# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Baolong Li' _publ_contact_author_address ; College of Chemistry and Chemical Engineering Suzhou University Suzhou 215006 CHINA ; _publ_contact_author_email BLLI1965@PUB.SZ.JSINFO.NET _publ_section_title ; Supramolecular isomers in the same crystal: a new type of polycatenation involving ribbons of rings and 2D square networks polycatenated in 3D architecture ; loop_ _publ_author_name 'Baolong Li' 'Li Baozong' 'Peng Yanfen' 'Zhang Yong' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 256591' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H87.50 B6 Cd3 F24 N36 O7.75' _chemical_formula_weight 2439.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2 1/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5472(14) _cell_length_b 24.032(2) _cell_length_c 14.8451(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.943(2) _cell_angle_gamma 90.00 _cell_volume 5161.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 193.15 _cell_measurement_reflns_used 20830 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2447 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7094 _exptl_absorpt_correction_T_max 0.7912 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 193.15 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56824 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11781 _reflns_number_gt 10230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+4.9950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11781 _refine_ls_number_parameters 710 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1828 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.03351(12) Uani 1 2 d S . . Cd2 Cd 0.07860(2) 0.248032(11) -0.43081(2) 0.03806(11) Uani 1 1 d D . . O1 O 0.0304(3) 0.08609(15) 0.0674(3) 0.0651(10) Uani 1 1 d D . . HW1 H 0.061(4) 0.109(2) 0.042(4) 0.073(19) Uiso 1 1 d D . . HW2 H -0.014(4) 0.106(3) 0.091(5) 0.10(2) Uiso 1 1 d D . . O2 O 0.2242(3) 0.2926(2) -0.4267(4) 0.0918(17) Uani 1 1 d D . . HW3 H 0.274(4) 0.294(4) -0.386(4) 0.12(3) Uiso 1 1 d D . . HW4 H 0.235(4) 0.294(3) -0.482(3) 0.08(2) Uiso 1 1 d D . . O3 O 0.1356(3) 0.20013(15) -0.2987(2) 0.0576(8) Uani 1 1 d D . . HW5 H 0.093(6) 0.178(3) -0.280(4) 0.23(7) Uiso 1 1 d D . . HW6 H 0.151(4) 0.220(2) -0.251(3) 0.073(19) Uiso 1 1 d D . . O4 O 0.1330(6) 0.2551(3) -0.1337(5) 0.0602(18) Uiso 0.50 1 d P . . O5 O 0.4908(9) 0.1239(6) 0.4905(9) 0.053(3) Uiso 0.25 1 d P . . O6 O 0.491(2) 0.2244(13) 0.612(2) 0.063(7) Uiso 0.13 1 d P . . B1 B 0.7360(4) 0.3430(2) 0.5302(5) 0.076(2) Uani 1 1 d D . . B2 B 0.6069(4) 0.6551(2) 0.2648(3) 0.0595(15) Uani 1 1 d D . . B3 B 0.1278(5) 0.7655(3) 0.1234(5) 0.078(2) Uani 1 1 d D . . F1 F 0.6429(3) 0.3347(2) 0.5133(4) 0.147(2) Uani 1 1 d D . . F2 F 0.7583(4) 0.3717(2) 0.6072(3) 0.1294(19) Uani 1 1 d D . . F3 F 0.7804(3) 0.29400(16) 0.5297(4) 0.1224(18) Uani 1 1 d D . . F4 F 0.7605(5) 0.3758(2) 0.4601(4) 0.158(2) Uani 1 1 d D . . F5 F 0.6474(5) 0.70524(17) 0.2564(4) 0.156(3) Uani 1 1 d D . . F6 F 0.5264(3) 0.6489(4) 0.2183(4) 0.274(7) Uani 1 1 d D . . F7 F 0.6686(3) 0.61756(18) 0.2283(3) 0.1030(13) Uani 1 1 d D . . F8 F 0.6062(4) 0.6415(3) 0.3522(2) 0.149(3) Uani 1 1 d D . . F9 F 0.0795(4) 0.8074(2) 0.1554(3) 0.152(3) Uani 1 1 d D . . F10 F 0.1926(7) 0.7476(4) 0.1903(7) 0.250(6) Uani 1 1 d D . . F11 F 0.0722(8) 0.7224(3) 0.1012(9) 0.280(6) Uani 1 1 d D . . F12 F 0.1948(8) 0.7846(5) 0.0763(10) 0.125(5) Uani 0.50 1 d PD . . F12' F 0.1300(15) 0.7778(7) 0.0341(7) 0.185(9) Uani 0.50 1 d PD . . N1 N -0.2878(2) 0.03267(17) -0.1077(3) 0.0481(9) Uani 1 1 d . . . N2 N -0.2649(3) 0.0858(2) -0.0969(4) 0.0789(16) Uani 1 1 d . . . N3 N -0.1450(2) 0.03064(15) -0.0491(3) 0.0429(8) Uani 1 1 d . . . N4 N 0.1051(2) 0.03713(14) -0.2669(2) 0.0350(6) Uani 1 1 d . . . N5 N 0.0811(3) 0.08981(16) -0.2491(2) 0.0462(8) Uani 1 1 d . . . N6 N 0.0538(2) 0.03338(14) -0.1348(2) 0.0369(7) Uani 1 1 d . . . N7 N 0.0742(3) 0.37961(14) -0.2276(2) 0.0430(8) Uani 1 1 d . . . N8 N -0.0194(3) 0.37544(16) -0.2406(3) 0.0497(9) Uani 1 1 d . . . N9 N 0.0473(2) 0.31707(15) -0.3322(3) 0.0449(8) Uani 1 1 d . . . N10 N 0.0535(3) 0.66879(17) -0.3261(4) 0.0700(14) Uani 1 1 d . . . N11 N -0.0319(4) 0.6686(2) -0.2981(3) 0.0734(14) Uani 1 1 d . . . N12 N -0.0338(3) 0.70674(15) -0.4351(3) 0.0475(8) Uani 1 1 d . . . N13 N -0.1871(3) 0.16268(15) -0.4005(3) 0.0505(9) Uani 1 1 d . . . N14 N -0.1915(3) 0.15792(17) -0.4922(3) 0.0572(10) Uani 1 1 d . . . N15 N -0.0623(2) 0.20224(14) -0.4369(3) 0.0441(8) Uani 1 1 d . . . N16 N -0.2204(2) -0.13040(15) -0.3989(2) 0.0424(8) Uani 1 1 d . . . N17 N -0.2756(3) -0.1255(2) -0.4773(3) 0.0674(13) Uani 1 1 d . . . N18 N -0.1557(2) -0.18105(14) -0.4954(2) 0.0415(7) Uani 1 1 d . . . C1 C -0.4423(2) 0.00824(18) -0.0685(3) 0.0394(8) Uani 1 1 d . . . C2 C -0.4700(3) 0.05273(19) -0.0193(3) 0.0474(10) Uani 1 1 d . . . H2A H -0.4496 0.0892 -0.0319 0.057 Uiso 1 1 calc R . . C3 C -0.4725(3) -0.04447(19) -0.0486(3) 0.0477(10) Uani 1 1 d . . . H3A H -0.4536 -0.0755 -0.0818 0.057 Uiso 1 1 calc R . . C4 C -0.3824(3) 0.0168(3) -0.1428(3) 0.0569(12) Uani 1 1 d . . . H4A H -0.3804 -0.0179 -0.1784 0.068 Uiso 1 1 calc R . . H4B H -0.4094 0.0464 -0.1838 0.068 Uiso 1 1 calc R . . C5 C -0.1778(3) 0.0824(2) -0.0603(5) 0.0715(17) Uani 1 1 d . . . H5A H -0.1416 0.1144 -0.0433 0.086 Uiso 1 1 calc R . . C6 C -0.2172(3) 0.00041(19) -0.0820(3) 0.0451(9) Uani 1 1 d . . . H6A H -0.2177 -0.0390 -0.0864 0.054 Uiso 1 1 calc R . . C7 C 0.0682(3) 0.01082(18) -0.4288(2) 0.0354(8) Uani 1 1 d . . . C8 C 0.0454(4) -0.0429(2) -0.4537(3) 0.0544(12) Uani 1 1 d . . . H8A H 0.0759 -0.0730 -0.4217 0.065 Uiso 1 1 calc R . . C9 C 0.0218(4) 0.05378(19) -0.4748(3) 0.0550(12) Uani 1 1 d . . . H9A H 0.0357 0.0912 -0.4577 0.066 Uiso 1 1 calc R . . C10 C 0.1433(3) 0.0216(2) -0.3529(3) 0.0455(10) Uani 1 1 d . . . H10A H 0.1818 -0.0122 -0.3426 0.055 Uiso 1 1 calc R . . H10B H 0.1836 0.0520 -0.3708 0.055 Uiso 1 1 calc R . . C11 C 0.0499(3) 0.08548(18) -0.1688(3) 0.0439(9) Uani 1 1 d . . . H11A H 0.0269 0.1163 -0.1378 0.053 Uiso 1 1 calc R . . C12 C 0.0896(3) 0.00393(17) -0.1985(3) 0.0386(8) Uani 1 1 d . . . H12A H 0.1022 -0.0349 -0.1955 0.046 Uiso 1 1 calc R . . C13 C 0.1188(3) 0.47689(18) -0.1921(3) 0.0436(9) Uani 1 1 d . . . C14 C 0.1492(4) 0.4915(2) -0.2740(3) 0.0567(12) Uani 1 1 d . . . H14A H 0.1669 0.4632 -0.3135 0.068 Uiso 1 1 calc R . . C15 C 0.1541(4) 0.5467(2) -0.2995(4) 0.0692(16) Uani 1 1 d . . . H15A H 0.1754 0.5560 -0.3560 0.083 Uiso 1 1 calc R . . C16 C 0.1281(4) 0.5884(2) -0.2430(5) 0.075(2) Uani 1 1 d . . . C17 C 0.0959(4) 0.5740(2) -0.1623(5) 0.0701(17) Uani 1 1 d . . . H17A H 0.0761 0.6023 -0.1241 0.084 Uiso 1 1 calc R . . C18 C 0.0920(3) 0.5187(2) -0.1356(4) 0.0576(12) Uani 1 1 d . . . H18A H 0.0710 0.5096 -0.0789 0.069 Uiso 1 1 calc R . . C19 C 0.1194(4) 0.41785(19) -0.1598(3) 0.0517(11) Uani 1 1 d . . . H19A H 0.1842 0.4058 -0.1441 0.062 Uiso 1 1 calc R . . H19B H 0.0875 0.4158 -0.1041 0.062 Uiso 1 1 calc R . . C20 C 0.1360(5) 0.6488(3) -0.2688(7) 0.116(4) Uani 1 1 d . . . H20A H 0.1447 0.6716 -0.2131 0.139 Uiso 1 1 calc R . . H20B H 0.1911 0.6537 -0.3019 0.139 Uiso 1 1 calc R . . C21 C -0.0317(3) 0.33727(17) -0.3034(3) 0.0449(9) Uani 1 1 d . . . H21A H -0.0912 0.3246 -0.3269 0.054 Uiso 1 1 calc R . . C22 C 0.1122(3) 0.34578(19) -0.2816(4) 0.0519(11) Uani 1 1 d . . . H22A H 0.1768 0.3421 -0.2846 0.062 Uiso 1 1 calc R . . C23 C -0.0809(4) 0.6922(2) -0.3659(4) 0.0585(12) Uani 1 1 d . . . H23A H -0.1454 0.6985 -0.3663 0.070 Uiso 1 1 calc R . . C24 C 0.0516(3) 0.6906(2) -0.4069(5) 0.0648(15) Uani 1 1 d . . . H24A H 0.1035 0.6944 -0.4404 0.078 Uiso 1 1 calc R . . C25 C -0.2527(3) 0.07588(19) -0.3465(3) 0.0481(10) Uani 1 1 d . . . C26 C -0.1716(3) 0.0490(2) -0.3158(4) 0.0624(13) Uani 1 1 d . . . H26A H -0.1171 0.0701 -0.3002 0.075 Uiso 1 1 calc R . . C27 C -0.1691(3) -0.0081(2) -0.3074(4) 0.0552(11) Uani 1 1 d . . . H27A H -0.1126 -0.0259 -0.2863 0.066 Uiso 1 1 calc R . . C28 C -0.2469(3) -0.03980(17) -0.3291(3) 0.0419(9) Uani 1 1 d . . . C29 C -0.3285(3) -0.01312(19) -0.3600(3) 0.0482(10) Uani 1 1 d . . . H29A H -0.3832 -0.0343 -0.3740 0.058 Uiso 1 1 calc R . . C30 C -0.3313(3) 0.04423(19) -0.3706(4) 0.0502(10) Uani 1 1 d . . . H30A H -0.3870 0.0619 -0.3945 0.060 Uiso 1 1 calc R . . C31 C -0.2583(4) 0.1385(2) -0.3510(4) 0.0622(14) Uani 1 1 d . . . H31A H -0.3198 0.1495 -0.3806 0.075 Uiso 1 1 calc R . . H31B H -0.2523 0.1537 -0.2886 0.075 Uiso 1 1 calc R . . C32 C -0.2440(4) -0.10236(19) -0.3171(3) 0.0512(11) Uani 1 1 d . . . H32A H -0.1977 -0.1120 -0.2658 0.061 Uiso 1 1 calc R . . H32B H -0.3051 -0.1156 -0.3022 0.061 Uiso 1 1 calc R . . C33 C -0.1158(3) 0.18264(19) -0.5098(3) 0.0496(10) Uani 1 1 d . . . H33A H -0.0993 0.1866 -0.5698 0.059 Uiso 1 1 calc R . . C34 C -0.1103(3) 0.18930(18) -0.3693(3) 0.0481(10) Uani 1 1 d . . . H34A H -0.0926 0.1978 -0.3074 0.058 Uiso 1 1 calc R . . C35 C -0.2331(4) -0.1563(2) -0.5329(4) 0.0684(16) Uani 1 1 d . . . H35A H -0.2553 -0.1608 -0.5950 0.082 Uiso 1 1 calc R . . C36 C -0.1503(3) -0.16306(17) -0.4107(3) 0.0427(9) Uani 1 1 d . . . H36A H -0.1024 -0.1725 -0.3648 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02766(19) 0.0388(2) 0.0350(2) 0.00364(15) 0.00794(14) 0.00097(14) Cd2 0.03655(18) 0.03093(17) 0.0477(2) -0.00019(11) 0.00886(13) -0.00081(10) O1 0.063(2) 0.0512(19) 0.086(3) -0.0230(19) 0.033(2) -0.0186(18) O2 0.056(2) 0.111(4) 0.114(4) -0.056(3) 0.033(3) -0.043(2) O3 0.073(2) 0.0476(18) 0.0516(19) 0.0082(16) 0.0053(17) -0.0034(17) B1 0.053(3) 0.062(4) 0.112(6) -0.023(4) 0.008(4) 0.015(3) B2 0.056(3) 0.070(4) 0.050(3) 0.015(3) -0.009(2) -0.017(3) B3 0.086(5) 0.068(4) 0.088(5) -0.007(4) 0.042(4) 0.001(4) F1 0.073(3) 0.162(5) 0.201(6) -0.069(4) -0.016(3) 0.035(3) F2 0.156(5) 0.114(4) 0.109(4) -0.026(3) -0.028(3) 0.030(3) F3 0.107(3) 0.073(2) 0.196(5) 0.008(3) 0.058(3) 0.040(2) F4 0.204(7) 0.116(4) 0.160(6) 0.016(4) 0.040(5) 0.021(4) F5 0.237(7) 0.072(3) 0.171(5) 0.028(3) 0.081(5) 0.013(4) F6 0.067(3) 0.612(19) 0.130(5) -0.159(8) -0.048(3) 0.106(6) F7 0.069(2) 0.103(3) 0.138(4) -0.016(3) 0.013(2) -0.011(2) F8 0.148(4) 0.242(7) 0.056(2) 0.016(3) 0.002(2) -0.103(5) F9 0.180(6) 0.183(6) 0.098(3) 0.008(3) 0.045(4) 0.111(5) F10 0.237(11) 0.275(13) 0.233(11) -0.037(8) -0.004(8) 0.163(10) F11 0.318(15) 0.138(7) 0.391(17) -0.046(9) 0.064(13) -0.093(9) F12 0.109(8) 0.121(9) 0.163(12) -0.033(8) 0.092(8) -0.024(7) F12' 0.30(2) 0.159(12) 0.115(10) -0.021(9) 0.127(13) -0.091(16) N1 0.0281(16) 0.062(2) 0.055(2) 0.0160(18) 0.0105(14) 0.0037(16) N2 0.041(2) 0.060(3) 0.135(5) 0.019(3) 0.003(3) 0.007(2) N3 0.0293(16) 0.0450(18) 0.056(2) 0.0098(16) 0.0105(14) 0.0016(14) N4 0.0324(15) 0.0427(17) 0.0301(15) -0.0020(13) 0.0042(12) -0.0001(13) N5 0.058(2) 0.0464(19) 0.0347(17) 0.0070(15) 0.0058(15) 0.0020(17) N6 0.0339(16) 0.0403(17) 0.0373(16) 0.0031(13) 0.0071(13) 0.0008(13) N7 0.0452(19) 0.0365(17) 0.0470(19) 0.0015(15) 0.0026(15) 0.0001(14) N8 0.0423(19) 0.047(2) 0.061(2) -0.0085(17) 0.0126(17) -0.0020(16) N9 0.0404(18) 0.0382(17) 0.057(2) -0.0042(16) 0.0086(16) -0.0009(14) N10 0.061(3) 0.042(2) 0.098(4) 0.015(2) -0.036(3) -0.0120(19) N11 0.089(4) 0.066(3) 0.062(3) 0.015(2) -0.012(3) 0.002(3) N12 0.0397(18) 0.0392(18) 0.063(2) 0.0095(16) 0.0035(16) 0.0033(15) N13 0.044(2) 0.0382(18) 0.071(3) -0.0071(17) 0.0177(18) -0.0048(15) N14 0.051(2) 0.047(2) 0.072(3) -0.0038(19) 0.001(2) -0.0078(18) N15 0.0416(18) 0.0372(17) 0.055(2) 0.0004(15) 0.0129(16) -0.0037(14) N16 0.0436(18) 0.0430(18) 0.0404(17) -0.0011(14) 0.0040(14) 0.0052(15) N17 0.065(3) 0.080(3) 0.054(2) -0.016(2) -0.013(2) 0.033(2) N18 0.0398(18) 0.0401(17) 0.0438(18) -0.0037(14) 0.0003(14) 0.0046(14) C1 0.0215(16) 0.057(2) 0.0385(19) 0.0008(17) -0.0004(14) 0.0016(15) C2 0.046(2) 0.041(2) 0.055(2) -0.0004(19) 0.0089(19) -0.0054(18) C3 0.049(2) 0.043(2) 0.052(2) -0.0094(18) 0.0074(19) 0.0064(19) C4 0.031(2) 0.096(4) 0.044(2) 0.007(2) 0.0040(17) 0.000(2) C5 0.037(2) 0.049(3) 0.127(5) 0.011(3) 0.001(3) 0.004(2) C6 0.0337(19) 0.055(2) 0.048(2) 0.0066(19) 0.0106(17) 0.0045(17) C7 0.0326(18) 0.048(2) 0.0256(16) -0.0002(14) 0.0027(13) 0.0034(15) C8 0.065(3) 0.045(2) 0.049(2) 0.0012(19) -0.020(2) 0.012(2) C9 0.074(3) 0.037(2) 0.049(2) 0.0015(19) -0.017(2) -0.003(2) C10 0.0334(19) 0.071(3) 0.0324(19) -0.0047(19) 0.0056(15) -0.0020(19) C11 0.051(2) 0.041(2) 0.041(2) 0.0003(17) 0.0098(18) 0.0048(18) C12 0.0372(19) 0.042(2) 0.0364(19) 0.0037(16) 0.0041(15) -0.0001(16) C13 0.040(2) 0.039(2) 0.048(2) -0.0050(18) -0.0123(17) -0.0005(17) C14 0.061(3) 0.056(3) 0.047(2) 0.001(2) -0.018(2) -0.003(2) C15 0.068(3) 0.066(3) 0.065(3) 0.020(3) -0.033(3) -0.015(3) C16 0.057(3) 0.047(3) 0.110(5) 0.018(3) -0.051(3) -0.013(2) C17 0.051(3) 0.045(3) 0.108(5) -0.015(3) -0.019(3) 0.005(2) C18 0.041(2) 0.055(3) 0.076(3) -0.017(2) -0.002(2) 0.002(2) C19 0.062(3) 0.044(2) 0.047(2) -0.0024(19) -0.004(2) 0.002(2) C20 0.090(5) 0.048(3) 0.188(8) 0.039(4) -0.085(5) -0.022(3) C21 0.039(2) 0.038(2) 0.059(3) -0.0039(18) 0.0110(18) -0.0036(17) C22 0.043(2) 0.042(2) 0.070(3) -0.009(2) 0.003(2) 0.0028(18) C23 0.054(3) 0.059(3) 0.062(3) 0.015(2) 0.005(2) 0.008(2) C24 0.042(2) 0.038(2) 0.112(5) 0.018(3) -0.005(3) 0.0005(19) C25 0.039(2) 0.047(2) 0.062(3) -0.003(2) 0.0242(19) -0.0042(18) C26 0.040(2) 0.055(3) 0.092(4) -0.011(3) 0.008(2) -0.010(2) C27 0.042(2) 0.060(3) 0.063(3) 0.000(2) 0.003(2) 0.006(2) C28 0.051(2) 0.042(2) 0.0352(19) -0.0031(16) 0.0165(17) 0.0014(18) C29 0.042(2) 0.047(2) 0.056(3) -0.004(2) 0.0104(19) -0.0108(19) C30 0.038(2) 0.044(2) 0.070(3) 0.002(2) 0.014(2) -0.0008(18) C31 0.047(3) 0.046(2) 0.099(4) -0.007(3) 0.033(3) -0.005(2) C32 0.067(3) 0.046(2) 0.043(2) 0.0003(18) 0.016(2) 0.008(2) C33 0.054(3) 0.043(2) 0.052(2) -0.0039(19) 0.007(2) -0.0039(19) C34 0.046(2) 0.042(2) 0.057(3) -0.0014(19) 0.0096(19) -0.0074(18) C35 0.071(3) 0.078(4) 0.051(3) -0.022(3) -0.020(2) 0.037(3) C36 0.045(2) 0.038(2) 0.044(2) 0.0034(17) 0.0002(17) 0.0027(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.282(3) 3 ? Cd1 N3 2.282(3) . ? Cd1 O1 2.321(3) . ? Cd1 O1 2.321(3) 3 ? Cd1 N6 2.363(3) . ? Cd1 N6 2.363(3) 3 ? Cd2 N9 2.289(4) . ? Cd2 N12 2.302(4) 3_564 ? Cd2 N18 2.303(3) 3_554 ? Cd2 N15 2.319(3) . ? Cd2 O3 2.350(3) . ? Cd2 O2 2.369(4) . ? O1 HW1 0.83(4) . ? O1 HW2 0.89(4) . ? O2 HW3 0.89(4) . ? O2 HW4 0.84(4) . ? O3 HW5 0.87(4) . ? O3 HW6 0.87(4) . ? B1 F3 1.343(6) . ? B1 F2 1.346(6) . ? B1 F1 1.365(6) . ? B1 F4 1.383(7) . ? B2 F6 1.305(6) . ? B2 F8 1.339(6) . ? B2 F5 1.353(6) . ? B2 F7 1.419(6) . ? B3 F11 1.333(7) . ? B3 F12 1.338(8) . ? B3 F9 1.343(6) . ? B3 F12' 1.361(9) . ? B3 F10 1.367(8) . ? F12 F12' 1.090(19) . ? N1 C6 1.310(6) . ? N1 N2 1.324(6) . ? N1 C4 1.471(6) . ? N2 C5 1.328(7) . ? N3 C6 1.328(6) . ? N3 C5 1.337(6) . ? N4 C12 1.329(5) . ? N4 N5 1.346(5) . ? N4 C10 1.492(5) . ? N5 C11 1.323(5) . ? N6 C12 1.329(5) . ? N6 C11 1.349(5) . ? N7 C22 1.304(6) . ? N7 N8 1.360(5) . ? N7 C19 1.467(6) . ? N8 C21 1.306(6) . ? N9 C22 1.336(6) . ? N9 C21 1.356(5) . ? N10 C24 1.307(8) . ? N10 N11 1.351(8) . ? N10 C20 1.476(7) . ? N11 C23 1.301(7) . ? N12 C24 1.328(6) . ? N12 C23 1.339(6) . ? N12 Cd2 2.302(4) 3_564 ? N13 C34 1.329(6) . ? N13 N14 1.362(6) . ? N13 C31 1.451(6) . ? N14 C33 1.301(6) . ? N15 C34 1.319(6) . ? N15 C33 1.351(6) . ? N16 C36 1.313(6) . ? N16 N17 1.349(5) . ? N16 C32 1.461(5) . ? N17 C35 1.312(6) . ? N18 C36 1.324(5) . ? N18 C35 1.343(6) . ? N18 Cd2 2.303(3) 3_554 ? C1 C2 1.378(6) . ? C1 C3 1.382(6) . ? C1 C4 1.489(6) . ? C2 C3 1.390(7) 3_455 ? C2 H2A 0.9500 . ? C3 C2 1.390(7) 3_455 ? C3 H3A 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.375(6) . ? C7 C9 1.376(6) . ? C7 C10 1.509(5) . ? C8 C9 1.390(6) 3_554 ? C8 H8A 0.9500 . ? C9 C8 1.390(6) 3_554 ? C9 H9A 0.9500 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.382(7) . ? C13 C18 1.391(7) . ? C13 C19 1.497(6) . ? C14 C15 1.383(7) . ? C14 H14A 0.9500 . ? C15 C16 1.384(10) . ? C15 H15A 0.9500 . ? C16 C17 1.375(10) . ? C16 C20 1.510(8) . ? C17 C18 1.388(8) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.380(7) . ? C25 C30 1.388(6) . ? C25 C31 1.509(7) . ? C26 C27 1.380(7) . ? C26 H26A 0.9500 . ? C27 C28 1.373(7) . ? C27 H27A 0.9500 . ? C28 C29 1.385(7) . ? C28 C32 1.514(6) . ? C29 C30 1.388(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? 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 N3 Cd1 N3 180.0(3) 3 . ? N3 Cd1 O1 91.21(14) 3 . ? N3 Cd1 O1 88.79(14) . . ? N3 Cd1 O1 88.79(14) 3 3 ? N3 Cd1 O1 91.21(14) . 3 ? O1 Cd1 O1 180.00(19) . 3 ? N3 Cd1 N6 90.23(12) 3 . ? N3 Cd1 N6 89.77(12) . . ? O1 Cd1 N6 89.86(13) . . ? O1 Cd1 N6 90.14(13) 3 . ? N3 Cd1 N6 89.77(12) 3 3 ? N3 Cd1 N6 90.23(12) . 3 ? O1 Cd1 N6 90.14(13) . 3 ? O1 Cd1 N6 89.86(13) 3 3 ? N6 Cd1 N6 180.0(2) . 3 ? N9 Cd2 N12 98.82(14) . 3_564 ? N9 Cd2 N18 161.76(13) . 3_554 ? N12 Cd2 N18 91.53(13) 3_564 3_554 ? N9 Cd2 N15 97.77(13) . . ? N12 Cd2 N15 91.18(13) 3_564 . ? N18 Cd2 N15 96.99(13) 3_554 . ? N9 Cd2 O3 84.16(13) . . ? N12 Cd2 O3 175.35(13) 3_564 . ? N18 Cd2 O3 84.69(13) 3_554 . ? N15 Cd2 O3 91.96(14) . . ? N9 Cd2 O2 83.82(14) . . ? N12 Cd2 O2 88.9(2) 3_564 . ? N18 Cd2 O2 81.39(15) 3_554 . ? N15 Cd2 O2 178.37(14) . . ? O3 Cd2 O2 87.9(2) . . ? Cd1 O1 HW1 119(4) . . ? Cd1 O1 HW2 122(4) . . ? HW1 O1 HW2 105(5) . . ? Cd2 O2 HW3 134(5) . . ? Cd2 O2 HW4 104(4) . . ? HW3 O2 HW4 116(5) . . ? Cd2 O3 HW5 111(4) . . ? Cd2 O3 HW6 117(4) . . ? HW5 O3 HW6 101(4) . . ? F3 B1 F2 112.3(5) . . ? F3 B1 F1 109.9(5) . . ? F2 B1 F1 112.2(5) . . ? F3 B1 F4 109.5(5) . . ? F2 B1 F4 106.8(5) . . ? F1 B1 F4 105.9(6) . . ? F6 B2 F8 112.9(5) . . ? F6 B2 F5 115.3(6) . . ? F8 B2 F5 110.7(5) . . ? F6 B2 F7 107.1(5) . . ? F8 B2 F7 106.4(5) . . ? F5 B2 F7 103.4(4) . . ? F11 B3 F12 126.4(9) . . ? F11 B3 F9 110.1(7) . . ? F12 B3 F9 111.3(8) . . ? F11 B3 F12' 90.1(10) . . ? F12 B3 F12' 47.6(9) . . ? F9 B3 F12' 104.4(10) . . ? F11 B3 F10 106.9(7) . . ? F12 B3 F10 90.1(10) . . ? F9 B3 F10 109.0(6) . . ? F12' B3 F10 133.8(12) . . ? F12' F12 B3 67.3(6) . . ? F12 F12' B3 65.1(8) . . ? C6 N1 N2 110.9(4) . . ? C6 N1 C4 128.7(4) . . ? N2 N1 C4 120.4(4) . . ? N1 N2 C5 102.0(4) . . ? C6 N3 C5 101.8(4) . . ? C6 N3 Cd1 127.7(3) . . ? C5 N3 Cd1 130.3(3) . . ? C12 N4 N5 110.3(3) . . ? C12 N4 C10 127.7(4) . . ? N5 N4 C10 122.0(3) . . ? C11 N5 N4 102.8(3) . . ? C12 N6 C11 103.5(3) . . ? C12 N6 Cd1 127.6(3) . . ? C11 N6 Cd1 128.8(3) . . ? C22 N7 N8 110.4(4) . . ? C22 N7 C19 128.6(4) . . ? N8 N7 C19 121.0(4) . . ? C21 N8 N7 102.3(4) . . ? C22 N9 C21 102.1(4) . . ? C22 N9 Cd2 123.9(3) . . ? C21 N9 Cd2 133.8(3) . . ? C24 N10 N11 110.5(4) . . ? C24 N10 C20 126.7(7) . . ? N11 N10 C20 122.7(6) . . ? C23 N11 N10 102.1(5) . . ? C24 N12 C23 102.6(4) . . ? C24 N12 Cd2 125.6(4) . 3_564 ? C23 N12 Cd2 131.7(3) . 3_564 ? C34 N13 N14 109.8(4) . . ? C34 N13 C31 129.4(5) . . ? N14 N13 C31 120.7(4) . . ? C33 N14 N13 102.1(4) . . ? C34 N15 C33 102.7(4) . . ? C34 N15 Cd2 128.2(3) . . ? C33 N15 Cd2 129.1(3) . . ? C36 N16 N17 109.8(4) . . ? C36 N16 C32 129.7(4) . . ? N17 N16 C32 120.4(4) . . ? C35 N17 N16 102.5(4) . . ? C36 N18 C35 102.4(4) . . ? C36 N18 Cd2 134.1(3) . 3_554 ? C35 N18 Cd2 122.7(3) . 3_554 ? C2 C1 C3 118.7(4) . . ? C2 C1 C4 120.7(4) . . ? C3 C1 C4 120.5(4) . . ? C1 C2 C3 120.3(4) . 3_455 ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 3_455 . ? C1 C3 C2 120.9(4) . 3_455 ? C1 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 3_455 . ? N1 C4 C1 111.8(4) . . ? N1 C4 H4A 109.3 . . ? C1 C4 H4A 109.3 . . ? N1 C4 H4B 109.3 . . ? C1 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N2 C5 N3 114.9(5) . . ? N2 C5 H5A 122.6 . . ? N3 C5 H5A 122.6 . . ? N1 C6 N3 110.4(4) . . ? N1 C6 H6A 124.8 . . ? N3 C6 H6A 124.8 . . ? C8 C7 C9 118.6(4) . . ? C8 C7 C10 119.9(4) . . ? C9 C7 C10 121.5(4) . . ? C7 C8 C9 120.8(4) . 3_554 ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 3_554 . ? C7 C9 C8 120.6(4) . 3_554 ? C7 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 3_554 . ? N4 C10 C7 112.1(3) . . ? N4 C10 H10A 109.2 . . ? C7 C10 H10A 109.2 . . ? N4 C10 H10B 109.2 . . ? C7 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N5 C11 N6 113.9(4) . . ? N5 C11 H11A 123.1 . . ? N6 C11 H11A 123.1 . . ? N4 C12 N6 109.5(4) . . ? N4 C12 H12A 125.3 . . ? N6 C12 H12A 125.3 . . ? C14 C13 C18 118.8(5) . . ? C14 C13 C19 122.0(4) . . ? C18 C13 C19 119.0(5) . . ? C13 C14 C15 121.0(5) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C14 C15 C16 120.2(6) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 119.0(5) . . ? C17 C16 C20 120.3(7) . . ? C15 C16 C20 120.7(8) . . ? C16 C17 C18 121.1(6) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C17 C18 C13 119.8(6) . . ? C17 C18 H18A 120.1 . . ? C13 C18 H18A 120.1 . . ? N7 C19 C13 112.8(4) . . ? N7 C19 H19A 109.0 . . ? C13 C19 H19A 109.0 . . ? N7 C19 H19B 109.0 . . ? C13 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? N10 C20 C16 112.4(4) . . ? N10 C20 H20A 109.1 . . ? C16 C20 H20A 109.1 . . ? N10 C20 H20B 109.1 . . ? C16 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? N8 C21 N9 114.8(4) . . ? N8 C21 H21A 122.6 . . ? N9 C21 H21A 122.6 . . ? N7 C22 N9 110.4(4) . . ? N7 C22 H22A 124.8 . . ? N9 C22 H22A 124.8 . . ? N11 C23 N12 115.1(5) . . ? N11 C23 H23A 122.4 . . ? N12 C23 H23A 122.4 . . ? N10 C24 N12 109.7(5) . . ? N10 C24 H24A 125.2 . . ? N12 C24 H24A 125.2 . . ? C26 C25 C30 118.8(4) . . ? C26 C25 C31 121.4(4) . . ? C30 C25 C31 119.7(4) . . ? C27 C26 C25 120.6(5) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C28 C27 C26 121.1(5) . . ? C28 C27 H27A 119.4 . . ? C26 C27 H27A 119.4 . . ? C27 C28 C29 118.6(4) . . ? C27 C28 C32 120.7(4) . . ? C29 C28 C32 120.7(4) . . ? C28 C29 C30 120.8(4) . . ? C28 C29 H29A 119.6 . . ? C30 C29 H29A 119.6 . . ? C29 C30 C25 120.1(4) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? N13 C31 C25 112.5(4) . . ? N13 C31 H31A 109.1 . . ? C25 C31 H31A 109.1 . . ? N13 C31 H31B 109.1 . . ? C25 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? N16 C32 C28 111.5(4) . . ? N16 C32 H32A 109.3 . . ? C28 C32 H32A 109.3 . . ? N16 C32 H32B 109.3 . . ? C28 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? N14 C33 N15 115.3(4) . . ? N14 C33 H33A 122.3 . . ? N15 C33 H33A 122.3 . . ? N15 C34 N13 110.0(4) . . ? N15 C34 H34A 125.0 . . ? N13 C34 H34A 125.0 . . ? N17 C35 N18 114.7(4) . . ? N17 C35 H35A 122.6 . . ? N18 C35 H35A 122.6 . . ? N16 C36 N18 110.6(4) . . ? N16 C36 H36A 124.7 . . ? N18 C36 H36A 124.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F11 B3 F12 F12' 48.0(18) . . . . ? F9 B3 F12 F12' -90.3(14) . . . . ? F10 B3 F12 F12' 159.2(14) . . . . ? F11 B3 F12' F12 -143.3(14) . . . . ? F9 B3 F12' F12 105.9(13) . . . . ? F10 B3 F12' F12 -29.4(19) . . . . ? C6 N1 N2 C5 -2.2(6) . . . . ? C4 N1 N2 C5 176.8(5) . . . . ? N3 Cd1 N3 C6 150(100) 3 . . . ? O1 Cd1 N3 C6 -165.9(4) . . . . ? O1 Cd1 N3 C6 14.1(4) 3 . . . ? N6 Cd1 N3 C6 104.3(4) . . . . ? N6 Cd1 N3 C6 -75.7(4) 3 . . . ? N3 Cd1 N3 C5 -23(100) 3 . . . ? O1 Cd1 N3 C5 20.8(5) . . . . ? O1 Cd1 N3 C5 -159.2(5) 3 . . . ? N6 Cd1 N3 C5 -69.0(5) . . . . ? N6 Cd1 N3 C5 111.0(5) 3 . . . ? C12 N4 N5 C11 -1.0(4) . . . . ? C10 N4 N5 C11 179.1(3) . . . . ? N3 Cd1 N6 C12 62.6(3) 3 . . . ? N3 Cd1 N6 C12 -117.4(3) . . . . ? O1 Cd1 N6 C12 153.8(3) . . . . ? O1 Cd1 N6 C12 -26.2(3) 3 . . . ? N6 Cd1 N6 C12 -74(100) 3 . . . ? N3 Cd1 N6 C11 -122.4(4) 3 . . . ? N3 Cd1 N6 C11 57.6(4) . . . . ? O1 Cd1 N6 C11 -31.2(4) . . . . ? O1 Cd1 N6 C11 148.8(4) 3 . . . ? N6 Cd1 N6 C11 101(100) 3 . . . ? C22 N7 N8 C21 0.8(5) . . . . ? C19 N7 N8 C21 -178.7(4) . . . . ? N12 Cd2 N9 C22 -109.7(4) 3_564 . . . ? N18 Cd2 N9 C22 14.1(7) 3_554 . . . ? N15 Cd2 N9 C22 157.8(4) . . . . ? O3 Cd2 N9 C22 66.6(4) . . . . ? O2 Cd2 N9 C22 -21.8(4) . . . . ? N12 Cd2 N9 C21 75.8(4) 3_564 . . . ? N18 Cd2 N9 C21 -160.3(4) 3_554 . . . ? N15 Cd2 N9 C21 -16.6(4) . . . . ? O3 Cd2 N9 C21 -107.8(4) . . . . ? O2 Cd2 N9 C21 163.7(5) . . . . ? C24 N10 N11 C23 -1.0(6) . . . . ? C20 N10 N11 C23 176.5(5) . . . . ? C34 N13 N14 C33 -0.2(5) . . . . ? C31 N13 N14 C33 -178.0(4) . . . . ? N9 Cd2 N15 C34 -44.5(4) . . . . ? N12 Cd2 N15 C34 -143.5(4) 3_564 . . . ? N18 Cd2 N15 C34 124.8(4) 3_554 . . . ? O3 Cd2 N15 C34 39.9(4) . . . . ? O2 Cd2 N15 C34 123(7) . . . . ? N9 Cd2 N15 C33 134.9(4) . . . . ? N12 Cd2 N15 C33 35.9(4) 3_564 . . . ? N18 Cd2 N15 C33 -55.8(4) 3_554 . . . ? O3 Cd2 N15 C33 -140.7(4) . . . . ? O2 Cd2 N15 C33 -57(7) . . . . ? C36 N16 N17 C35 -0.4(6) . . . . ? C32 N16 N17 C35 -179.2(5) . . . . ? C3 C1 C2 C3 -0.4(7) . . . 3_455 ? C4 C1 C2 C3 178.6(4) . . . 3_455 ? C2 C1 C3 C2 0.4(7) . . . 3_455 ? C4 C1 C3 C2 -178.6(4) . . . 3_455 ? C6 N1 C4 C1 87.8(6) . . . . ? N2 N1 C4 C1 -91.1(6) . . . . ? C2 C1 C4 N1 70.6(6) . . . . ? C3 C1 C4 N1 -110.4(5) . . . . ? N1 N2 C5 N3 1.0(8) . . . . ? C6 N3 C5 N2 0.5(7) . . . . ? Cd1 N3 C5 N2 175.1(4) . . . . ? N2 N1 C6 N3 2.8(6) . . . . ? C4 N1 C6 N3 -176.1(4) . . . . ? C5 N3 C6 N1 -1.9(5) . . . . ? Cd1 N3 C6 N1 -176.7(3) . . . . ? C9 C7 C8 C9 1.3(9) . . . 3_554 ? C10 C7 C8 C9 -178.1(5) . . . 3_554 ? C8 C7 C9 C8 -1.3(9) . . . 3_554 ? C10 C7 C9 C8 178.1(5) . . . 3_554 ? C12 N4 C10 C7 95.5(5) . . . . ? N5 N4 C10 C7 -84.6(5) . . . . ? C8 C7 C10 N4 -102.7(5) . . . . ? C9 C7 C10 N4 77.9(5) . . . . ? N4 N5 C11 N6 0.6(5) . . . . ? C12 N6 C11 N5 0.0(5) . . . . ? Cd1 N6 C11 N5 -175.9(3) . . . . ? N5 N4 C12 N6 1.0(5) . . . . ? C10 N4 C12 N6 -179.0(3) . . . . ? C11 N6 C12 N4 -0.6(4) . . . . ? Cd1 N6 C12 N4 175.4(2) . . . . ? C18 C13 C14 C15 0.8(7) . . . . ? C19 C13 C14 C15 -175.4(4) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? C14 C15 C16 C17 -1.1(7) . . . . ? C14 C15 C16 C20 178.1(5) . . . . ? C15 C16 C17 C18 2.1(8) . . . . ? C20 C16 C17 C18 -177.2(5) . . . . ? C16 C17 C18 C13 -1.6(7) . . . . ? C14 C13 C18 C17 0.1(7) . . . . ? C19 C13 C18 C17 176.4(5) . . . . ? C22 N7 C19 C13 101.3(6) . . . . ? N8 N7 C19 C13 -79.3(5) . . . . ? C14 C13 C19 N7 -51.3(6) . . . . ? C18 C13 C19 N7 132.5(4) . . . . ? C24 N10 C20 C16 -122.4(8) . . . . ? N11 N10 C20 C16 60.5(10) . . . . ? C17 C16 C20 N10 -94.4(8) . . . . ? C15 C16 C20 N10 86.3(9) . . . . ? N7 N8 C21 N9 -0.7(5) . . . . ? C22 N9 C21 N8 0.3(5) . . . . ? Cd2 N9 C21 N8 175.6(3) . . . . ? N8 N7 C22 N9 -0.7(5) . . . . ? C19 N7 C22 N9 178.8(4) . . . . ? C21 N9 C22 N7 0.3(5) . . . . ? Cd2 N9 C22 N7 -175.6(3) . . . . ? N10 N11 C23 N12 0.6(7) . . . . ? C24 N12 C23 N11 0.0(6) . . . . ? Cd2 N12 C23 N11 -177.3(4) 3_564 . . . ? N11 N10 C24 N12 1.1(6) . . . . ? C20 N10 C24 N12 -176.2(5) . . . . ? C23 N12 C24 N10 -0.7(6) . . . . ? Cd2 N12 C24 N10 176.8(3) 3_564 . . . ? C30 C25 C26 C27 -1.3(8) . . . . ? C31 C25 C26 C27 176.3(5) . . . . ? C25 C26 C27 C28 -0.2(8) . . . . ? C26 C27 C28 C29 0.2(7) . . . . ? C26 C27 C28 C32 -178.2(5) . . . . ? C27 C28 C29 C30 1.3(7) . . . . ? C32 C28 C29 C30 179.7(4) . . . . ? C28 C29 C30 C25 -2.8(7) . . . . ? C26 C25 C30 C29 2.8(7) . . . . ? C31 C25 C30 C29 -174.9(5) . . . . ? C34 N13 C31 C25 -104.8(6) . . . . ? N14 N13 C31 C25 72.5(6) . . . . ? C26 C25 C31 N13 52.9(7) . . . . ? C30 C25 C31 N13 -129.5(5) . . . . ? C36 N16 C32 C28 119.9(5) . . . . ? N17 N16 C32 C28 -61.7(6) . . . . ? C27 C28 C32 N16 -90.3(5) . . . . ? C29 C28 C32 N16 91.3(5) . . . . ? N13 N14 C33 N15 0.9(5) . . . . ? C34 N15 C33 N14 -1.3(5) . . . . ? Cd2 N15 C33 N14 179.2(3) . . . . ? C33 N15 C34 N13 1.0(5) . . . . ? Cd2 N15 C34 N13 -179.4(3) . . . . ? N14 N13 C34 N15 -0.5(5) . . . . ? C31 N13 C34 N15 177.0(4) . . . . ? N16 N17 C35 N18 0.9(7) . . . . ? C36 N18 C35 N17 -1.0(7) . . . . ? Cd2 N18 C35 N17 170.3(4) 3_554 . . . ? N17 N16 C36 N18 -0.2(5) . . . . ? C32 N16 C36 N18 178.4(4) . . . . ? C35 N18 C36 N16 0.7(5) . . . . ? Cd2 N18 C36 N16 -169.1(3) 3_554 . . . ? 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 O1 HW1 F1 0.83(4) 1.87(4) 2.687(6) 166(7) 4_565 O1 HW2 F8 0.89(4) 1.87(4) 2.764(6) 174(6) 2_545 O2 HW3 F5 0.89(4) 2.13(4) 2.984(10) 159(7) 3_665 O2 HW3 F8 0.89(4) 2.34(7) 3.042(6) 135(7) 3_665 O2 HW4 F12 0.84(4) 1.84(5) 2.627(11) 155(6) 2_544 O2 HW4 F12' 0.84(4) 2.22(6) 2.805(15) 126(5) 2_544 O3 HW5 N5 0.87(4) 2.19(7) 2.885(5) 136(10) . O3 HW6 O4 0.87(4) 1.97(5) 2.788(9) 155(6) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.163 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.111 ###=========================== data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 256592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 B2 Cd F8 N15 O5' _chemical_formula_weight 1021.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9995(4) _cell_length_b 11.6029(5) _cell_length_c 20.2826(10) _cell_angle_alpha 82.925(3) _cell_angle_beta 88.436(3) _cell_angle_gamma 77.008(2) _cell_volume 2275.55(17) _cell_formula_units_Z 2 _cell_measurement_temperature 193.15 _cell_measurement_reflns_used 8877 _cell_measurement_theta_min 3.0312 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7265 _exptl_absorpt_correction_T_max 0.8479 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 193.15 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22439 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8259 _reflns_number_gt 7779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.9800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8259 _refine_ls_number_parameters 600 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.492276(19) 0.271784(19) 0.246279(10) 0.02603(10) Uani 1 1 d . . . B1 B 0.0616(3) 0.0955(3) 0.16048(17) 0.0275(7) Uani 1 1 d . . . B2 B -0.0524(4) 0.4151(4) 0.3590(2) 0.0377(9) Uani 1 1 d . . . F1 F 0.1454(3) 0.1302(3) 0.20559(15) 0.0876(9) Uani 1 1 d . . . F2 F 0.1422(4) 0.0543(3) 0.11064(15) 0.0916(10) Uani 1 1 d . . . F3 F -0.0403(3) 0.1920(3) 0.1399(2) 0.0944(11) Uani 1 1 d . . . F4 F 0.0010(3) 0.0104(2) 0.19345(14) 0.0703(7) Uani 1 1 d . . . F5 F -0.0062(4) 0.4377(4) 0.4191(2) 0.1181(13) Uani 1 1 d . . . F6 F 0.0499(3) 0.3218(2) 0.33978(15) 0.0752(8) Uani 1 1 d . . . F7 F -0.1610(4) 0.3727(6) 0.3782(3) 0.164(2) Uani 1 1 d . . . F8 F -0.0543(7) 0.5091(3) 0.3170(2) 0.180(3) Uani 1 1 d . . . O1 O 0.3491(2) 0.1462(2) 0.29350(13) 0.0400(6) Uani 1 1 d D . . HW1 H 0.281(3) 0.142(4) 0.2737(16) 0.048(12) Uiso 1 1 d D . . HW2 H 0.334(4) 0.141(4) 0.3345(12) 0.057(13) Uiso 1 1 d D . . O2 O 0.6384(3) 0.3851(2) 0.19537(12) 0.0388(5) Uani 1 1 d D . . HW3 H 0.608(4) 0.455(2) 0.2009(18) 0.049(12) Uiso 1 1 d D . . HW4 H 0.645(4) 0.381(3) 0.1548(13) 0.054(13) Uiso 1 1 d D . . O3 O 0.5215(4) 0.6092(3) 0.21613(18) 0.0792(10) Uani 1 1 d . . . O4 O 0.6370(3) 0.3799(3) 0.06155(13) 0.0591(7) Uani 1 1 d . . . O5 O 0.3399(3) 0.1286(3) 0.42612(13) 0.0564(7) Uani 1 1 d . . . N1 N 0.8732(3) 0.0805(2) 0.35241(13) 0.0292(5) Uani 1 1 d . . . N2 N 0.7849(3) 0.0405(3) 0.39730(13) 0.0358(6) Uani 1 1 d . . . N3 N 0.6711(3) 0.1563(2) 0.31095(12) 0.0299(5) Uani 1 1 d . . . N4 N 1.3461(3) -0.5050(2) 0.40950(12) 0.0287(5) Uani 1 1 d . . . N5 N 1.4775(3) -0.4893(3) 0.40536(14) 0.0375(6) Uani 1 1 d . . . N6 N 1.4427(3) -0.6096(2) 0.33229(12) 0.0290(5) Uani 1 1 d . . . N7 N 0.0975(3) 0.4416(2) 0.14685(13) 0.0293(5) Uani 1 1 d . . . N8 N 0.1798(3) 0.4617(3) 0.09390(13) 0.0401(7) Uani 1 1 d . . . N9 N 0.3050(3) 0.3750(2) 0.18346(13) 0.0308(6) Uani 1 1 d . . . N10 N -0.3433(3) 1.0403(2) 0.08938(13) 0.0316(6) Uani 1 1 d . . . N11 N -0.4755(3) 1.0268(3) 0.08663(14) 0.0401(7) Uani 1 1 d . . . N12 N -0.4535(3) 1.1488(2) 0.16133(12) 0.0281(5) Uani 1 1 d . . . N13 N 0.5208(4) 0.7832(3) 0.25258(17) 0.0598(9) Uani 1 1 d . . . N14 N 0.6824(3) 0.2911(3) -0.03219(15) 0.0463(7) Uani 1 1 d . . . N15 N 0.3068(3) 0.2268(3) 0.51699(15) 0.0434(7) Uani 1 1 d . . . C1 C 1.0791(3) -0.0754(3) 0.38794(17) 0.0330(7) Uani 1 1 d . . . C2 C 1.1377(3) -0.1096(3) 0.45004(17) 0.0373(7) Uani 1 1 d . . . H2A H 1.1399 -0.0510 0.4785 0.045 Uiso 1 1 calc R . . C3 C 1.1934(3) -0.2286(3) 0.47149(16) 0.0344(7) Uani 1 1 d . . . H3A H 1.2331 -0.2507 0.5145 0.041 Uiso 1 1 calc R . . C4 C 1.1913(3) -0.3149(3) 0.43073(15) 0.0300(6) Uani 1 1 d . . . C5 C 1.1323(4) -0.2808(3) 0.36817(17) 0.0426(8) Uani 1 1 d . . . H5A H 1.1296 -0.3394 0.3397 0.051 Uiso 1 1 calc R . . C6 C 1.0772(4) -0.1617(3) 0.34689(17) 0.0441(8) Uani 1 1 d . . . H6A H 1.0379 -0.1393 0.3038 0.053 Uiso 1 1 calc R . . C7 C 1.0211(3) 0.0545(3) 0.3651(2) 0.0430(8) Uani 1 1 d . . . H7A H 1.0393 0.1027 0.3994 0.052 Uiso 1 1 calc R . . H7B H 1.0686 0.0782 0.3239 0.052 Uiso 1 1 calc R . . C8 C 1.2478(4) -0.4449(3) 0.45600(16) 0.0348(7) Uani 1 1 d . . . H8A H 1.2935 -0.4503 0.4993 0.042 Uiso 1 1 calc R . . H8B H 1.1709 -0.4859 0.4631 0.042 Uiso 1 1 calc R . . C9 C 0.6649(3) 0.0885(3) 0.37016(16) 0.0338(7) Uani 1 1 d . . . H9A H 0.5810 0.0769 0.3900 0.041 Uiso 1 1 calc R . . C10 C 0.8040(3) 0.1490(3) 0.30214(15) 0.0299(6) Uani 1 1 d . . . H10A H 0.8438 0.1873 0.2651 0.036 Uiso 1 1 calc R . . C11 C 1.5302(3) -0.5539(3) 0.35860(16) 0.0366(7) Uani 1 1 d . . . H11A H 1.6226 -0.5612 0.3442 0.044 Uiso 1 1 calc R . . C12 C 1.3281(3) -0.5762(3) 0.36556(15) 0.0293(6) Uani 1 1 d . . . H12A H 1.2448 -0.5996 0.3590 0.035 Uiso 1 1 calc R . . C13 C -0.1033(3) 0.6043(3) 0.11753(16) 0.0307(7) Uani 1 1 d . . . C14 C -0.1534(4) 0.6412(3) 0.05436(18) 0.0425(8) Uani 1 1 d . . . H14A H -0.1581 0.5837 0.0255 0.051 Uiso 1 1 calc R . . C15 C -0.1974(4) 0.7617(3) 0.03205(17) 0.0429(8) Uani 1 1 d . . . H15A H -0.2320 0.7859 -0.0118 0.051 Uiso 1 1 calc R . . C16 C -0.1911(3) 0.8458(3) 0.07315(16) 0.0344(7) Uani 1 1 d . . . C17 C -0.1391(4) 0.8088(3) 0.13704(18) 0.0426(8) Uani 1 1 d . . . H17A H -0.1330 0.8664 0.1656 0.051 Uiso 1 1 calc R . . C18 C -0.0963(4) 0.6897(3) 0.15913(17) 0.0404(8) Uani 1 1 d . . . H18A H -0.0618 0.6654 0.2030 0.048 Uiso 1 1 calc R . . C19 C -0.0529(3) 0.4737(3) 0.14127(19) 0.0389(8) Uani 1 1 d . . . H19A H -0.0939 0.4548 0.1851 0.047 Uiso 1 1 calc R . . H19B H -0.0827 0.4258 0.1097 0.047 Uiso 1 1 calc R . . C20 C -0.2350(4) 0.9770(3) 0.04802(18) 0.0462(9) Uani 1 1 d . . . H20A H -0.1545 1.0136 0.0475 0.055 Uiso 1 1 calc R . . H20B H -0.2688 0.9860 0.0018 0.055 Uiso 1 1 calc R . . C21 C 0.3035(3) 0.4198(3) 0.11856(16) 0.0368(7) Uani 1 1 d . . . H21A H 0.3846 0.4207 0.0932 0.044 Uiso 1 1 calc R . . C22 C 0.1743(3) 0.3907(3) 0.19902(16) 0.0317(7) Uani 1 1 d . . . H22A H 0.1399 0.3685 0.2417 0.038 Uiso 1 1 calc R . . C23 C -0.5370(3) 1.0955(3) 0.13040(16) 0.0333(7) Uani 1 1 d . . . H23A H -0.6324 1.1068 0.1396 0.040 Uiso 1 1 calc R . . C24 C -0.3328(3) 1.1118(3) 0.13417(15) 0.0303(6) Uani 1 1 d . . . H24A H -0.2505 1.1332 0.1451 0.036 Uiso 1 1 calc R . . C25 C 0.3799(7) 0.8299(6) 0.2437(5) 0.131(3) Uani 1 1 d . . . H25A H 0.3635 0.8771 0.2000 0.197 Uiso 1 1 calc R . . H25B H 0.3455 0.8808 0.2784 0.197 Uiso 1 1 calc R . . H25C H 0.3319 0.7645 0.2465 0.197 Uiso 1 1 calc R . . C26 C 0.5998(7) 0.8640(5) 0.2739(3) 0.0885(18) Uani 1 1 d . . . H26A H 0.6930 0.8194 0.2859 0.133 Uiso 1 1 calc R . . H26B H 0.5553 0.8996 0.3125 0.133 Uiso 1 1 calc R . . H26C H 0.6040 0.9271 0.2376 0.133 Uiso 1 1 calc R . . C27 C 0.5807(6) 0.6778(4) 0.2380(2) 0.0649(12) Uani 1 1 d . . . H27A H 0.6769 0.6523 0.2449 0.078 Uiso 1 1 calc R . . C28 C 0.7839(6) 0.2485(5) -0.0812(2) 0.0710(14) Uani 1 1 d . . . H28A H 0.8760 0.2439 -0.0642 0.106 Uiso 1 1 calc R . . H28B H 0.7684 0.3035 -0.1224 0.106 Uiso 1 1 calc R . . H28C H 0.7759 0.1692 -0.0901 0.106 Uiso 1 1 calc R . . C29 C 0.5404(5) 0.2897(5) -0.0433(2) 0.0677(12) Uani 1 1 d . . . H29A H 0.4854 0.3150 -0.0047 0.102 Uiso 1 1 calc R . . H29B H 0.5335 0.2089 -0.0496 0.102 Uiso 1 1 calc R . . H29C H 0.5062 0.3444 -0.0830 0.102 Uiso 1 1 calc R . . C30 C 0.7173(4) 0.3376(3) 0.01932(18) 0.0476(9) Uani 1 1 d . . . H30A H 0.8114 0.3385 0.0240 0.057 Uiso 1 1 calc R . . C31 C 0.2101(5) 0.2802(4) 0.5648(2) 0.0669(12) Uani 1 1 d . . . H31A H 0.1184 0.3050 0.5449 0.100 Uiso 1 1 calc R . . H31B H 0.2379 0.3499 0.5780 0.100 Uiso 1 1 calc R . . H31C H 0.2085 0.2220 0.6040 0.100 Uiso 1 1 calc R . . C32 C 0.4522(5) 0.2170(5) 0.5270(2) 0.0651(12) Uani 1 1 d . . . H32A H 0.4921 0.1395 0.5519 0.098 Uiso 1 1 calc R . . H32B H 0.4649 0.2807 0.5521 0.098 Uiso 1 1 calc R . . H32C H 0.4979 0.2241 0.4838 0.098 Uiso 1 1 calc R . . C33 C 0.2655(4) 0.1814(4) 0.46707(19) 0.0490(9) Uani 1 1 d . . . H33A H 0.1693 0.1902 0.4623 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02153(14) 0.02603(14) 0.02920(14) -0.00759(9) -0.00291(9) 0.00016(9) B1 0.0210(16) 0.0274(17) 0.0365(18) -0.0081(14) -0.0023(13) -0.0082(13) B2 0.0237(18) 0.045(2) 0.047(2) -0.0137(18) 0.0083(15) -0.0095(16) F1 0.0797(19) 0.113(3) 0.088(2) -0.0335(18) -0.0192(15) -0.0463(18) F2 0.101(2) 0.104(2) 0.0730(19) -0.0340(17) 0.0346(17) -0.0222(19) F3 0.0524(16) 0.0557(17) 0.164(3) 0.0176(19) -0.0199(18) -0.0036(13) F4 0.0796(18) 0.0626(16) 0.0756(17) 0.0048(13) 0.0006(14) -0.0377(14) F5 0.123(3) 0.131(3) 0.109(3) -0.046(2) -0.012(2) -0.028(3) F6 0.0842(19) 0.0526(15) 0.0863(19) -0.0097(14) 0.0302(15) -0.0127(14) F7 0.059(2) 0.254(6) 0.176(4) -0.004(4) 0.021(2) -0.043(3) F8 0.331(7) 0.066(2) 0.087(3) 0.020(2) 0.034(3) 0.052(3) O1 0.0334(13) 0.0530(16) 0.0387(14) -0.0046(11) -0.0016(10) -0.0208(11) O2 0.0419(14) 0.0365(14) 0.0414(14) -0.0077(11) 0.0037(11) -0.0151(11) O3 0.117(3) 0.0374(17) 0.086(2) -0.0142(16) 0.016(2) -0.0209(18) O4 0.079(2) 0.0548(18) 0.0401(14) -0.0067(13) 0.0099(14) -0.0072(15) O5 0.0643(18) 0.0653(19) 0.0428(15) -0.0103(14) 0.0050(13) -0.0198(15) N1 0.0250(13) 0.0243(13) 0.0365(14) -0.0028(10) -0.0070(10) -0.0015(10) N2 0.0357(15) 0.0370(15) 0.0322(14) 0.0009(11) -0.0026(11) -0.0054(12) N3 0.0257(13) 0.0293(14) 0.0321(13) -0.0055(11) -0.0037(10) 0.0007(10) N4 0.0277(13) 0.0272(13) 0.0294(13) -0.0069(10) 0.0002(10) -0.0004(10) N5 0.0318(14) 0.0438(17) 0.0402(15) -0.0145(13) -0.0026(11) -0.0101(12) N6 0.0252(13) 0.0281(13) 0.0337(13) -0.0103(11) -0.0022(10) -0.0019(10) N7 0.0248(13) 0.0245(13) 0.0352(13) -0.0026(10) -0.0049(10) 0.0013(10) N8 0.0380(16) 0.0437(17) 0.0317(14) -0.0012(12) -0.0015(12) 0.0038(13) N9 0.0266(13) 0.0307(14) 0.0314(13) -0.0053(11) -0.0018(10) 0.0027(10) N10 0.0375(15) 0.0227(13) 0.0311(13) -0.0038(10) 0.0056(11) 0.0003(11) N11 0.0403(16) 0.0419(17) 0.0405(15) -0.0141(13) -0.0021(12) -0.0090(13) N12 0.0262(13) 0.0241(13) 0.0327(13) -0.0079(10) -0.0008(10) -0.0003(10) N13 0.088(3) 0.0365(19) 0.054(2) -0.0040(15) 0.0054(18) -0.0115(18) N14 0.0528(19) 0.0462(18) 0.0419(16) -0.0064(14) 0.0107(14) -0.0155(15) N15 0.0429(17) 0.0479(18) 0.0406(16) -0.0028(13) 0.0048(13) -0.0149(14) C1 0.0209(14) 0.0302(17) 0.0449(18) 0.0005(14) -0.0053(12) -0.0014(12) C2 0.0352(17) 0.0302(17) 0.0454(19) -0.0106(14) -0.0124(14) -0.0002(14) C3 0.0353(17) 0.0336(18) 0.0311(16) -0.0054(13) -0.0094(13) 0.0005(13) C4 0.0279(15) 0.0303(16) 0.0296(15) -0.0070(12) 0.0051(12) -0.0006(12) C5 0.055(2) 0.0341(19) 0.0352(18) -0.0111(14) -0.0071(15) 0.0015(16) C6 0.050(2) 0.044(2) 0.0327(17) -0.0029(15) -0.0130(15) 0.0009(16) C7 0.0266(17) 0.0332(19) 0.067(2) 0.0059(16) -0.0162(15) -0.0070(14) C8 0.0408(18) 0.0281(17) 0.0315(16) -0.0057(13) 0.0061(13) 0.0010(13) C9 0.0273(16) 0.0381(18) 0.0340(16) -0.0059(14) 0.0014(12) -0.0025(13) C10 0.0267(15) 0.0255(15) 0.0343(16) 0.0002(12) -0.0039(12) -0.0009(12) C11 0.0233(15) 0.048(2) 0.0404(18) -0.0153(15) -0.0010(13) -0.0072(14) C12 0.0276(15) 0.0251(15) 0.0346(16) -0.0064(12) -0.0014(12) -0.0030(12) C13 0.0184(14) 0.0280(16) 0.0439(17) -0.0046(13) -0.0054(12) -0.0009(11) C14 0.047(2) 0.0306(18) 0.047(2) -0.0144(15) -0.0138(16) 0.0027(15) C15 0.052(2) 0.0354(19) 0.0348(17) -0.0053(14) -0.0097(15) 0.0049(16) C16 0.0340(17) 0.0279(17) 0.0367(17) -0.0059(13) 0.0107(13) 0.0027(13) C17 0.053(2) 0.0333(19) 0.0403(18) -0.0151(15) 0.0005(16) -0.0026(16) C18 0.045(2) 0.0380(19) 0.0353(17) -0.0055(14) -0.0071(14) -0.0014(15) C19 0.0260(16) 0.0293(17) 0.060(2) -0.0002(15) -0.0111(14) -0.0043(13) C20 0.058(2) 0.0291(18) 0.0428(19) -0.0036(15) 0.0224(17) 0.0047(16) C21 0.0322(17) 0.0408(19) 0.0308(16) -0.0026(14) 0.0029(13) 0.0042(14) C22 0.0280(16) 0.0309(17) 0.0324(16) -0.0016(13) -0.0020(12) 0.0003(12) C23 0.0257(15) 0.0369(18) 0.0383(17) -0.0130(14) -0.0010(13) -0.0048(13) C24 0.0277(15) 0.0244(15) 0.0375(16) -0.0053(13) 0.0010(12) -0.0021(12) C25 0.085(5) 0.082(5) 0.228(10) -0.052(5) 0.018(5) -0.005(4) C26 0.139(5) 0.059(3) 0.073(3) -0.007(3) -0.020(3) -0.033(3) C27 0.086(3) 0.043(2) 0.063(3) -0.006(2) 0.016(2) -0.012(2) C28 0.085(3) 0.065(3) 0.068(3) -0.023(2) 0.031(3) -0.021(3) C29 0.062(3) 0.083(3) 0.061(3) -0.013(2) -0.006(2) -0.022(2) C30 0.057(2) 0.044(2) 0.042(2) 0.0007(17) 0.0005(17) -0.0156(18) C31 0.072(3) 0.067(3) 0.052(2) -0.005(2) 0.011(2) 0.001(2) C32 0.053(3) 0.087(4) 0.064(3) -0.022(2) 0.000(2) -0.027(2) C33 0.042(2) 0.060(3) 0.046(2) 0.0019(19) -0.0006(17) -0.0185(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.309(2) . ? Cd1 N9 2.305(2) . ? Cd1 O2 2.318(2) . ? Cd1 N6 2.328(2) 1_465 ? Cd1 N12 2.346(2) 1_645 ? Cd1 O1 2.368(2) . ? B1 F2 1.342(4) . ? B1 F3 1.364(4) . ? B1 F1 1.409(4) . ? B1 F4 1.369(4) . ? B2 F7 1.320(5) . ? B2 F8 1.296(6) . ? B2 F6 1.398(5) . ? B2 F5 1.389(5) . ? O1 HW1 0.81(2) . ? O1 HW2 0.84(2) . ? O2 HW3 0.82(2) . ? O2 HW4 0.83(2) . ? O3 C27 1.222(6) . ? O4 C30 1.228(5) . ? O5 C33 1.227(5) . ? N1 C10 1.320(4) . ? N1 N2 1.364(4) . ? N1 C7 1.464(4) . ? N2 C9 1.309(4) . ? N3 C10 1.321(4) . ? N3 C9 1.361(4) . ? N4 C12 1.329(4) . ? N4 N5 1.366(4) . ? N4 C8 1.465(4) . ? N5 C11 1.307(4) . ? N6 C12 1.320(4) . ? N6 C11 1.354(4) . ? N6 Cd1 2.328(2) 1_645 ? N7 C22 1.321(4) . ? N7 N8 1.364(4) . ? N7 C19 1.469(4) . ? N8 C21 1.311(4) . ? N9 C22 1.314(4) . ? N9 C21 1.353(4) . ? N10 C24 1.325(4) . ? N10 N11 1.369(4) . ? N10 C20 1.470(4) . ? N11 C23 1.314(4) . ? N12 C24 1.316(4) . ? N12 C23 1.353(4) . ? N12 Cd1 2.346(2) 1_465 ? N13 C27 1.300(6) . ? N13 C25 1.400(8) . ? N13 C26 1.464(6) . ? N14 C30 1.323(5) . ? N14 C29 1.447(5) . ? N14 C28 1.450(5) . ? N15 C33 1.314(5) . ? N15 C31 1.445(5) . ? N15 C32 1.450(5) . ? C1 C2 1.378(5) . ? C1 C6 1.383(5) . ? C1 C7 1.507(5) . ? C2 C3 1.387(5) . ? C2 H2A 0.9500 . ? C3 C4 1.378(4) . ? C3 H3A 0.9500 . ? C4 C5 1.388(5) . ? C4 C8 1.516(4) . ? C5 C6 1.387(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.371(5) . ? C13 C18 1.392(5) . ? C13 C19 1.508(4) . ? C14 C15 1.390(5) . ? C14 H14A 0.9500 . ? C15 C16 1.372(5) . ? C15 H15A 0.9500 . ? C16 C17 1.390(5) . ? C16 C20 1.514(5) . ? C17 C18 1.373(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9500 . ? 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 N3 Cd1 N9 175.51(9) . . ? N3 Cd1 O2 90.32(9) . . ? N9 Cd1 O2 93.89(9) . . ? N3 Cd1 N6 87.20(9) . 1_465 ? N9 Cd1 N6 94.16(9) . 1_465 ? O2 Cd1 N6 92.35(9) . 1_465 ? N3 Cd1 N12 91.34(9) . 1_645 ? N9 Cd1 N12 87.28(9) . 1_645 ? O2 Cd1 N12 87.82(9) . 1_645 ? N6 Cd1 N12 178.53(8) 1_465 1_645 ? N3 Cd1 O1 88.99(9) . . ? N9 Cd1 O1 86.70(9) . . ? O2 Cd1 O1 176.14(9) . . ? N6 Cd1 O1 91.41(9) 1_465 . ? N12 Cd1 O1 88.40(9) 1_645 . ? F2 B1 F3 113.1(3) . . ? F2 B1 F1 107.4(3) . . ? F3 B1 F1 108.1(3) . . ? F2 B1 F4 112.1(3) . . ? F3 B1 F4 107.5(3) . . ? F1 B1 F4 108.5(3) . . ? F7 B2 F8 125.1(5) . . ? F7 B2 F6 108.5(4) . . ? F8 B2 F6 108.5(3) . . ? F7 B2 F5 101.4(4) . . ? F8 B2 F5 106.9(4) . . ? F6 B2 F5 104.5(3) . . ? Cd1 O1 HW1 120(3) . . ? Cd1 O1 HW2 120(3) . . ? HW1 O1 HW2 110(3) . . ? Cd1 O2 HW3 109(3) . . ? Cd1 O2 HW4 112(3) . . ? HW3 O2 HW4 108(3) . . ? C10 N1 N2 110.0(2) . . ? C10 N1 C7 128.3(3) . . ? N2 N1 C7 121.5(3) . . ? C9 N2 N1 102.7(3) . . ? C10 N3 C9 103.4(3) . . ? C10 N3 Cd1 128.0(2) . . ? C9 N3 Cd1 128.4(2) . . ? C12 N4 N5 109.5(2) . . ? C12 N4 C8 129.5(3) . . ? N5 N4 C8 120.9(3) . . ? C11 N5 N4 102.5(2) . . ? C12 N6 C11 103.0(2) . . ? C12 N6 Cd1 131.0(2) . 1_645 ? C11 N6 Cd1 125.9(2) . 1_645 ? C22 N7 N8 109.5(2) . . ? C22 N7 C19 128.9(3) . . ? N8 N7 C19 121.6(3) . . ? C21 N8 N7 102.8(3) . . ? C22 N9 C21 103.6(3) . . ? C22 N9 Cd1 128.4(2) . . ? C21 N9 Cd1 127.5(2) . . ? C24 N10 N11 110.2(2) . . ? C24 N10 C20 128.7(3) . . ? N11 N10 C20 121.1(3) . . ? C23 N11 N10 101.9(3) . . ? C24 N12 C23 103.5(3) . . ? C24 N12 Cd1 128.0(2) . 1_465 ? C23 N12 Cd1 128.5(2) . 1_465 ? C27 N13 C25 122.5(5) . . ? C27 N13 C26 121.4(5) . . ? C25 N13 C26 115.9(5) . . ? C30 N14 C29 120.5(3) . . ? C30 N14 C28 120.6(4) . . ? C29 N14 C28 118.7(4) . . ? C33 N15 C31 121.0(4) . . ? C33 N15 C32 119.9(3) . . ? C31 N15 C32 119.0(4) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 C7 120.2(3) . . ? C6 C1 C7 121.0(3) . . ? C1 C2 C3 120.9(3) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 C8 121.4(3) . . ? C3 C4 C8 119.6(3) . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C1 C6 C5 120.4(3) . . ? C1 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? N1 C7 C1 112.6(3) . . ? N1 C7 H7A 109.1 . . ? C1 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C1 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N4 C8 C4 112.0(3) . . ? N4 C8 H8A 109.2 . . ? C4 C8 H8A 109.2 . . ? N4 C8 H8B 109.2 . . ? C4 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N2 C9 N3 113.9(3) . . ? N2 C9 H9A 123.0 . . ? N3 C9 H9A 123.0 . . ? N1 C10 N3 110.0(3) . . ? N1 C10 H10A 125.0 . . ? N3 C10 H10A 125.0 . . ? N5 C11 N6 114.7(3) . . ? N5 C11 H11A 122.6 . . ? N6 C11 H11A 122.6 . . ? N4 C12 N6 110.2(3) . . ? N4 C12 H12A 124.9 . . ? N6 C12 H12A 124.9 . . ? C14 C13 C18 118.9(3) . . ? C14 C13 C19 120.8(3) . . ? C18 C13 C19 120.3(3) . . ? C13 C14 C15 120.8(3) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 119.1(3) . . ? C15 C16 C20 120.1(3) . . ? C17 C16 C20 120.7(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C13 120.3(3) . . ? C17 C18 H18A 119.8 . . ? C13 C18 H18A 119.8 . . ? N7 C19 C13 111.1(3) . . ? N7 C19 H19A 109.4 . . ? C13 C19 H19A 109.4 . . ? N7 C19 H19B 109.4 . . ? C13 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N10 C20 C16 112.2(3) . . ? N10 C20 H20A 109.2 . . ? C16 C20 H20A 109.2 . . ? N10 C20 H20B 109.2 . . ? C16 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? N8 C21 N9 113.9(3) . . ? N8 C21 H21A 123.1 . . ? N9 C21 H21A 123.1 . . ? N7 C22 N9 110.3(3) . . ? N7 C22 H22A 124.9 . . ? N9 C22 H22A 124.9 . . ? N11 C23 N12 114.6(3) . . ? N11 C23 H23A 122.7 . . ? N12 C23 H23A 122.7 . . ? N12 C24 N10 109.8(3) . . ? N12 C24 H24A 125.1 . . ? N10 C24 H24A 125.1 . . ? N13 C25 H25A 109.5 . . ? N13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N13 C26 H26A 109.5 . . ? N13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 N13 124.4(5) . . ? O3 C27 H27A 117.8 . . ? N13 C27 H27A 117.8 . . ? N14 C28 H28A 109.5 . . ? N14 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N14 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N14 C29 H29A 109.5 . . ? N14 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N14 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O4 C30 N14 124.7(4) . . ? O4 C30 H30A 117.6 . . ? N14 C30 H30A 117.6 . . ? N15 C31 H31A 109.5 . . ? N15 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N15 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N15 C32 H32A 109.5 . . ? N15 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N15 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 N15 125.8(4) . . ? O5 C33 H33A 117.1 . . ? N15 C33 H33A 117.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 N1 N2 C9 0.3(3) . . . . ? C7 N1 N2 C9 175.8(3) . . . . ? N9 Cd1 N3 C10 144.4(9) . . . . ? O2 Cd1 N3 C10 -15.5(3) . . . . ? N6 Cd1 N3 C10 -107.9(3) 1_465 . . . ? N12 Cd1 N3 C10 72.3(3) 1_645 . . . ? O1 Cd1 N3 C10 160.7(3) . . . . ? N9 Cd1 N3 C9 -42.3(11) . . . . ? O2 Cd1 N3 C9 157.8(3) . . . . ? N6 Cd1 N3 C9 65.4(3) 1_465 . . . ? N12 Cd1 N3 C9 -114.4(3) 1_645 . . . ? O1 Cd1 N3 C9 -26.0(3) . . . . ? C12 N4 N5 C11 -0.3(4) . . . . ? C8 N4 N5 C11 -178.7(3) . . . . ? C22 N7 N8 C21 0.3(4) . . . . ? C19 N7 N8 C21 -178.9(3) . . . . ? N3 Cd1 N9 C22 47.3(11) . . . . ? O2 Cd1 N9 C22 -152.8(3) . . . . ? N6 Cd1 N9 C22 -60.2(3) 1_465 . . . ? N12 Cd1 N9 C22 119.5(3) 1_645 . . . ? O1 Cd1 N9 C22 31.0(3) . . . . ? N3 Cd1 N9 C21 -122.8(10) . . . . ? O2 Cd1 N9 C21 37.0(3) . . . . ? N6 Cd1 N9 C21 129.7(3) 1_465 . . . ? N12 Cd1 N9 C21 -50.6(3) 1_645 . . . ? O1 Cd1 N9 C21 -139.1(3) . . . . ? C24 N10 N11 C23 1.3(3) . . . . ? C20 N10 N11 C23 179.4(3) . . . . ? C6 C1 C2 C3 -0.3(5) . . . . ? C7 C1 C2 C3 -179.0(3) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C2 C3 C4 C8 -177.7(3) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C8 C4 C5 C6 177.9(3) . . . . ? C2 C1 C6 C5 0.6(5) . . . . ? C7 C1 C6 C5 179.2(3) . . . . ? C4 C5 C6 C1 -0.6(6) . . . . ? C10 N1 C7 C1 -136.7(3) . . . . ? N2 N1 C7 C1 48.6(4) . . . . ? C2 C1 C7 N1 -117.5(3) . . . . ? C6 C1 C7 N1 63.9(4) . . . . ? C12 N4 C8 C4 -100.4(4) . . . . ? N5 N4 C8 C4 77.6(4) . . . . ? C5 C4 C8 N4 53.3(4) . . . . ? C3 C4 C8 N4 -129.4(3) . . . . ? N1 N2 C9 N3 0.0(4) . . . . ? C10 N3 C9 N2 -0.3(4) . . . . ? Cd1 N3 C9 N2 -174.9(2) . . . . ? N2 N1 C10 N3 -0.5(4) . . . . ? C7 N1 C10 N3 -175.7(3) . . . . ? C9 N3 C10 N1 0.5(3) . . . . ? Cd1 N3 C10 N1 175.07(19) . . . . ? N4 N5 C11 N6 0.1(4) . . . . ? C12 N6 C11 N5 0.1(4) . . . . ? Cd1 N6 C11 N5 178.1(2) 1_645 . . . ? N5 N4 C12 N6 0.4(4) . . . . ? C8 N4 C12 N6 178.6(3) . . . . ? C11 N6 C12 N4 -0.3(3) . . . . ? Cd1 N6 C12 N4 -178.15(19) 1_645 . . . ? C18 C13 C14 C15 -0.4(5) . . . . ? C19 C13 C14 C15 -178.8(3) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C14 C15 C16 C17 0.5(6) . . . . ? C14 C15 C16 C20 178.1(3) . . . . ? C15 C16 C17 C18 -0.9(5) . . . . ? C20 C16 C17 C18 -178.5(3) . . . . ? C16 C17 C18 C13 0.7(6) . . . . ? C14 C13 C18 C17 0.0(5) . . . . ? C19 C13 C18 C17 178.4(3) . . . . ? C22 N7 C19 C13 123.8(3) . . . . ? N8 N7 C19 C13 -57.1(4) . . . . ? C14 C13 C19 N7 107.6(4) . . . . ? C18 C13 C19 N7 -70.8(4) . . . . ? C24 N10 C20 C16 103.6(4) . . . . ? N11 N10 C20 C16 -74.0(4) . . . . ? C15 C16 C20 N10 123.5(4) . . . . ? C17 C16 C20 N10 -59.0(5) . . . . ? N7 N8 C21 N9 -0.2(4) . . . . ? C22 N9 C21 N8 0.1(4) . . . . ? Cd1 N9 C21 N8 172.2(2) . . . . ? N8 N7 C22 N9 -0.3(4) . . . . ? C19 N7 C22 N9 178.9(3) . . . . ? C21 N9 C22 N7 0.1(4) . . . . ? Cd1 N9 C22 N7 -171.9(2) . . . . ? N10 N11 C23 N12 -1.3(4) . . . . ? C24 N12 C23 N11 0.9(4) . . . . ? Cd1 N12 C23 N11 -176.9(2) 1_465 . . . ? C23 N12 C24 N10 0.1(3) . . . . ? Cd1 N12 C24 N10 177.80(19) 1_465 . . . ? N11 N10 C24 N12 -0.9(4) . . . . ? C20 N10 C24 N12 -178.7(3) . . . . ? C25 N13 C27 O3 -0.7(8) . . . . ? C26 N13 C27 O3 -175.3(4) . . . . ? C29 N14 C30 O4 1.6(6) . . . . ? C28 N14 C30 O4 177.1(4) . . . . ? C31 N15 C33 O5 -175.8(4) . . . . ? C32 N15 C33 O5 0.3(6) . . . . ? 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 O1 HW1 F1 0.81(2) 2.00(2) 2.796(3) 166(4) . O1 HW2 O5 0.84(2) 1.85(2) 2.673(4) 167(4) . O2 HW3 O3 0.82(2) 1.87(2) 2.680(4) 174(4) . O2 HW4 O4 0.83(2) 1.90(3) 2.723(4) 173(4) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.652 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.076 ###======================== data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 256593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 Cd Cl2 N12 O12' _chemical_formula_weight 863.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.744(3) _cell_length_b 16.954(3) _cell_length_c 14.824(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.91(3) _cell_angle_gamma 90.00 _cell_volume 3463.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 193.15 _cell_measurement_reflns_used 7614 _cell_measurement_theta_min 3.1005 _cell_measurement_theta_max 27.02 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6261 _exptl_absorpt_correction_T_max 0.8817 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 193.15 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18243 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.05 _reflns_number_total 3772 _reflns_number_gt 3555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+1.9820P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3772 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.359484(13) 0.7500 0.03125(12) Uani 1 2 d S . . Cl1 Cl 0.26903(6) 0.15070(4) 0.76057(7) 0.0495(2) Uani 1 1 d . . . O1 O 0.34370(19) 0.35642(15) 0.7213(2) 0.0548(6) Uani 1 1 d . . . O2 O 0.2995(2) 0.22706(16) 0.8043(2) 0.0818(8) Uani 1 1 d . . . O3 O 0.3502(3) 0.1018(2) 0.7850(3) 0.1096(12) Uani 1 1 d . . . O4 O 0.2159(4) 0.1565(3) 0.6554(3) 0.141(2) Uani 1 1 d . . . O5 O 0.2110(4) 0.1184(3) 0.7979(5) 0.1367(19) Uani 1 1 d . . . O6 O 0.2024(2) 0.45750(16) 0.6200(2) 0.0689(7) Uani 1 1 d . . . N1 N 0.55099(17) 0.21150(14) 1.01720(16) 0.0398(5) Uani 1 1 d . . . N2 N 0.5800(2) 0.15639(16) 0.9721(2) 0.0508(6) Uani 1 1 d . . . N3 N 0.53312(17) 0.26547(13) 0.87688(17) 0.0368(5) Uani 1 1 d . . . N4 N 0.14105(15) 0.02730(14) 1.01110(15) 0.0352(5) Uani 1 1 d . . . N5 N 0.06325(18) 0.07378(14) 0.95412(19) 0.0439(5) Uani 1 1 d . . . N6 N 0.04990(17) -0.04090(13) 0.87371(17) 0.0365(5) Uani 1 1 d . . . C1 C 0.4663(2) 0.15898(17) 1.1090(2) 0.0389(6) Uani 1 1 d . . . C2 C 0.3899(2) 0.20452(17) 1.0990(2) 0.0508(7) Uani 1 1 d . . . H2A H 0.3927 0.2602 1.0936 0.061 Uiso 1 1 calc R . . C3 C 0.3091(2) 0.17059(19) 1.0965(2) 0.0480(7) Uani 1 1 d . . . H3A H 0.2565 0.2029 1.0884 0.058 Uiso 1 1 calc R . . C4 C 0.30447(19) 0.08948(16) 1.10601(18) 0.0360(5) Uani 1 1 d . . . C5 C 0.3810(2) 0.04394(16) 1.1156(2) 0.0455(6) Uani 1 1 d . . . H5A H 0.3784 -0.0117 1.1213 0.055 Uiso 1 1 calc R . . C6 C 0.4611(2) 0.07777(18) 1.1171(2) 0.0458(6) Uani 1 1 d . . . H6A H 0.5131 0.0454 1.1236 0.055 Uiso 1 1 calc R . . C7 C 0.5560(2) 0.1979(2) 1.1177(2) 0.0484(7) Uani 1 1 d . . . H7A H 0.5658 0.2490 1.1536 0.058 Uiso 1 1 calc R . . H7B H 0.6130 0.1642 1.1602 0.058 Uiso 1 1 calc R . . C8 C 0.2195(2) 0.0534(2) 1.1114(2) 0.0456(7) Uani 1 1 d . . . H8A H 0.2427 0.0076 1.1587 0.055 Uiso 1 1 calc R . . H8B H 0.1932 0.0926 1.1409 0.055 Uiso 1 1 calc R . . C9 C 0.5684(2) 0.19179(17) 0.8886(2) 0.0469(7) Uani 1 1 d . . . H9A H 0.5836 0.1676 0.8404 0.056 Uiso 1 1 calc R . . C10 C 0.52199(19) 0.27540(16) 0.95920(19) 0.0386(6) Uani 1 1 d . . . H10A H 0.4969 0.3216 0.9742 0.046 Uiso 1 1 calc R . . C11 C 0.0107(2) 0.03061(16) 0.8723(2) 0.0411(6) Uani 1 1 d . . . H11A H -0.0494 0.0479 0.8171 0.049 Uiso 1 1 calc R . . C12 C 0.1317(2) -0.04009(16) 0.9625(2) 0.0393(6) Uani 1 1 d . . . H12A H 0.1772 -0.0821 0.9877 0.047 Uiso 1 1 calc R . . HW1 H 0.322(3) 0.317(3) 0.726(3) 0.065(13) Uiso 1 1 d . . . HW2 H 0.293(3) 0.389(3) 0.688(3) 0.077(13) Uiso 1 1 d . . . HW3 H 0.157(3) 0.442(3) 0.566(4) 0.079(14) Uiso 1 1 d . . . HW4 H 0.196(4) 0.516(4) 0.629(4) 0.105(17) Uiso 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 Cd1 0.03798(17) 0.02837(16) 0.02611(17) 0.000 0.01448(12) 0.000 Cl1 0.0467(4) 0.0405(4) 0.0523(4) 0.0003(3) 0.0168(3) -0.0001(3) O1 0.0453(13) 0.0504(14) 0.0764(18) 0.0148(11) 0.0355(13) 0.0067(10) O2 0.107(2) 0.0569(15) 0.101(2) -0.0225(15) 0.0661(19) -0.0285(15) O3 0.073(2) 0.086(2) 0.146(3) -0.003(2) 0.034(2) 0.0279(18) O4 0.173(5) 0.128(3) 0.058(2) -0.014(2) 0.006(2) 0.063(3) O5 0.149(4) 0.092(2) 0.226(6) -0.019(3) 0.136(4) -0.049(3) O6 0.0642(16) 0.0509(14) 0.0585(15) -0.0100(12) 0.0035(12) 0.0023(12) N1 0.0444(12) 0.0423(12) 0.0304(11) 0.0017(9) 0.0162(9) -0.0096(10) N2 0.0648(18) 0.0426(13) 0.0446(14) 0.0107(11) 0.0260(13) 0.0100(12) N3 0.0463(12) 0.0345(11) 0.0324(11) 0.0039(9) 0.0211(10) 0.0025(9) N4 0.0389(12) 0.0388(12) 0.0314(11) -0.0055(8) 0.0197(9) -0.0047(9) N5 0.0486(13) 0.0396(12) 0.0440(13) -0.0089(10) 0.0226(11) 0.0005(10) N6 0.0403(11) 0.0324(11) 0.0339(11) -0.0057(9) 0.0157(9) -0.0018(9) C1 0.0468(15) 0.0443(14) 0.0217(12) 0.0025(11) 0.0133(11) -0.0099(12) C2 0.064(2) 0.0325(14) 0.0530(17) 0.0024(13) 0.0259(15) -0.0061(13) C3 0.0550(17) 0.0421(15) 0.0475(16) -0.0004(13) 0.0252(14) 0.0041(13) C4 0.0436(14) 0.0403(13) 0.0219(11) -0.0060(10) 0.0141(10) -0.0083(11) C5 0.0569(17) 0.0326(13) 0.0476(16) 0.0018(12) 0.0257(14) -0.0021(12) C6 0.0471(16) 0.0450(15) 0.0473(15) 0.0042(13) 0.0245(13) 0.0040(12) C7 0.0490(16) 0.0648(19) 0.0262(12) 0.0007(12) 0.0140(11) -0.0169(14) C8 0.0502(16) 0.0597(17) 0.0288(13) -0.0106(12) 0.0206(12) -0.0134(14) C9 0.0639(19) 0.0394(14) 0.0420(14) 0.0087(12) 0.0292(14) 0.0128(13) C10 0.0430(14) 0.0377(13) 0.0346(13) 0.0012(11) 0.0184(11) -0.0004(11) C11 0.0419(14) 0.0388(14) 0.0403(14) -0.0039(11) 0.0182(12) 0.0037(11) C12 0.0439(14) 0.0390(14) 0.0333(13) -0.0024(11) 0.0173(11) 0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.286(3) 2_656 ? Cd1 O1 2.286(3) . ? Cd1 N3 2.324(2) 2_656 ? Cd1 N3 2.324(2) . ? Cd1 N6 2.332(2) 3 ? Cd1 N6 2.332(2) 4_556 ? Cl1 O4 1.371(4) . ? Cl1 O5 1.388(4) . ? Cl1 O3 1.415(3) . ? Cl1 O2 1.423(3) . ? O1 HW1 0.77(4) . ? O1 HW2 0.89(5) . ? O6 HW3 0.82(5) . ? O6 HW4 1.01(6) . ? N1 C10 1.320(3) . ? N1 N2 1.350(4) . ? N1 C7 1.471(3) . ? N2 C9 1.307(4) . ? N3 C10 1.325(3) . ? N3 C9 1.344(4) . ? N4 C12 1.320(3) . ? N4 N5 1.354(3) . ? N4 C8 1.469(3) . ? N5 C11 1.311(4) . ? N6 C12 1.324(4) . ? N6 C11 1.356(3) . ? N6 Cd1 2.332(2) 3_445 ? C1 C2 1.376(5) . ? C1 C6 1.388(4) . ? C1 C7 1.507(4) . ? C2 C3 1.380(5) . ? C2 H2A 0.9500 . ? C3 C4 1.388(4) . ? C3 H3A 0.9500 . ? C4 C5 1.380(4) . ? C4 C8 1.508(4) . ? C5 C6 1.376(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 177.40(13) 2_656 . ? O1 Cd1 N3 86.30(9) 2_656 2_656 ? O1 Cd1 N3 91.92(9) . 2_656 ? O1 Cd1 N3 91.92(9) 2_656 . ? O1 Cd1 N3 86.30(9) . . ? N3 Cd1 N3 93.40(11) 2_656 . ? O1 Cd1 N6 86.96(9) 2_656 3 ? O1 Cd1 N6 94.93(9) . 3 ? N3 Cd1 N6 172.49(8) 2_656 3 ? N3 Cd1 N6 90.10(9) . 3 ? O1 Cd1 N6 94.93(9) 2_656 4_556 ? O1 Cd1 N6 86.96(9) . 4_556 ? N3 Cd1 N6 90.10(9) 2_656 4_556 ? N3 Cd1 N6 172.49(8) . 4_556 ? N6 Cd1 N6 87.21(11) 3 4_556 ? O4 Cl1 O5 108.9(4) . . ? O4 Cl1 O3 108.2(3) . . ? O5 Cl1 O3 110.7(3) . . ? O4 Cl1 O2 109.8(2) . . ? O5 Cl1 O2 108.6(2) . . ? O3 Cl1 O2 110.6(2) . . ? Cd1 O1 HW1 119(3) . . ? Cd1 O1 HW2 132(3) . . ? HW1 O1 HW2 106(4) . . ? HW3 O6 HW4 111(4) . . ? C10 N1 N2 109.8(2) . . ? C10 N1 C7 128.4(3) . . ? N2 N1 C7 121.8(2) . . ? C9 N2 N1 103.0(2) . . ? C10 N3 C9 103.3(2) . . ? C10 N3 Cd1 125.48(18) . . ? C9 N3 Cd1 131.21(18) . . ? C12 N4 N5 109.5(2) . . ? C12 N4 C8 129.1(2) . . ? N5 N4 C8 121.4(2) . . ? C11 N5 N4 103.2(2) . . ? C12 N6 C11 102.8(2) . . ? C12 N6 Cd1 125.83(18) . 3_445 ? C11 N6 Cd1 131.14(19) . 3_445 ? C2 C1 C6 118.8(3) . . ? C2 C1 C7 119.9(3) . . ? C6 C1 C7 121.2(3) . . ? C1 C2 C3 121.0(3) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 118.6(3) . . ? C5 C4 C8 121.4(3) . . ? C3 C4 C8 119.9(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C1 120.3(3) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? N1 C7 C1 113.1(2) . . ? N1 C7 H7A 108.9 . . ? C1 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C1 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? N4 C8 C4 113.7(2) . . ? N4 C8 H8A 108.8 . . ? C4 C8 H8A 108.8 . . ? N4 C8 H8B 108.8 . . ? C4 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N2 C9 N3 114.1(3) . . ? N2 C9 H9A 122.9 . . ? N3 C9 H9A 122.9 . . ? N1 C10 N3 109.7(2) . . ? N1 C10 H10A 125.1 . . ? N3 C10 H10A 125.1 . . ? N5 C11 N6 114.0(3) . . ? N5 C11 H11A 123.0 . . ? N6 C11 H11A 123.0 . . ? N4 C12 N6 110.5(2) . . ? N4 C12 H12A 124.8 . . ? N6 C12 H12A 124.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 N1 N2 C9 1.3(3) . . . . ? C7 N1 N2 C9 -177.2(3) . . . . ? O1 Cd1 N3 C10 121.2(2) 2_656 . . . ? O1 Cd1 N3 C10 -60.7(2) . . . . ? N3 Cd1 N3 C10 -152.4(3) 2_656 . . . ? N6 Cd1 N3 C10 34.2(2) 3 . . . ? N6 Cd1 N3 C10 -34.7(7) 4_556 . . . ? O1 Cd1 N3 C9 -57.1(3) 2_656 . . . ? O1 Cd1 N3 C9 121.0(3) . . . . ? N3 Cd1 N3 C9 29.3(2) 2_656 . . . ? N6 Cd1 N3 C9 -144.1(3) 3 . . . ? N6 Cd1 N3 C9 147.0(5) 4_556 . . . ? C12 N4 N5 C11 -0.4(3) . . . . ? C8 N4 N5 C11 -179.8(2) . . . . ? C6 C1 C2 C3 -0.2(5) . . . . ? C7 C1 C2 C3 -176.4(3) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C2 C3 C4 C8 175.3(3) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C8 C4 C5 C6 -175.9(3) . . . . ? C4 C5 C6 C1 0.1(5) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? C7 C1 C6 C5 175.8(3) . . . . ? C10 N1 C7 C1 93.6(4) . . . . ? N2 N1 C7 C1 -88.2(4) . . . . ? C2 C1 C7 N1 -89.3(4) . . . . ? C6 C1 C7 N1 94.6(3) . . . . ? C12 N4 C8 C4 84.9(4) . . . . ? N5 N4 C8 C4 -95.8(3) . . . . ? C5 C4 C8 N4 -89.4(3) . . . . ? C3 C4 C8 N4 94.0(3) . . . . ? N1 N2 C9 N3 -0.6(4) . . . . ? C10 N3 C9 N2 -0.3(4) . . . . ? Cd1 N3 C9 N2 178.3(2) . . . . ? N2 N1 C10 N3 -1.6(3) . . . . ? C7 N1 C10 N3 176.8(2) . . . . ? C9 N3 C10 N1 1.2(3) . . . . ? Cd1 N3 C10 N1 -177.57(17) . . . . ? N4 N5 C11 N6 0.3(3) . . . . ? C12 N6 C11 N5 -0.2(3) . . . . ? Cd1 N6 C11 N5 -175.33(19) 3_445 . . . ? N5 N4 C12 N6 0.3(3) . . . . ? C8 N4 C12 N6 179.6(2) . . . . ? C11 N6 C12 N4 -0.1(3) . . . . ? Cd1 N6 C12 N4 175.43(16) 3_445 . . . ? 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 O1 HW1 O2 0.77(4) 2.04(4) 2.763(4) 155(4) . O1 HW2 O6 0.89(5) 1.74(5) 2.629(4) 175(4) . O6 HW3 N2 0.82(5) 2.13(5) 2.857(4) 148(4) 8_455 O6 HW4 O5 1.01(6) 2.20(6) 3.030(6) 139(4) 4_556 O6 HW4 O3 1.01(6) 2.27(6) 3.127(5) 142(4) 4_556 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.831 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.071 ###=================== data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 256594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 Cd Cl2 N15 O13' _chemical_formula_weight 1047.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6707(7) _cell_length_b 14.1256(11) _cell_length_c 14.9212(9) _cell_angle_alpha 89.544(5) _cell_angle_beta 71.742(4) _cell_angle_gamma 82.640(4) _cell_volume 2315.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193.15 _cell_measurement_reflns_used 8159 _cell_measurement_theta_min 3.1680 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7777 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 193.15 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23008 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8403 _reflns_number_gt 7408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+1.8801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8403 _refine_ls_number_parameters 618 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.262198(19) 0.257539(14) 0.233941(15) 0.02851(9) Uani 1 1 d . . . Cl1 Cl -0.12337(7) 0.55819(6) 0.38549(5) 0.03574(18) Uani 1 1 d . . . Cl2 Cl 0.65726(8) -0.07525(6) 0.14264(6) 0.0421(2) Uani 1 1 d . . . O1 O 0.0682(2) 0.27778(19) 0.35292(17) 0.0409(6) Uani 1 1 d D . . O2 O 0.4454(2) 0.23646(17) 0.11302(18) 0.0379(5) Uani 1 1 d D . . O3 O 0.6121(3) 0.2672(3) 0.1929(2) 0.0727(9) Uani 1 1 d . . . O4 O 0.0579(3) 0.14144(19) 0.47941(18) 0.0584(7) Uani 1 1 d . . . O5 O 0.4457(2) 0.3654(2) -0.02140(18) 0.0555(7) Uani 1 1 d . . . O6 O -0.2519(3) 0.5724(3) 0.4181(3) 0.0858(11) Uani 1 1 d . . . O7 O -0.0751(5) 0.5849(3) 0.2916(2) 0.1128(15) Uani 1 1 d . . . O8 O -0.0850(3) 0.4595(2) 0.3909(3) 0.0814(10) Uani 1 1 d . . . O9 O -0.0814(2) 0.6111(2) 0.4474(2) 0.0639(8) Uani 1 1 d . . . O10 O 0.7609(3) -0.0591(2) 0.0656(2) 0.0692(8) Uani 1 1 d . . . O11 O 0.6586(4) -0.0322(3) 0.2264(2) 0.1008(13) Uani 1 1 d . . . N1 N 0.2487(2) 0.55668(17) 0.32400(18) 0.0294(5) Uani 1 1 d . . . N2 N 0.3265(2) 0.56145(19) 0.23459(19) 0.0381(6) Uani 1 1 d . . . N3 N 0.2791(2) 0.41285(17) 0.26455(17) 0.0309(6) Uani 1 1 d . . . N4 N 0.6039(2) 0.83087(18) 0.52576(17) 0.0325(6) Uani 1 1 d . . . N5 N 0.5300(3) 0.89729(19) 0.5912(2) 0.0405(7) Uani 1 1 d . . . N6 N 0.6506(2) 0.80103(17) 0.65420(17) 0.0305(6) Uani 1 1 d . . . N7 N 0.2782(2) -0.04111(17) 0.14423(18) 0.0288(5) Uani 1 1 d . . . N8 N 0.2069(3) -0.04896(19) 0.23460(19) 0.0391(6) Uani 1 1 d . . . N9 N 0.2437(2) 0.10202(17) 0.20649(18) 0.0316(6) Uani 1 1 d . . . N10 N -0.0933(2) -0.34172(17) -0.01011(16) 0.0267(5) Uani 1 1 d . . . N11 N -0.0216(2) -0.40625(19) -0.07854(19) 0.0376(6) Uani 1 1 d . . . N12 N -0.1602(2) -0.31649(17) -0.12969(17) 0.0283(5) Uani 1 1 d . . . N13 N 0.7867(3) 0.2226(3) 0.2259(2) 0.0586(9) Uani 1 1 d . . . N14 N 0.1082(3) 0.0880(2) 0.6070(2) 0.0451(7) Uani 1 1 d . . . N15 N 0.3728(2) 0.4330(2) -0.13331(19) 0.0406(7) Uani 1 1 d . . . C1 C 0.3012(3) 0.6913(2) 0.4000(2) 0.0325(7) Uani 1 1 d . . . C2 C 0.3720(3) 0.6495(2) 0.4524(2) 0.0402(8) Uani 1 1 d . . . H2A H 0.3559 0.5901 0.4808 0.048 Uiso 1 1 calc R . . C3 C 0.4657(3) 0.6934(2) 0.4638(2) 0.0398(8) Uani 1 1 d . . . H3A H 0.5141 0.6638 0.4995 0.048 Uiso 1 1 calc R . . C4 C 0.4902(3) 0.7809(2) 0.4233(2) 0.0326(7) Uani 1 1 d . . . C5 C 0.4181(3) 0.8233(2) 0.3727(2) 0.0385(8) Uani 1 1 d . . . H5A H 0.4326 0.8835 0.3458 0.046 Uiso 1 1 calc R . . C6 C 0.3245(3) 0.7784(2) 0.3609(2) 0.0388(8) Uani 1 1 d . . . H6A H 0.2758 0.8080 0.3254 0.047 Uiso 1 1 calc R . . C7 C 0.2010(3) 0.6427(2) 0.3850(3) 0.0415(8) Uani 1 1 d . . . H7A H 0.1472 0.6253 0.4469 0.050 Uiso 1 1 calc R . . H7B H 0.1515 0.6877 0.3562 0.050 Uiso 1 1 calc R . . C8 C 0.5967(3) 0.8268(3) 0.4298(2) 0.0426(8) Uani 1 1 d . . . H8A H 0.6727 0.7906 0.3881 0.051 Uiso 1 1 calc R . . H8B H 0.5905 0.8926 0.4066 0.051 Uiso 1 1 calc R . . C9 C 0.3416(3) 0.4733(2) 0.2026(2) 0.0350(7) Uani 1 1 d . . . H9A H 0.3925 0.4532 0.1407 0.042 Uiso 1 1 calc R . . C10 C 0.2218(3) 0.4687(2) 0.3396(2) 0.0323(7) Uani 1 1 d . . . H10A H 0.1687 0.4487 0.3968 0.039 Uiso 1 1 calc R . . C11 C 0.5619(3) 0.8765(2) 0.6663(2) 0.0362(7) Uani 1 1 d . . . H11A H 0.5258 0.9113 0.7247 0.043 Uiso 1 1 calc R . . C12 C 0.6734(3) 0.7743(2) 0.5647(2) 0.0328(7) Uani 1 1 d . . . H12A H 0.7312 0.7220 0.5330 0.039 Uiso 1 1 calc R . . C13 C 0.2210(3) -0.1796(2) 0.0783(2) 0.0287(6) Uani 1 1 d . . . C14 C 0.1230(3) -0.1365(2) 0.0523(2) 0.0392(8) Uani 1 1 d . . . H14A H 0.1205 -0.0719 0.0342 0.047 Uiso 1 1 calc R . . C15 C 0.0285(3) -0.1872(2) 0.0528(2) 0.0371(7) Uani 1 1 d . . . H15A H -0.0384 -0.1569 0.0351 0.044 Uiso 1 1 calc R . . C16 C 0.0309(3) -0.2816(2) 0.0787(2) 0.0283(6) Uani 1 1 d . . . C17 C 0.1278(3) -0.3238(2) 0.1049(2) 0.0347(7) Uani 1 1 d . . . H17A H 0.1302 -0.3884 0.1232 0.042 Uiso 1 1 calc R . . C18 C 0.2222(3) -0.2734(2) 0.1050(2) 0.0360(7) Uani 1 1 d . . . H18A H 0.2882 -0.3036 0.1237 0.043 Uiso 1 1 calc R . . C19 C 0.3236(3) -0.1250(2) 0.0793(2) 0.0366(7) Uani 1 1 d . . . H19A H 0.3851 -0.1673 0.0991 0.044 Uiso 1 1 calc R . . H19B H 0.3635 -0.1041 0.0148 0.044 Uiso 1 1 calc R . . C20 C -0.0734(3) -0.3360(2) 0.0820(2) 0.0334(7) Uani 1 1 d . . . H20A H -0.0564 -0.4014 0.1031 0.040 Uiso 1 1 calc R . . H20B H -0.1486 -0.3042 0.1289 0.040 Uiso 1 1 calc R . . C21 C 0.1888(3) 0.0389(2) 0.2689(2) 0.0378(7) Uani 1 1 d . . . H21A H 0.1411 0.0567 0.3322 0.045 Uiso 1 1 calc R . . C22 C 0.2997(3) 0.0483(2) 0.1288(2) 0.0303(7) Uani 1 1 d . . . H22A H 0.3479 0.0707 0.0707 0.036 Uiso 1 1 calc R . . C23 C -0.0667(3) -0.3881(2) -0.1480(2) 0.0360(7) Uani 1 1 d . . . H23A H -0.0359 -0.4228 -0.2068 0.043 Uiso 1 1 calc R . . C24 C -0.1742(3) -0.2896(2) -0.0421(2) 0.0288(6) Uani 1 1 d . . . H24A H -0.2338 -0.2400 -0.0069 0.035 Uiso 1 1 calc R . . C25 C 0.7689(6) 0.3038(5) 0.2890(5) 0.120(3) Uani 1 1 d . . . H25A H 0.8202 0.3514 0.2566 0.180 Uiso 1 1 calc R . . H25B H 0.7913 0.2832 0.3449 0.180 Uiso 1 1 calc R . . H25C H 0.6833 0.3320 0.3084 0.180 Uiso 1 1 calc R . . C26 C 0.8992(5) 0.1577(4) 0.2061(4) 0.0866(16) Uani 1 1 d . . . H26A H 0.8930 0.1003 0.1723 0.130 Uiso 1 1 calc R . . H26B H 0.9137 0.1396 0.2656 0.130 Uiso 1 1 calc R . . H26C H 0.9670 0.1892 0.1671 0.130 Uiso 1 1 calc R . . C27 C 0.7053(4) 0.2116(4) 0.1837(3) 0.0623(11) Uani 1 1 d . . . H27A H 0.7198 0.1568 0.1433 0.075 Uiso 1 1 calc R . . C28 C 0.0931(4) 0.1041(4) 0.7065(3) 0.0673(12) Uani 1 1 d . . . H28A H 0.0564 0.1701 0.7256 0.101 Uiso 1 1 calc R . . H28B H 0.1728 0.0929 0.7165 0.101 Uiso 1 1 calc R . . H28C H 0.0401 0.0602 0.7443 0.101 Uiso 1 1 calc R . . C29 C 0.1760(4) -0.0010(3) 0.5605(3) 0.0709(13) Uani 1 1 d . . . H29A H 0.1224 -0.0510 0.5735 0.106 Uiso 1 1 calc R . . H29B H 0.2445 -0.0197 0.5844 0.106 Uiso 1 1 calc R . . H29C H 0.2067 0.0074 0.4923 0.106 Uiso 1 1 calc R . . C30 C 0.0572(3) 0.1506(3) 0.5616(3) 0.0497(9) Uani 1 1 d . . . H30A H 0.0158 0.2084 0.5949 0.060 Uiso 1 1 calc R . . C31 C 0.3730(4) 0.4296(4) -0.2305(3) 0.0657(12) Uani 1 1 d . . . H31A H 0.4187 0.4790 -0.2656 0.099 Uiso 1 1 calc R . . H31B H 0.2891 0.4408 -0.2321 0.099 Uiso 1 1 calc R . . H31C H 0.4115 0.3667 -0.2594 0.099 Uiso 1 1 calc R . . C32 C 0.3096(4) 0.5168(3) -0.0748(3) 0.0627(11) Uani 1 1 d . . . H32A H 0.3119 0.5074 -0.0102 0.094 Uiso 1 1 calc R . . H32B H 0.2247 0.5271 -0.0743 0.094 Uiso 1 1 calc R . . H32C H 0.3493 0.5727 -0.1002 0.094 Uiso 1 1 calc R . . C33 C 0.4359(3) 0.3652(3) -0.1006(3) 0.0420(8) Uani 1 1 d . . . H33A H 0.4770 0.3121 -0.1418 0.050 Uiso 1 1 calc R . . HW1 H 0.060(3) 0.241(2) 0.394(2) 0.048(12) Uiso 1 1 d D . . HW3 H 0.451(4) 0.272(2) 0.070(2) 0.054(13) Uiso 1 1 d D . . HW2 H 0.033(3) 0.3274(18) 0.366(3) 0.055(13) Uiso 1 1 d D . . HW4 H 0.499(4) 0.246(3) 0.137(3) 0.082(17) Uiso 1 1 d D . . O12 O 0.6326(11) -0.1673(9) 0.1365(12) 0.182(9) Uani 0.50 1 d P . . O13 O 0.5543(10) -0.0135(9) 0.1210(7) 0.090(4) Uani 0.50 1 d P . . O14 O 0.6851(8) -0.1727(6) 0.1680(8) 0.072(3) Uani 0.50 1 d P . . O15 O 0.5522(11) -0.0586(9) 0.1324(11) 0.106(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03371(14) 0.02405(13) 0.03148(14) -0.00236(9) -0.01581(10) -0.00298(9) Cl1 0.0373(4) 0.0378(4) 0.0290(4) -0.0056(3) -0.0092(3) 0.0036(3) Cl2 0.0400(4) 0.0400(5) 0.0416(5) -0.0103(4) -0.0075(4) -0.0006(4) O1 0.0434(14) 0.0367(14) 0.0359(13) 0.0038(12) -0.0061(11) 0.0032(12) O2 0.0351(13) 0.0388(14) 0.0371(13) 0.0004(11) -0.0094(11) -0.0002(10) O3 0.0460(17) 0.104(3) 0.074(2) 0.0126(18) -0.0245(15) -0.0198(17) O4 0.0764(19) 0.0536(16) 0.0438(15) 0.0089(13) -0.0184(14) -0.0054(14) O5 0.0583(17) 0.0653(18) 0.0463(15) 0.0184(13) -0.0203(13) -0.0118(14) O6 0.0388(15) 0.109(3) 0.109(3) -0.043(2) -0.0300(17) 0.0118(16) O7 0.175(4) 0.109(3) 0.0361(17) 0.0139(18) -0.009(2) -0.014(3) O8 0.094(2) 0.0449(17) 0.096(2) -0.0043(16) -0.026(2) 0.0156(16) O9 0.0540(16) 0.079(2) 0.0593(17) -0.0202(15) -0.0127(14) -0.0236(15) O10 0.0473(16) 0.076(2) 0.0696(19) 0.0196(16) -0.0005(14) -0.0018(14) O11 0.103(3) 0.124(3) 0.072(2) -0.043(2) -0.042(2) 0.037(2) N1 0.0286(13) 0.0255(13) 0.0359(14) -0.0031(11) -0.0118(11) -0.0052(10) N2 0.0411(15) 0.0343(15) 0.0371(15) 0.0021(12) -0.0076(13) -0.0105(12) N3 0.0363(14) 0.0300(13) 0.0306(13) 0.0016(11) -0.0150(12) -0.0091(11) N4 0.0339(14) 0.0370(15) 0.0301(13) -0.0018(12) -0.0143(12) -0.0071(12) N5 0.0445(16) 0.0357(15) 0.0414(16) -0.0032(13) -0.0172(13) 0.0040(13) N6 0.0326(13) 0.0286(13) 0.0330(14) -0.0051(11) -0.0149(11) -0.0017(11) N7 0.0292(13) 0.0248(13) 0.0357(14) -0.0027(11) -0.0143(11) -0.0050(10) N8 0.0488(17) 0.0330(15) 0.0368(15) 0.0025(12) -0.0129(13) -0.0111(13) N9 0.0383(14) 0.0267(13) 0.0350(14) -0.0028(11) -0.0185(12) -0.0052(11) N10 0.0288(13) 0.0272(13) 0.0252(12) -0.0037(10) -0.0098(10) -0.0048(10) N11 0.0421(15) 0.0354(15) 0.0348(14) -0.0084(12) -0.0163(13) 0.0083(12) N12 0.0309(13) 0.0262(13) 0.0305(13) -0.0039(10) -0.0141(11) -0.0017(10) N13 0.0490(19) 0.085(2) 0.0513(19) 0.0169(18) -0.0228(16) -0.0257(18) N14 0.0436(16) 0.0486(18) 0.0400(16) 0.0087(14) -0.0095(14) -0.0042(14) N15 0.0371(15) 0.0497(17) 0.0333(14) 0.0028(13) -0.0085(12) -0.0053(13) C1 0.0295(15) 0.0265(16) 0.0390(17) -0.0115(13) -0.0084(14) -0.0003(12) C2 0.0449(19) 0.0320(17) 0.0457(19) 0.0040(15) -0.0147(16) -0.0117(15) C3 0.0432(19) 0.0443(19) 0.0389(18) 0.0058(15) -0.0217(16) -0.0086(15) C4 0.0343(16) 0.0369(17) 0.0280(15) -0.0051(13) -0.0102(13) -0.0092(14) C5 0.0449(19) 0.0313(17) 0.0432(19) 0.0031(15) -0.0172(16) -0.0107(14) C6 0.0420(18) 0.0345(18) 0.0454(19) -0.0012(15) -0.0226(16) -0.0017(14) C7 0.0277(16) 0.0375(18) 0.057(2) -0.0157(16) -0.0110(16) -0.0022(14) C8 0.0439(19) 0.058(2) 0.0323(17) 0.0032(16) -0.0164(15) -0.0189(17) C9 0.0378(17) 0.0355(18) 0.0311(16) -0.0009(14) -0.0091(14) -0.0071(14) C10 0.0360(17) 0.0355(17) 0.0281(16) -0.0024(14) -0.0111(14) -0.0119(14) C11 0.0423(18) 0.0317(17) 0.0333(17) -0.0057(14) -0.0133(15) 0.0041(14) C12 0.0311(16) 0.0317(16) 0.0362(17) -0.0091(14) -0.0114(14) -0.0029(13) C13 0.0289(15) 0.0253(15) 0.0321(16) -0.0070(13) -0.0100(13) -0.0022(12) C14 0.0452(19) 0.0260(16) 0.054(2) 0.0076(15) -0.0253(17) -0.0067(14) C15 0.0382(18) 0.0319(17) 0.049(2) 0.0044(15) -0.0253(16) -0.0024(14) C16 0.0312(15) 0.0295(16) 0.0260(15) -0.0043(12) -0.0111(13) -0.0054(13) C17 0.0411(18) 0.0232(15) 0.0440(18) -0.0012(14) -0.0199(15) -0.0029(13) C18 0.0339(17) 0.0283(16) 0.051(2) -0.0019(15) -0.0232(15) 0.0018(13) C19 0.0302(16) 0.0273(16) 0.050(2) -0.0096(15) -0.0101(15) -0.0022(13) C20 0.0391(17) 0.0386(18) 0.0266(15) 0.0013(13) -0.0137(14) -0.0113(14) C21 0.0467(19) 0.0361(18) 0.0323(17) -0.0016(14) -0.0129(15) -0.0105(15) C22 0.0328(16) 0.0295(16) 0.0324(16) 0.0021(13) -0.0148(14) -0.0069(13) C23 0.0422(18) 0.0328(17) 0.0309(16) -0.0075(14) -0.0121(14) 0.0048(14) C24 0.0268(15) 0.0285(15) 0.0310(16) -0.0075(13) -0.0091(13) -0.0024(12) C25 0.087(4) 0.178(7) 0.104(5) -0.051(5) -0.041(4) -0.016(4) C26 0.070(3) 0.099(4) 0.099(4) 0.033(3) -0.038(3) -0.011(3) C27 0.056(3) 0.084(3) 0.054(2) 0.012(2) -0.020(2) -0.028(2) C28 0.062(3) 0.098(4) 0.045(2) 0.007(2) -0.019(2) -0.019(2) C29 0.082(3) 0.047(2) 0.074(3) 0.007(2) -0.017(3) 0.008(2) C30 0.046(2) 0.044(2) 0.050(2) -0.0045(18) -0.0051(18) 0.0025(17) C31 0.065(3) 0.094(3) 0.041(2) 0.003(2) -0.022(2) -0.009(2) C32 0.061(3) 0.056(2) 0.067(3) -0.007(2) -0.021(2) 0.011(2) C33 0.0326(17) 0.045(2) 0.045(2) 0.0038(16) -0.0064(16) -0.0079(15) O12 0.123(11) 0.084(8) 0.242(17) -0.108(10) 0.107(10) -0.072(8) O13 0.046(5) 0.149(11) 0.058(5) -0.003(6) -0.016(4) 0.050(7) O14 0.070(6) 0.031(4) 0.096(5) 0.017(4) 0.001(4) -0.005(3) O15 0.061(6) 0.128(11) 0.162(10) 0.046(8) -0.074(6) -0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N9 2.287(2) . ? Cd1 N3 2.290(2) . ? Cd1 N6 2.309(2) 2_666 ? Cd1 O2 2.312(2) . ? Cd1 N12 2.327(2) 2 ? Cd1 O1 2.384(2) . ? Cl1 O7 1.405(3) . ? Cl1 O6 1.412(3) . ? Cl1 O8 1.418(3) . ? Cl1 O9 1.428(3) . ? Cl2 O15 1.275(12) . ? Cl2 O12 1.376(10) . ? Cl2 O11 1.399(3) . ? Cl2 O10 1.425(3) . ? Cl2 O14 1.449(8) . ? Cl2 O13 1.510(10) . ? O1 HW1 0.79(2) . ? O1 HW2 0.76(2) . ? O2 HW3 0.80(2) . ? O2 HW4 0.83(2) . ? O3 C27 1.227(5) . ? O4 C30 1.231(5) . ? O5 C33 1.223(4) . ? N1 C10 1.321(4) . ? N1 N2 1.365(4) . ? N1 C7 1.464(4) . ? N2 C9 1.307(4) . ? N3 C10 1.317(4) . ? N3 C9 1.358(4) . ? N4 C12 1.325(4) . ? N4 N5 1.363(4) . ? N4 C8 1.462(4) . ? N5 C11 1.307(4) . ? N6 C12 1.325(4) . ? N6 C11 1.358(4) . ? N6 Cd1 2.309(2) 2_666 ? N7 C22 1.324(4) . ? N7 N8 1.357(4) . ? N7 C19 1.469(4) . ? N8 C21 1.312(4) . ? N9 C22 1.326(4) . ? N9 C21 1.354(4) . ? N10 C24 1.327(4) . ? N10 N11 1.363(3) . ? N10 C20 1.469(4) . ? N11 C23 1.311(4) . ? N12 C24 1.317(4) . ? N12 C23 1.350(4) . ? N12 Cd1 2.327(2) 2 ? N13 C27 1.318(5) . ? N13 C26 1.451(6) . ? N13 C25 1.441(7) . ? N14 C30 1.305(5) . ? N14 C28 1.455(5) . ? N14 C29 1.450(5) . ? N15 C33 1.317(4) . ? N15 C31 1.450(5) . ? N15 C32 1.448(5) . ? C1 C2 1.385(5) . ? C1 C6 1.379(5) . ? C1 C7 1.503(4) . ? C2 C3 1.379(5) . ? C2 H2A 0.9500 . ? C3 C4 1.394(5) . ? C3 H3A 0.9500 . ? C4 C5 1.377(5) . ? C4 C8 1.503(4) . ? C5 C6 1.389(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.380(4) . ? C13 C14 1.388(4) . ? C13 C19 1.509(4) . ? C14 C15 1.388(4) . ? C14 H14A 0.9500 . ? C15 C16 1.385(4) . ? C15 H15A 0.9500 . ? C16 C17 1.374(4) . ? C16 C20 1.509(4) . ? C17 C18 1.386(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9500 . ? O12 O14 0.88(2) . ? O12 O15 1.705(19) . ? O13 O15 0.660(18) . ? 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 N9 Cd1 N3 178.87(9) . . ? N9 Cd1 N6 85.87(9) . 2_666 ? N3 Cd1 N6 93.39(9) . 2_666 ? N9 Cd1 O2 87.64(9) . . ? N3 Cd1 O2 93.26(9) . . ? N6 Cd1 O2 93.26(9) 2_666 . ? N9 Cd1 N12 93.66(8) . 2 ? N3 Cd1 N12 87.01(8) . 2 ? N6 Cd1 N12 175.71(8) 2_666 2 ? O2 Cd1 N12 90.98(9) . 2 ? N9 Cd1 O1 91.03(9) . . ? N3 Cd1 O1 88.10(9) . . ? N6 Cd1 O1 89.23(9) 2_666 . ? O2 Cd1 O1 177.09(9) . . ? N12 Cd1 O1 86.52(9) 2 . ? O7 Cl1 O6 112.7(3) . . ? O7 Cl1 O8 108.5(2) . . ? O6 Cl1 O8 107.7(2) . . ? O7 Cl1 O9 110.9(2) . . ? O6 Cl1 O9 107.94(18) . . ? O8 Cl1 O9 109.0(2) . . ? O15 Cl2 O12 80.0(9) . . ? O15 Cl2 O11 111.1(8) . . ? O12 Cl2 O11 123.4(8) . . ? O15 Cl2 O10 118.7(7) . . ? O12 Cl2 O10 109.9(5) . . ? O11 Cl2 O10 111.1(2) . . ? O15 Cl2 O14 112.7(6) . . ? O12 Cl2 O14 36.0(8) . . ? O11 Cl2 O14 96.2(5) . . ? O10 Cl2 O14 104.6(4) . . ? O15 Cl2 O13 25.7(8) . . ? O12 Cl2 O13 104.6(9) . . ? O11 Cl2 O13 102.3(5) . . ? O10 Cl2 O13 102.9(4) . . ? O14 Cl2 O13 138.4(6) . . ? Cd1 O1 HW1 115(3) . . ? Cd1 O1 HW2 120(3) . . ? HW1 O1 HW2 117(3) . . ? Cd1 O2 HW3 116(3) . . ? Cd1 O2 HW4 106(3) . . ? HW3 O2 HW4 107(3) . . ? C10 N1 N2 110.0(2) . . ? C10 N1 C7 129.1(3) . . ? N2 N1 C7 120.8(3) . . ? C9 N2 N1 102.1(2) . . ? C10 N3 C9 102.8(3) . . ? C10 N3 Cd1 130.0(2) . . ? C9 N3 Cd1 126.7(2) . . ? C12 N4 N5 109.6(2) . . ? C12 N4 C8 129.1(3) . . ? N5 N4 C8 121.3(3) . . ? C11 N5 N4 102.7(3) . . ? C12 N6 C11 102.7(3) . . ? C12 N6 Cd1 131.0(2) . 2_666 ? C11 N6 Cd1 126.3(2) . 2_666 ? C22 N7 N8 110.1(2) . . ? C22 N7 C19 128.7(3) . . ? N8 N7 C19 121.2(2) . . ? C21 N8 N7 102.6(2) . . ? C22 N9 C21 103.2(2) . . ? C22 N9 Cd1 127.7(2) . . ? C21 N9 Cd1 128.5(2) . . ? C24 N10 N11 109.7(2) . . ? C24 N10 C20 129.5(3) . . ? N11 N10 C20 120.9(2) . . ? C23 N11 N10 102.1(2) . . ? C24 N12 C23 102.9(2) . . ? C24 N12 Cd1 130.7(2) . 2 ? C23 N12 Cd1 126.41(19) . 2 ? C27 N13 C26 121.5(4) . . ? C27 N13 C25 120.2(4) . . ? C26 N13 C25 118.2(4) . . ? C30 N14 C28 120.6(3) . . ? C30 N14 C29 120.6(3) . . ? C28 N14 C29 118.7(3) . . ? C33 N15 C31 121.1(3) . . ? C33 N15 C32 120.3(3) . . ? C31 N15 C32 118.4(3) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 C7 120.9(3) . . ? C6 C1 C7 120.2(3) . . ? C1 C2 C3 120.4(3) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 C8 119.7(3) . . ? C3 C4 C8 121.3(3) . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C1 C6 C5 120.9(3) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? N1 C7 C1 111.9(2) . . ? N1 C7 H7A 109.2 . . ? C1 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N4 C8 C4 113.1(3) . . ? N4 C8 H8A 109.0 . . ? C4 C8 H8A 109.0 . . ? N4 C8 H8B 109.0 . . ? C4 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N2 C9 N3 114.8(3) . . ? N2 C9 H9A 122.6 . . ? N3 C9 H9A 122.6 . . ? N1 C10 N3 110.3(3) . . ? N1 C10 H10A 124.9 . . ? N3 C10 H10A 124.9 . . ? N5 C11 N6 114.6(3) . . ? N5 C11 H11A 122.7 . . ? N6 C11 H11A 122.7 . . ? N6 C12 N4 110.3(3) . . ? N6 C12 H12A 124.8 . . ? N4 C12 H12A 124.8 . . ? C18 C13 C14 118.7(3) . . ? C18 C13 C19 120.3(3) . . ? C14 C13 C19 121.0(3) . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C17 C16 C15 118.8(3) . . ? C17 C16 C20 120.5(3) . . ? C15 C16 C20 120.6(3) . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C17 C18 C13 120.6(3) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? N7 C19 C13 110.9(2) . . ? N7 C19 H19A 109.4 . . ? C13 C19 H19A 109.4 . . ? N7 C19 H19B 109.4 . . ? C13 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N10 C20 C16 112.3(2) . . ? N10 C20 H20A 109.1 . . ? C16 C20 H20A 109.1 . . ? N10 C20 H20B 109.1 . . ? C16 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? N8 C21 N9 114.3(3) . . ? N8 C21 H21A 122.9 . . ? N9 C21 H21A 122.9 . . ? N7 C22 N9 109.8(3) . . ? N7 C22 H22A 125.1 . . ? N9 C22 H22A 125.1 . . ? N11 C23 N12 115.0(3) . . ? N11 C23 H23A 122.5 . . ? N12 C23 H23A 122.5 . . ? N12 C24 N10 110.3(3) . . ? N12 C24 H24A 124.8 . . ? N10 C24 H24A 124.8 . . ? N13 C25 H25A 109.5 . . ? N13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N13 C26 H26A 109.5 . . ? N13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 N13 124.7(5) . . ? O3 C27 H27A 117.7 . . ? N13 C27 H27A 117.7 . . ? N14 C28 H28A 109.5 . . ? N14 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N14 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N14 C29 H29A 109.5 . . ? N14 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N14 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O4 C30 N14 125.9(4) . . ? O4 C30 H30A 117.1 . . ? N14 C30 H30A 117.1 . . ? N15 C31 H31A 109.5 . . ? N15 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N15 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N15 C32 H32A 109.5 . . ? N15 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N15 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 N15 125.1(4) . . ? O5 C33 H33A 117.4 . . ? N15 C33 H33A 117.4 . . ? O14 O12 Cl2 76.5(11) . . ? O14 O12 O15 119.5(15) . . ? Cl2 O12 O15 47.4(6) . . ? O15 O13 Cl2 56.8(17) . . ? O12 O14 Cl2 67.5(11) . . ? O13 O15 Cl2 97(2) . . ? O13 O15 O12 147(2) . . ? Cl2 O15 O12 52.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 N1 N2 C9 -0.5(3) . . . . ? C7 N1 N2 C9 -176.4(3) . . . . ? N9 Cd1 N3 C10 -19(4) . . . . ? N6 Cd1 N3 C10 -68.9(3) 2_666 . . . ? O2 Cd1 N3 C10 -162.4(3) . . . . ? N12 Cd1 N3 C10 106.8(3) 2 . . . ? O1 Cd1 N3 C10 20.2(3) . . . . ? N9 Cd1 N3 C9 170(4) . . . . ? N6 Cd1 N3 C9 120.1(3) 2_666 . . . ? O2 Cd1 N3 C9 26.6(3) . . . . ? N12 Cd1 N3 C9 -64.2(3) 2 . . . ? O1 Cd1 N3 C9 -150.8(3) . . . . ? C12 N4 N5 C11 0.8(3) . . . . ? C8 N4 N5 C11 178.7(3) . . . . ? C22 N7 N8 C21 0.3(3) . . . . ? C19 N7 N8 C21 178.6(3) . . . . ? N3 Cd1 N9 C22 -163(4) . . . . ? N6 Cd1 N9 C22 -113.8(3) 2_666 . . . ? O2 Cd1 N9 C22 -20.4(3) . . . . ? N12 Cd1 N9 C22 70.5(3) 2 . . . ? O1 Cd1 N9 C22 157.0(3) . . . . ? N3 Cd1 N9 C21 6(4) . . . . ? N6 Cd1 N9 C21 55.1(3) 2_666 . . . ? O2 Cd1 N9 C21 148.6(3) . . . . ? N12 Cd1 N9 C21 -120.6(3) 2 . . . ? O1 Cd1 N9 C21 -34.0(3) . . . . ? C24 N10 N11 C23 -0.5(3) . . . . ? C20 N10 N11 C23 -179.3(3) . . . . ? C6 C1 C2 C3 -1.2(5) . . . . ? C7 C1 C2 C3 178.3(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C2 C3 C4 C8 -176.1(3) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C8 C4 C5 C6 175.7(3) . . . . ? C2 C1 C6 C5 0.7(5) . . . . ? C7 C1 C6 C5 -178.9(3) . . . . ? C4 C5 C6 C1 0.6(5) . . . . ? C10 N1 C7 C1 126.6(3) . . . . ? N2 N1 C7 C1 -58.4(4) . . . . ? C2 C1 C7 N1 -68.9(4) . . . . ? C6 C1 C7 N1 110.6(3) . . . . ? C12 N4 C8 C4 100.0(4) . . . . ? N5 N4 C8 C4 -77.5(4) . . . . ? C5 C4 C8 N4 133.9(3) . . . . ? C3 C4 C8 N4 -49.2(4) . . . . ? N1 N2 C9 N3 0.3(4) . . . . ? C10 N3 C9 N2 0.0(4) . . . . ? Cd1 N3 C9 N2 173.0(2) . . . . ? N2 N1 C10 N3 0.6(4) . . . . ? C7 N1 C10 N3 176.1(3) . . . . ? C9 N3 C10 N1 -0.4(3) . . . . ? Cd1 N3 C10 N1 -172.98(19) . . . . ? N4 N5 C11 N6 -0.3(4) . . . . ? C12 N6 C11 N5 -0.3(4) . . . . ? Cd1 N6 C11 N5 178.2(2) 2_666 . . . ? C11 N6 C12 N4 0.8(3) . . . . ? Cd1 N6 C12 N4 -177.59(19) 2_666 . . . ? N5 N4 C12 N6 -1.0(4) . . . . ? C8 N4 C12 N6 -178.8(3) . . . . ? C18 C13 C14 C15 -0.4(5) . . . . ? C19 C13 C14 C15 -179.2(3) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C17 0.7(5) . . . . ? C14 C15 C16 C20 178.1(3) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C20 C16 C17 C18 -177.9(3) . . . . ? C16 C17 C18 C13 -0.3(5) . . . . ? C14 C13 C18 C17 0.7(5) . . . . ? C19 C13 C18 C17 179.5(3) . . . . ? C22 N7 C19 C13 -131.1(3) . . . . ? N8 N7 C19 C13 51.0(4) . . . . ? C18 C13 C19 N7 -119.3(3) . . . . ? C14 C13 C19 N7 59.4(4) . . . . ? C24 N10 C20 C16 -99.1(4) . . . . ? N11 N10 C20 C16 79.4(3) . . . . ? C17 C16 C20 N10 -122.6(3) . . . . ? C15 C16 C20 N10 60.0(4) . . . . ? N7 N8 C21 N9 0.0(4) . . . . ? C22 N9 C21 N8 -0.3(4) . . . . ? Cd1 N9 C21 N8 -171.3(2) . . . . ? N8 N7 C22 N9 -0.5(3) . . . . ? C19 N7 C22 N9 -178.6(3) . . . . ? C21 N9 C22 N7 0.5(3) . . . . ? Cd1 N9 C22 N7 171.59(18) . . . . ? N10 N11 C23 N12 0.8(4) . . . . ? C24 N12 C23 N11 -0.8(4) . . . . ? Cd1 N12 C23 N11 177.8(2) 2 . . . ? C23 N12 C24 N10 0.4(3) . . . . ? Cd1 N12 C24 N10 -178.10(18) 2 . . . ? N11 N10 C24 N12 0.1(3) . . . . ? C20 N10 C24 N12 178.7(3) . . . . ? C26 N13 C27 O3 -175.3(4) . . . . ? C25 N13 C27 O3 0.8(7) . . . . ? C28 N14 C30 O4 -175.3(4) . . . . ? C29 N14 C30 O4 1.6(6) . . . . ? C31 N15 C33 O5 175.9(4) . . . . ? C32 N15 C33 O5 1.0(6) . . . . ? O15 Cl2 O12 O14 -155.5(16) . . . . ? O11 Cl2 O12 O14 -46.8(15) . . . . ? O10 Cl2 O12 O14 87.5(14) . . . . ? O13 Cl2 O12 O14 -162.6(13) . . . . ? O11 Cl2 O12 O15 108.7(9) . . . . ? O10 Cl2 O12 O15 -117.0(8) . . . . ? O14 Cl2 O12 O15 155.5(16) . . . . ? O13 Cl2 O12 O15 -7.1(11) . . . . ? O12 Cl2 O13 O15 16(3) . . . . ? O11 Cl2 O13 O15 -113(2) . . . . ? O10 Cl2 O13 O15 131(2) . . . . ? O14 Cl2 O13 O15 1(3) . . . . ? O15 O12 O14 Cl2 -20.6(12) . . . . ? O15 Cl2 O14 O12 26.3(17) . . . . ? O11 Cl2 O14 O12 142.3(13) . . . . ? O10 Cl2 O14 O12 -104.0(13) . . . . ? O13 Cl2 O14 O12 25.9(19) . . . . ? Cl2 O13 O15 O12 -24(4) . . . . ? O12 Cl2 O15 O13 -164(3) . . . . ? O11 Cl2 O15 O13 74(2) . . . . ? O10 Cl2 O15 O13 -57(3) . . . . ? O14 Cl2 O15 O13 -179(2) . . . . ? O11 Cl2 O15 O12 -122.1(7) . . . . ? O10 Cl2 O15 O12 107.3(7) . . . . ? O14 Cl2 O15 O12 -15.4(11) . . . . ? O13 Cl2 O15 O12 164(3) . . . . ? O14 O12 O15 O13 58(6) . . . . ? Cl2 O12 O15 O13 30(5) . . . . ? O14 O12 O15 Cl2 27.6(16) . . . . ? 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 O1 HW1 O4 0.79(2) 1.89(2) 2.673(4) 172(4) . O2 HW3 O5 0.80(2) 1.90(2) 2.698(4) 173(4) . O1 HW2 O8 0.76(2) 2.13(2) 2.885(4) 170(4) . O2 HW4 O3 0.83(2) 1.83(3) 2.659(4) 178(4) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.687 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.066 ###=====================