.15323(10) 0.0781(18) Uani 1 1 d . . . O2 O 0.8264(5) 0.5856(3) 0.28236(10) 0.0443(13) Uani 1 1 d D . . H2AO H 0.786(7) 0.607(4) 0.2666(10) 0.066 Uiso 1 1 d D . . H2BO H 0.865(7) 0.616(4) 0.2961(11) 0.066 Uiso 1 1 d D . . O10 O 0.6170(7) 0.2598(6) 0.09838(16) 0.119(2) Uani 1 1 d . . . H10 H 0.6845 0.2573 0.1132 0.179 Uiso 1 1 calc R . . C10 C 0.6531(10) 0.2071(7) 0.0724(2) 0.119(4) Uani 1 1 d . . . H10C H 0.5847 0.2205 0.0537 0.179 Uiso 1 1 calc R . . H10D H 0.6497 0.1402 0.0776 0.179 Uiso 1 1 calc R . . H10E H 0.7504 0.2238 0.0677 0.179 Uiso 1 1 calc R . . C20 C 0.4122(14) 0.0901(10) 0.1272(3) 0.120(6) Uiso 0.692(7) 1 d PD . . H20A H 0.311 0.1087 0.1259 0.18 Uiso 0.692(7) 1 calc PR . . H20B H 0.4219 0.0343 0.114 0.18 Uiso 0.692(7) 1 calc PR . . H20C H 0.469 0.1414 0.1195 0.18 Uiso 0.692(7) 1 calc PR . . O20 O 0.4522(9) 0.0737(7) 0.1528(2) 0.115(4) Uiso 0.692(7) 1 d PD . . O30 O 0.1227(18) 0.0522(13) 0.1397(4) 0.091(7) Uiso 0.308(7) 1 d P . . C30 C 0.071(2) 0.0968(16) 0.1143(5) 0.056(8) Uiso 0.308(7) 1 d P . . H30A H 0.1056 0.1616 0.1153 0.084 Uiso 0.308(7) 1 calc PR . . H30B H -0.0344 0.0965 0.1129 0.084 Uiso 0.308(7) 1 calc PR . . H30C H 0.1021 0.0659 0.0954 0.084 Uiso 0.308(7) 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(4) 0.017(4) 0.035(4) -0.001(3) -0.008(3) 0.001(3) N0 0.025(3) 0.014(3) 0.046(4) 0.011(3) -0.001(3) -0.002(2) C11 0.027(4) 0.031(4) 0.022(4) 0.002(3) -0.005(3) 0.003(3) C12 0.040(4) 0.023(4) 0.043(4) -0.001(3) 0.000(3) 0.000(3) C13 0.033(4) 0.022(4) 0.051(5) -0.002(3) -0.001(3) 0.010(3) C14 0.031(4) 0.040(4) 0.029(4) 0.001(4) -0.005(3) 0.002(3) C15 0.026(4) 0.031(4) 0.046(4) 0.002(4) -0.008(3) -0.004(3) C16 0.041(4) 0.024(4) 0.037(4) -0.009(3) 0.006(3) 0.007(3) C17 0.033(4) 0.034(4) 0.045(5) 0.000(4) 0.005(3) 0.003(3) C18 0.042(4) 0.026(4) 0.051(5) -0.008(4) -0.007(4) 0.002(3) C19 0.032(4) 0.035(4) 0.045(5) -0.005(4) 0.002(3) 0.007(3) C110 0.038(4) 0.028(4) 0.051(5) -0.008(4) -0.007(4) 0.002(3) C111 0.027(4) 0.034(4) 0.039(4) 0.000(3) -0.012(3) 0.009(3) C112 0.036(4) 0.039(5) 0.045(5) -0.007(4) -0.008(4) -0.001(4) C113 0.045(5) 0.042(5) 0.058(5) -0.011(4) -0.007(4) 0.013(4) C114 0.064(5) 0.057(6) 0.079(6) -0.010(5) -0.032(5) 0.009(4) C2A 0.029(4) 0.022(4) 0.025(4) 0.003(3) 0.002(3) 0.004(3) N3A 0.023(3) 0.019(3) 0.037(3) -0.005(3) 0.002(3) -0.004(2) C4A 0.036(4) 0.028(4) 0.028(4) 0.000(3) 0.009(3) -0.015(3) C4A' 0.029(4) 0.019(4) 0.029(4) 0.003(3) -0.003(3) -0.004(3) N3A' 0.025(3) 0.024(3) 0.029(3) -0.001(3) 0.003(2) -0.002(2) C2A' 0.024(4) 0.019(4) 0.031(4) 0.006(3) -0.003(3) 0.000(3) C2B 0.025(4) 0.030(4) 0.039(4) 0.003(3) -0.010(3) -0.003(3) N3B 0.022(3) 0.022(3) 0.037(4) 0.007(3) 0.001(2) 0.004(2) C4B 0.025(4) 0.028(4) 0.035(4) 0.009(3) -0.002(3) 0.000(3) C4B' 0.032(4) 0.019(4) 0.027(4) -0.003(3) -0.008(3) -0.004(3) N3B' 0.020(3) 0.021(3) 0.030(3) -0.001(3) 0.001(2) 0.002(2) C2B' 0.020(4) 0.028(4) 0.031(4) -0.001(3) 0.001(3) -0.005(3) C2C 0.020(4) 0.036(4) 0.021(4) 0.003(3) -0.007(3) 0.002(3) N3C 0.031(3) 0.020(3) 0.044(4) 0.010(3) -0.001(3) 0.002(2) C4C 0.023(4) 0.024(4) 0.039(4) 0.007(3) 0.008(3) -0.004(3) C4C' 0.032(4) 0.025(4) 0.031(4) 0.006(3) 0.007(3) -0.001(3) N3C' 0.036(3) 0.025(3) 0.022(4) 0.002(3) 0.004(3) 0.001(3) C2C' 0.034(4) 0.018(4) 0.030(4) 0.005(3) 0.000(3) 0.000(3) C1' 0.030(4) 0.022(4) 0.031(4) 0.000(3) -0.008(3) 0.003(3) N1' 0.027(3) 0.015(3) 0.027(3) 0.001(2) 0.001(2) 0.002(2) C11' 0.026(4) 0.033(4) 0.021(4) 0.002(3) 0.000(3) -0.001(3) C12' 0.030(4) 0.036(4) 0.028(4) 0.004(3) -0.003(3) 0.008(3) C13' 0.029(4) 0.033(4) 0.031(4) -0.002(3) 0.002(3) -0.007(3) C14' 0.027(4) 0.032(4) 0.025(4) -0.007(3) -0.003(3) 0.007(3) C15' 0.028(4) 0.033(4) 0.044(4) -0.002(4) -0.005(3) 0.006(3) C16' 0.027(4) 0.033(4) 0.028(4) -0.004(3) 0.002(3) 0.007(3) C17' 0.036(4) 0.033(4) 0.037(4) -0.006(3) -0.001(3) 0.002(3) C18' 0.037(4) 0.037(4) 0.033(4) -0.001(3) 0.002(3) 0.009(4) C19' 0.023(4) 0.037(4) 0.037(4) 0.000(3) -0.006(3) 0.002(3) C10' 0.036(4) 0.032(4) 0.047(5) 0.004(4) 0.004(3) -0.003(3) C1A' 0.032(4) 0.031(4) 0.044(5) 0.003(3) -0.005(3) 0.002(3) C1B' 0.033(4) 0.029(4) 0.051(5) -0.002(3) 0.004(3) 0.004(3) C1C' 0.035(4) 0.041(5) 0.053(5) -0.011(4) 0.006(4) -0.003(4) C1D' 0.024(4) 0.074(6) 0.069(5) -0.008(5) -0.001(4) 0.002(4) Cl1 0.0543(11) 0.0251(10) 0.0464(11) 0.0018(9) -0.0005(9) -0.0058(9) Cl2 0.0328(9) 0.0171(9) 0.0334(10) 0.0009(8) 0.0033(7) -0.0064(7) Cl3 0.0209(8) 0.0178(8) 0.0361(10) 0.0006(8) 0.0067(7) -0.0004(7) Cl4 0.0371(10) 0.0294(10) 0.0516(12) 0.0047(9) 0.0027(9) 0.0005(8) O1 0.050(3) 0.129(5) 0.058(3) -0.023(3) 0.019(3) -0.019(3) O2 0.054(4) 0.029(3) 0.047(4) -0.001(3) -0.007(3) -0.005(2) O10 0.099(5) 0.150(7) 0.106(6) 0.002(5) 0.000(4) 0.035(5) C10 0.132(9) 0.118(10) 0.112(9) -0.033(8) 0.035(7) -0.004(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N0 1.502(6) . ? C1 C2A 1.525(7) . ? C1 C2C 1.540(7) . ? C1 C2B 1.561(8) . ? N0 C11 1.497(6) . ? N0 H0A 0.92 . ? N0 H0B 0.92 . ? C11 C12 1.506(7) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.544(7) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.506(7) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.505(7) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.514(7) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.490(7) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.520(7) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.488(7) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C110 1.537(7) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C110 C111 1.527(7) . ? C110 H11C 0.99 . ? C110 H11D 0.99 . ? C111 C112 1.506(7) . ? C111 H11E 0.99 . ? C111 H11F 0.99 . ? C112 C113 1.526(7) . ? C112 H11G 0.99 . ? C112 H11H 0.99 . ? C113 C114 1.516(8) . ? C113 H11I 0.99 . ? C113 H11J 0.99 . ? C114 H11K 0.98 . ? C114 H11L 0.98 . ? C114 H11M 0.98 . ? C2A N3A 1.493(7) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? N3A C4A 1.453(7) . ? N3A H3A 0.83(3) . ? C4A C4A' 1.490(7) . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? C4A' N3A' 1.483(6) . ? C4A' H4A3 0.99 . ? C4A' H4A4 0.99 . ? N3A' C2A' 1.494(6) . ? N3A' H3A1 0.92 . ? N3A' H3A2 0.92 . ? C2A' C1' 1.522(7) . ? C2A' H2A3 0.99 . ? C2A' H2A4 0.99 . ? C2B N3B 1.504(6) . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? N3B C4B 1.505(7) . ? N3B H3B 0.89(3) . ? C4B C4B' 1.498(7) . ? C4B H4B1 0.99 . ? C4B H4B2 0.99 . ? C4B' N3B' 1.464(6) . ? C4B' H4B3 0.99 . ? C4B' H4B4 0.99 . ? N3B' C2B' 1.483(6) . ? N3B' H3B' 0.88(2) . ? C2B' C1' 1.526(7) . ? C2B' H2B3 0.99 . ? C2B' H2B4 0.99 . ? C2C N3C 1.431(6) . ? C2C H2C1 0.99 . ? C2C H2C2 0.99 . ? N3C C4C 1.465(6) . ? N3C H3C1 0.92 . ? N3C H3C2 0.92 . ? C4C C4C' 1.493(7) . ? C4C H4C1 0.99 . ? C4C H4C2 0.99 . ? C4C' N3C' 1.480(7) . ? C4C' H4C3 0.99 . ? C4C' H4C4 0.99 . ? N3C' C2C' 1.478(6) . ? N3C' H3C' 0.85(5) . ? C2C' C1' 1.549(7) . ? C2C' H2C3 0.99 . ? C2C' H2C4 0.99 . ? C1' N1' 1.509(6) . ? N1' C11' 1.484(6) . ? N1' H1'1 0.92 . ? N1' H1'2 0.92 . ? C11' C12' 1.537(7) . ? C11' H11N 0.99 . ? C11' H11O 0.99 . ? C12' C13' 1.516(7) . ? C12' H12C 0.99 . ? C12' H12D 0.99 . ? C13' C14' 1.526(7) . ? C13' H13C 0.99 . ? C13' H13D 0.99 . ? C14' C15' 1.519(7) . ? C14' H14C 0.99 . ? C14' H14D 0.99 . ? C15' C16' 1.523(7) . ? C15' H15C 0.99 . ? C15' H15D 0.99 . ? C16' C17' 1.527(7) . ? C16' H16C 0.99 . ? C16' H16D 0.99 . ? C17' C18' 1.545(7) . ? C17' H17C 0.99 . ? C17' H17D 0.99 . ? C18' C19' 1.519(8) . ? C18' H18C 0.99 . ? C18' H18D 0.99 . ? C19' C10' 1.508(7) . ? C19' H19C 0.99 . ? C19' H19D 0.99 . ? C10' C1A' 1.506(8) . ? C10' H10A 0.99 . ? C10' H10B 0.99 . ? C1A' C1B' 1.515(7) . ? C1A' H1A1 0.99 . ? C1A' H1A2 0.99 . ? C1B' C1C' 1.512(8) . ? C1B' H1B1 0.99 . ? C1B' H1B2 0.99 . ? C1C' C1D' 1.498(7) . ? C1C' H1C1 0.99 . ? C1C' H1C2 0.99 . ? C1D' H1D1 0.98 . ? C1D' H1D2 0.98 . ? C1D' H1D3 0.98 . ? O2 H2AO 0.79(3) . ? O2 H2BO 0.78(3) . ? O10 C10 1.397(9) . ? O10 H10 0.84 . ? C10 H10C 0.98 . ? C10 H10D 0.98 . ? C10 H10E 0.98 . ? C20 O20 1.126(11) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? O30 C30 1.30(2) . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? 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 N0 C1 C2A 105.9(5) . . ? N0 C1 C2C 107.7(5) . . ? C2A C1 C2C 113.0(5) . . ? N0 C1 C2B 106.4(4) . . ? C2A C1 C2B 111.0(5) . . ? C2C C1 C2B 112.2(5) . . ? C11 N0 C1 118.9(4) . . ? C11 N0 H0A 107.6 . . ? C1 N0 H0A 107.6 . . ? C11 N0 H0B 107.6 . . ? C1 N0 H0B 107.6 . . ? H0A N0 H0B 107 . . ? N0 C11 C12 111.3(5) . . ? N0 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N0 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108 . . ? C11 C12 C13 116.7(5) . . ? C11 C12 H12A 108.1 . . ? C13 C12 H12A 108.1 . . ? C11 C12 H12B 108.1 . . ? C13 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C14 C13 C12 112.5(5) . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 115.3(5) . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C14 C15 C16 113.8(5) . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 116.2(5) . . ? C17 C16 H16A 108.2 . . ? C15 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C15 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 114.6(5) . . ? C16 C17 H17A 108.6 . . ? C18 C17 H17A 108.6 . . ? C16 C17 H17B 108.6 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C17 114.9(5) . . ? C19 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? C19 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C18 C19 C110 114.8(5) . . ? C18 C19 H19A 108.6 . . ? C110 C19 H19A 108.6 . . ? C18 C19 H19B 108.6 . . ? C110 C19 H19B 108.6 . . ? H19A C19 H19B 107.5 . . ? C111 C110 C19 114.0(5) . . ? C111 C110 H11C 108.8 . . ? C19 C110 H11C 108.8 . . ? C111 C110 H11D 108.8 . . ? C19 C110 H11D 108.8 . . ? H11C C110 H11D 107.6 . . ? C112 C111 C110 114.1(5) . . ? C112 C111 H11E 108.7 . . ? C110 C111 H11E 108.7 . . ? C112 C111 H11F 108.7 . . ? C110 C111 H11F 108.7 . . ? H11E C111 H11F 107.6 . . ? C111 C112 C113 112.9(5) . . ? C111 C112 H11G 109 . . ? C113 C112 H11G 109 . . ? C111 C112 H11H 109 . . ? C113 C112 H11H 109 . . ? H11G C112 H11H 107.8 . . ? C114 C113 C112 114.1(6) . . ? C114 C113 H11I 108.7 . . ? C112 C113 H11I 108.7 . . ? C114 C113 H11J 108.7 . . ? C112 C113 H11J 108.7 . . ? H11I C113 H11J 107.6 . . ? C113 C114 H11K 109.5 . . ? C113 C114 H11L 109.5 . . ? H11K C114 H11L 109.5 . . ? C113 C114 H11M 109.5 . . ? H11K C114 H11M 109.5 . . ? H11L C114 H11M 109.5 . . ? N3A C2A C1 111.7(5) . . ? N3A C2A H2A1 109.3 . . ? C1 C2A H2A1 109.3 . . ? N3A C2A H2A2 109.3 . . ? C1 C2A H2A2 109.3 . . ? H2A1 C2A H2A2 108 . . ? C4A N3A C2A 114.2(5) . . ? C4A N3A H3A 106(4) . . ? C2A N3A H3A 106(4) . . ? N3A C4A C4A' 112.3(5) . . ? N3A C4A H4A1 109.1 . . ? C4A' C4A H4A1 109.1 . . ? N3A C4A H4A2 109.1 . . ? C4A' C4A H4A2 109.1 . . ? H4A1 C4A H4A2 107.9 . . ? N3A' C4A' C4A 110.8(4) . . ? N3A' C4A' H4A3 109.5 . . ? C4A C4A' H4A3 109.5 . . ? N3A' C4A' H4A4 109.5 . . ? C4A C4A' H4A4 109.5 . . ? H4A3 C4A' H4A4 108.1 . . ? C4A' N3A' C2A' 115.6(4) . . ? C4A' N3A' H3A1 108.4 . . ? C2A' N3A' H3A1 108.4 . . ? C4A' N3A' H3A2 108.4 . . ? C2A' N3A' H3A2 108.4 . . ? H3A1 N3A' H3A2 107.5 . . ? N3A' C2A' C1' 111.1(4) . . ? N3A' C2A' H2A3 109.4 . . ? C1' C2A' H2A3 109.4 . . ? N3A' C2A' H2A4 109.4 . . ? C1' C2A' H2A4 109.4 . . ? H2A3 C2A' H2A4 108 . . ? N3B C2B C1 110.4(4) . . ? N3B C2B H2B1 109.6 . . ? C1 C2B H2B1 109.6 . . ? N3B C2B H2B2 109.6 . . ? C1 C2B H2B2 109.6 . . ? H2B1 C2B H2B2 108.1 . . ? C2B N3B C4B 111.6(4) . . ? C2B N3B H3B 105(3) . . ? C4B N3B H3B 103(4) . . ? C4B' C4B N3B 109.2(4) . . ? C4B' C4B H4B1 109.8 . . ? N3B C4B H4B1 109.8 . . ? C4B' C4B H4B2 109.8 . . ? N3B C4B H4B2 109.8 . . ? H4B1 C4B H4B2 108.3 . . ? N3B' C4B' C4B 110.0(5) . . ? N3B' C4B' H4B3 109.7 . . ? C4B C4B' H4B3 109.7 . . ? N3B' C4B' H4B4 109.7 . . ? C4B C4B' H4B4 109.7 . . ? H4B3 C4B' H4B4 108.2 . . ? C4B' N3B' C2B' 113.8(4) . . ? C4B' N3B' H3B' 105(4) . . ? C2B' N3B' H3B' 108(3) . . ? N3B' C2B' C1' 111.8(5) . . ? N3B' C2B' H2B3 109.3 . . ? C1' C2B' H2B3 109.3 . . ? N3B' C2B' H2B4 109.3 . . ? C1' C2B' H2B4 109.3 . . ? H2B3 C2B' H2B4 107.9 . . ? N3C C2C C1 111.7(4) . . ? N3C C2C H2C1 109.3 . . ? C1 C2C H2C1 109.3 . . ? N3C C2C H2C2 109.3 . . ? C1 C2C H2C2 109.3 . . ? H2C1 C2C H2C2 107.9 . . ? C2C N3C C4C 116.6(4) . . ? C2C N3C H3C1 108.1 . . ? C4C N3C H3C1 108.1 . . ? C2C N3C H3C2 108.1 . . ? C4C N3C H3C2 108.1 . . ? H3C1 N3C H3C2 107.3 . . ? N3C C4C C4C' 111.6(5) . . ? N3C C4C H4C1 109.3 . . ? C4C' C4C H4C1 109.3 . . ? N3C C4C H4C2 109.3 . . ? C4C' C4C H4C2 109.3 . . ? H4C1 C4C H4C2 108 . . ? N3C' C4C' C4C 110.4(5) . . ? N3C' C4C' H4C3 109.6 . . ? C4C C4C' H4C3 109.6 . . ? N3C' C4C' H4C4 109.6 . . ? C4C C4C' H4C4 109.6 . . ? H4C3 C4C' H4C4 108.1 . . ? C2C' N3C' C4C' 112.8(5) . . ? C2C' N3C' H3C' 112(4) . . ? C4C' N3C' H3C' 97(4) . . ? N3C' C2C' C1' 109.3(5) . . ? N3C' C2C' H2C3 109.8 . . ? C1' C2C' H2C3 109.8 . . ? N3C' C2C' H2C4 109.8 . . ? C1' C2C' H2C4 109.8 . . ? H2C3 C2C' H2C4 108.3 . . ? N1' C1' C2A' 107.6(4) . . ? N1' C1' C2B' 107.0(4) . . ? C2A' C1' C2B' 112.3(5) . . ? N1' C1' C2C' 104.3(4) . . ? C2A' C1' C2C' 113.0(5) . . ? C2B' C1' C2C' 112.0(5) . . ? C11' N1' C1' 118.7(4) . . ? C11' N1' H1'1 107.6 . . ? C1' N1' H1'1 107.6 . . ? C11' N1' H1'2 107.6 . . ? C1' N1' H1'2 107.6 . . ? H1'1 N1' H1'2 107.1 . . ? N1' C11' C12' 111.7(4) . . ? N1' C11' H11N 109.3 . . ? C12' C11' H11N 109.3 . . ? N1' C11' H11O 109.3 . . ? C12' C11' H11O 109.3 . . ? H11N C11' H11O 107.9 . . ? C13' C12' C11' 113.9(5) . . ? C13' C12' H12C 108.8 . . ? C11' C12' H12C 108.8 . . ? C13' C12' H12D 108.8 . . ? C11' C12' H12D 108.8 . . ? H12C C12' H12D 107.7 . . ? C12' C13' C14' 113.5(5) . . ? C12' C13' H13C 108.9 . . ? C14' C13' H13C 108.9 . . ? C12' C13' H13D 108.9 . . ? C14' C13' H13D 108.9 . . ? H13C C13' H13D 107.7 . . ? C15' C14' C13' 111.9(5) . . ? C15' C14' H14C 109.2 . . ? C13' C14' H14C 109.2 . . ? C15' C14' H14D 109.2 . . ? C13' C14' H14D 109.2 . . ? H14C C14' H14D 107.9 . . ? C14' C15' C16' 114.9(5) . . ? C14' C15' H15C 108.5 . . ? C16' C15' H15C 108.5 . . ? C14' C15' H15D 108.5 . . ? C16' C15' H15D 108.5 . . ? H15C C15' H15D 107.5 . . ? C15' C16' C17' 111.6(5) . . ? C15' C16' H16C 109.3 . . ? C17' C16' H16C 109.3 . . ? C15' C16' H16D 109.3 . . ? C17' C16' H16D 109.3 . . ? H16C C16' H16D 108 . . ? C16' C17' C18' 114.3(5) . . ? C16' C17' H17C 108.7 . . ? C18' C17' H17C 108.7 . . ? C16' C17' H17D 108.7 . . ? C18' C17' H17D 108.7 . . ? H17C C17' H17D 107.6 . . ? C19' C18' C17' 113.7(5) . . ? C19' C18' H18C 108.8 . . ? C17' C18' H18C 108.8 . . ? C19' C18' H18D 108.8 . . ? C17' C18' H18D 108.8 . . ? H18C C18' H18D 107.7 . . ? C10' C19' C18' 113.6(5) . . ? C10' C19' H19C 108.8 . . ? C18' C19' H19C 108.8 . . ? C10' C19' H19D 108.8 . . ? C18' C19' H19D 108.8 . . ? H19C C19' H19D 107.7 . . ? C1A' C10' C19' 113.3(5) . . ? C1A' C10' H10A 108.9 . . ? C19' C10' H10A 108.9 . . ? C1A' C10' H10B 108.9 . . ? C19' C10' H10B 108.9 . . ? H10A C10' H10B 107.7 . . ? C10' C1A' C1B' 114.8(5) . . ? C10' C1A' H1A1 108.6 . . ? C1B' C1A' H1A1 108.6 . . ? C10' C1A' H1A2 108.6 . . ? C1B' C1A' H1A2 108.6 . . ? H1A1 C1A' H1A2 107.5 . . ? C1C' C1B' C1A' 114.7(5) . . ? C1C' C1B' H1B1 108.6 . . ? C1A' C1B' H1B1 108.6 . . ? C1C' C1B' H1B2 108.6 . . ? C1A' C1B' H1B2 108.6 . . ? H1B1 C1B' H1B2 107.6 . . ? C1D' C1C' C1B' 115.8(6) . . ? C1D' C1C' H1C1 108.3 . . ? C1B' C1C' H1C1 108.3 . . ? C1D' C1C' H1C2 108.3 . . ? C1B' C1C' H1C2 108.3 . . ? H1C1 C1C' H1C2 107.4 . . ? C1C' C1D' H1D1 109.5 . . ? C1C' C1D' H1D2 109.5 . . ? H1D1 C1D' H1D2 109.5 . . ? C1C' C1D' H1D3 109.5 . . ? H1D1 C1D' H1D3 109.5 . . ? H1D2 C1D' H1D3 109.5 . . ? H2AO O2 H2BO 123(5) . . ? C10 O10 H10 109.5 . . ? O10 C10 H10C 109.5 . . ? O10 C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? O10 C10 H10E 109.5 . . ? H10C C10 H10E 109.5 . . ? H10D C10 H10E 109.5 . . ? O20 C20 H20A 109.5 . . ? O20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O20 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O30 C30 H30A 109.5 . . ? O30 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O30 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 N0 H0A Cl4 0.92 2.19 3.094(5) 165.8 1_455 N0 H0B Cl2 0.92 2.16 3.077(5) 171.2 2_655 N3A H3A Cl3 0.83(3) 2.58(3) 3.390(5) 163(5) . N3A' H3A1 O2 0.92 1.82 2.733(6) 169.7 . N3A' H3A2 N3B' 0.92 2.21 2.832(6) 124.5 . N3A' H3A2 N3C' 0.92 2.3 2.845(6) 117.5 . N3B H3B O1 0.89(3) 1.91(3) 2.796(6) 171(5) . N3B' H3B' Cl2 0.88(2) 2.52(3) 3.305(5) 148(4) . N3C H3C1 N3B 0.92 2.2 2.879(7) 129.9 . N3C H3C1 N3A 0.92 2.45 3.043(6) 122.7 . N3C H3C2 Cl3 0.92 2.58 3.466(5) 161.9 2_655 N3C' H3C' Cl4 0.85(5) 2.54(5) 3.363(5) 163(5) . N1' H1'1 Cl3 0.92 2.25 3.168(4) 175.6 1_655 N1' H1'2 Cl1 0.92 2.24 3.132(5) 162.1 . O2 H2AO Cl3 0.79(3) 2.38(4) 3.157(4) 169(7) 2_655 O2 H2BO Cl4 0.78(3) 2.45(5) 3.135(5) 147(6) 2_755 O10 H10 O1 0.84 1.96 2.779(8) 163 . #===END _publ_section_references ; Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Oxford Diffraction (2006). CrysAlis CCD. Oxford Diffraction Ltd, Abingdon, England. Oxford Diffraction (2006). CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ;