# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 893929' #TrackingRef 'crystallographic data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H34 Cd Cl2 N8 O10' _chemical_formula_weight 934.02 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' 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' H H 0.0000 0.0000 '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 C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 7.1159(14) _cell_length_b 17.478(3) _cell_length_c 15.208(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.66(3) _cell_angle_gamma 90.00 _cell_volume 1878.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2419 _cell_measurement_theta_min 2.3304 _cell_measurement_theta_max 27.8644 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113.15 _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 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7056 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1694 _reflns_number_gt 1649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0906P)^2^+12.4972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1694 _refine_ls_number_parameters 146 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.0000 0.5000 0.0220(3) Uani 1 4 d S . . N1 N 0.3774(6) 0.0954(2) 0.5809(2) 0.0260(8) Uani 1 1 d . . . N2 N 0.2941(5) 0.1646(2) 0.6913(2) 0.0230(8) Uani 1 1 d . . . C1 C 0.3961(7) 0.1050(3) 0.6685(3) 0.0285(10) Uani 1 1 d . . . H1 H 0.4704 0.0743 0.7086 0.034 Uiso 1 1 calc R . . C2 C 0.2579(8) 0.1522(3) 0.5477(3) 0.0343(11) Uani 1 1 d . . . H2 H 0.2185 0.1600 0.4879 0.041 Uiso 1 1 calc R . . C3 C 0.2050(8) 0.1957(3) 0.6148(3) 0.0346(11) Uani 1 1 d . . . H3 H 0.1248 0.2379 0.6098 0.041 Uiso 1 1 calc R . . C4 C 0.2791(6) 0.1894(3) 0.7802(3) 0.0263(10) Uani 1 1 d . . . C5 C 0.2661(10) 0.1362(3) 0.8452(4) 0.0454(15) Uani 1 1 d . . . H5 H 0.2640 0.0843 0.8316 0.054 Uiso 1 1 calc R . . C6 C 0.2561(10) 0.1602(3) 0.9315(4) 0.0453(14) Uani 1 1 d . . . H6 H 0.2495 0.1238 0.9756 0.054 Uiso 1 1 calc R . . C7 C 0.2556(6) 0.2373(3) 0.9533(3) 0.0261(10) Uani 1 1 d . . . C8 C 0.2656(7) 0.2895(3) 0.8856(3) 0.0302(10) Uani 1 1 d . . . H8 H 0.2633 0.3415 0.8982 0.036 Uiso 1 1 calc R . . C9 C 0.2789(7) 0.2663(3) 0.7996(3) 0.0287(10) Uani 1 1 d . . . H9 H 0.2876 0.3023 0.7553 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.1266(4) 0.0000 0.31661(16) 0.0208(6) Uani 0.50 2 d SPD . . O1 O 0.2208(10) 0.0259(4) 0.3984(5) 0.0393(18) Uiso 0.25 1 d PD . . O2 O 0.1286(16) -0.0898(7) 0.3338(8) 0.023(2) Uiso 0.25 1 d P . . O3 O 0.2389(12) 0.0000 0.2454(6) 0.0258(19) Uiso 0.50 2 d SP . . O4 O -0.0643(18) 0.0000 0.2971(9) 0.053(3) Uiso 0.50 2 d SP . . Cl2 Cl 0.1959(8) 0.0000 0.1729(3) 0.0658(13) Uani 0.50 2 d SPD . . O5 O 0.1699(19) 0.0639(8) 0.2258(8) 0.094(4) Uiso 0.50 1 d PD . . O6 O 0.3988(18) 0.0000 0.1550(15) 0.112(7) Uiso 0.50 2 d SPD . . O7 O 0.067(3) 0.0000 0.0963(9) 0.104(6) Uiso 0.50 2 d SPD . . C10 C 0.061(2) 0.0000 0.4299(9) 0.108(10) Uiso 0.50 2 d SPD . . O1' O 0.2208(10) 0.0259(4) 0.3984(5) 0.0393(18) Uiso 0.25 1 d P . . O1W O 0.200(3) 0.0000 0.0595(14) 0.095(5) Uiso 0.50 2 d SP . . 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 0.0353(4) 0.0187(4) 0.0137(4) 0.000 0.0093(2) 0.000 N1 0.039(2) 0.0219(19) 0.0189(18) -0.0024(14) 0.0097(16) 0.0011(16) N2 0.0242(18) 0.0246(19) 0.0207(18) -0.0059(15) 0.0057(14) -0.0018(15) C1 0.036(3) 0.029(2) 0.022(2) -0.0013(19) 0.0072(19) 0.006(2) C2 0.052(3) 0.030(2) 0.021(2) -0.0017(19) 0.003(2) 0.009(2) C3 0.044(3) 0.034(3) 0.025(2) -0.006(2) 0.000(2) 0.011(2) C4 0.024(2) 0.033(2) 0.023(2) -0.0116(19) 0.0080(17) -0.0015(18) C5 0.081(4) 0.027(3) 0.033(3) -0.012(2) 0.024(3) -0.012(3) C6 0.079(4) 0.034(3) 0.027(3) -0.009(2) 0.023(3) -0.015(3) C7 0.019(2) 0.033(2) 0.027(2) -0.0118(19) 0.0057(17) -0.0036(18) C8 0.033(2) 0.029(2) 0.027(2) -0.0116(19) 0.0004(19) 0.008(2) C9 0.030(2) 0.030(2) 0.025(2) -0.0045(19) 0.0008(19) 0.0053(19) Cl1 0.0122(12) 0.0427(17) 0.0072(12) 0.000 0.0002(9) 0.000 Cl2 0.089(4) 0.047(3) 0.058(3) 0.000 -0.007(3) 0.000 _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 N1 2.303(4) 2_656 ? Cd1 N1 2.303(4) 6 ? Cd1 N1 2.303(4) . ? Cd1 N1 2.303(4) 5_656 ? Cd1 O1' 2.414(7) 6 ? Cd1 O1 2.414(7) 6 ? Cd1 O1' 2.414(7) 2_656 ? Cd1 O1 2.414(7) 2_656 ? Cd1 O1 2.414(7) . ? Cd1 O1' 2.414(7) 5_656 ? Cd1 O1 2.414(7) 5_656 ? N1 C1 1.334(6) . ? N1 C2 1.365(6) . ? N2 C1 1.337(6) . ? N2 C3 1.371(6) . ? N2 C4 1.436(5) . ? C1 H1 0.9300 . ? C2 C3 1.360(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.366(7) . ? C4 C9 1.376(7) . ? C5 C6 1.387(7) . ? C5 H5 0.9300 . ? C6 C7 1.387(7) . ? C6 H6 0.9300 . ? C7 C8 1.384(7) . ? C7 C7 1.500(9) 7_557 ? C8 C9 1.381(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? Cl1 O4 1.357(13) . ? Cl1 O1 1.417(7) . ? Cl1 O1 1.417(7) 6 ? Cl1 O1' 1.417(7) 6 ? Cl1 O3 1.418(10) . ? Cl1 O2 1.591(12) 6 ? Cl1 O2 1.591(12) . ? Cl1 O5 1.830(14) 6 ? O1 O1' 0.906(13) 6 ? O1 O1 0.906(13) 6 ? O1 C10 1.362(10) . ? O1 O2 1.579(13) 6 ? O2 O1' 1.579(13) 6 ? O2 O1 1.579(13) 6 ? O2 O5 1.762(17) 6 ? O3 O5 1.242(14) 6 ? Cl2 O7 1.396(9) . ? Cl2 O5 1.401(12) 6 ? Cl2 O5 1.401(12) . ? Cl2 O6 1.500(10) . ? O5 O2 1.761(17) 6 ? C10 O1 1.362(10) 6 ? C10 O1' 1.362(10) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0 2_656 6 ? N1 Cd1 N1 87.26(19) 2_656 . ? N1 Cd1 N1 92.74(19) 6 . ? N1 Cd1 N1 92.74(19) 2_656 5_656 ? N1 Cd1 N1 87.26(19) 6 5_656 ? N1 Cd1 N1 179.999(1) . 5_656 ? N1 Cd1 O1' 97.38(19) 2_656 6 ? N1 Cd1 O1' 82.62(19) 6 6 ? N1 Cd1 O1' 98.23(19) . 6 ? N1 Cd1 O1' 81.77(19) 5_656 6 ? N1 Cd1 O1 97.38(19) 2_656 6 ? N1 Cd1 O1 82.62(19) 6 6 ? N1 Cd1 O1 98.23(19) . 6 ? N1 Cd1 O1 81.77(19) 5_656 6 ? O1' Cd1 O1 0.0(5) 6 6 ? N1 Cd1 O1' 82.62(19) 2_656 2_656 ? N1 Cd1 O1' 97.38(19) 6 2_656 ? N1 Cd1 O1' 81.77(19) . 2_656 ? N1 Cd1 O1' 98.23(19) 5_656 2_656 ? O1' Cd1 O1' 179.999(1) 6 2_656 ? O1 Cd1 O1' 179.999(1) 6 2_656 ? N1 Cd1 O1 82.62(19) 2_656 2_656 ? N1 Cd1 O1 97.38(19) 6 2_656 ? N1 Cd1 O1 81.77(19) . 2_656 ? N1 Cd1 O1 98.23(19) 5_656 2_656 ? O1' Cd1 O1 179.999(1) 6 2_656 ? O1 Cd1 O1 179.999(1) 6 2_656 ? O1' Cd1 O1 0.0(3) 2_656 2_656 ? N1 Cd1 O1 81.77(19) 2_656 . ? N1 Cd1 O1 98.23(19) 6 . ? N1 Cd1 O1 82.62(19) . . ? N1 Cd1 O1 97.38(19) 5_656 . ? O1' Cd1 O1 21.6(3) 6 . ? O1 Cd1 O1 21.6(3) 6 . ? O1' Cd1 O1 158.4(3) 2_656 . ? O1 Cd1 O1 158.4(3) 2_656 . ? N1 Cd1 O1' 98.23(19) 2_656 5_656 ? N1 Cd1 O1' 81.77(19) 6 5_656 ? N1 Cd1 O1' 97.38(19) . 5_656 ? N1 Cd1 O1' 82.62(19) 5_656 5_656 ? O1' Cd1 O1' 158.4(3) 6 5_656 ? O1 Cd1 O1' 158.4(3) 6 5_656 ? O1' Cd1 O1' 21.6(3) 2_656 5_656 ? O1 Cd1 O1' 21.6(3) 2_656 5_656 ? O1 Cd1 O1' 179.998(1) . 5_656 ? N1 Cd1 O1 98.23(19) 2_656 5_656 ? N1 Cd1 O1 81.77(19) 6 5_656 ? N1 Cd1 O1 97.38(19) . 5_656 ? N1 Cd1 O1 82.62(19) 5_656 5_656 ? O1' Cd1 O1 158.4(3) 6 5_656 ? O1 Cd1 O1 158.4(3) 6 5_656 ? O1' Cd1 O1 21.6(3) 2_656 5_656 ? O1 Cd1 O1 21.6(3) 2_656 5_656 ? O1 Cd1 O1 179.998(1) . 5_656 ? O1' Cd1 O1 0.0(5) 5_656 5_656 ? C1 N1 C2 105.3(4) . . ? C1 N1 Cd1 128.7(3) . . ? C2 N1 Cd1 125.9(3) . . ? C1 N2 C3 107.5(4) . . ? C1 N2 C4 125.5(4) . . ? C3 N2 C4 127.0(4) . . ? N1 C1 N2 111.2(4) . . ? N1 C1 H1 124.4 . . ? N2 C1 H1 124.4 . . ? C3 C2 N1 110.1(4) . . ? C3 C2 H2 124.9 . . ? N1 C2 H2 124.9 . . ? C2 C3 N2 105.9(4) . . ? C2 C3 H3 127.1 . . ? N2 C3 H3 127.1 . . ? C5 C4 C9 120.5(4) . . ? C5 C4 N2 119.7(4) . . ? C9 C4 N2 119.9(4) . . ? C4 C5 C6 119.6(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 121.4(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 117.4(4) . . ? C8 C7 C7 121.5(5) . 7_557 ? C6 C7 C7 121.1(6) . 7_557 ? C9 C8 C7 121.7(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C4 C9 C8 119.4(5) . . ? C4 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? O4 Cl1 O1 123.5(6) . . ? O4 Cl1 O1 123.5(6) . 6 ? O1 Cl1 O1 37.3(5) . 6 ? O4 Cl1 O1' 123.5(6) . 6 ? O1 Cl1 O1' 37.3(5) . 6 ? O1 Cl1 O1' 0.0(6) 6 6 ? O4 Cl1 O3 118.1(7) . . ? O1 Cl1 O3 114.8(5) . . ? O1 Cl1 O3 114.8(5) 6 . ? O1' Cl1 O3 114.8(5) 6 . ? O4 Cl1 O2 91.5(4) . 6 ? O1 Cl1 O2 63.0(5) . 6 ? O1 Cl1 O2 100.2(5) 6 6 ? O1' Cl1 O2 100.2(5) 6 6 ? O3 Cl1 O2 97.5(4) . 6 ? O4 Cl1 O2 91.5(4) . . ? O1 Cl1 O2 100.2(5) . . ? O1 Cl1 O2 63.0(5) 6 . ? O1' Cl1 O2 63.0(5) 6 . ? O3 Cl1 O2 97.5(4) . . ? O2 Cl1 O2 161.1(9) 6 . ? O4 Cl1 O5 95.0(6) . 6 ? O1 Cl1 O5 138.9(5) . 6 ? O1 Cl1 O5 111.3(4) 6 6 ? O1' Cl1 O5 111.3(4) 6 6 ? O3 Cl1 O5 42.7(4) . 6 ? O2 Cl1 O5 136.7(6) 6 6 ? O2 Cl1 O5 61.5(6) . 6 ? O1' O1 O1 0.0(13) 6 6 ? O1' O1 C10 70.6(3) 6 . ? O1 O1 C10 70.6(3) 6 . ? O1' O1 Cl1 71.4(3) 6 . ? O1 O1 Cl1 71.4(3) 6 . ? C10 O1 Cl1 82.7(7) . . ? O1' O1 O2 135.0(5) 6 6 ? O1 O1 O2 135.0(5) 6 6 ? C10 O1 O2 98.6(8) . 6 ? Cl1 O1 O2 63.9(5) . 6 ? O1' O1 Cd1 79.18(16) 6 . ? O1 O1 Cd1 79.18(16) 6 . ? C10 O1 Cd1 111.8(8) . . ? Cl1 O1 Cd1 140.6(4) . . ? O2 O1 Cd1 141.5(6) 6 . ? O1' O2 O1 0.0(7) 6 6 ? O1' O2 Cl1 53.1(5) 6 . ? O1 O2 Cl1 53.1(5) 6 . ? O1' O2 O5 107.2(8) 6 6 ? O1 O2 O5 107.2(8) 6 6 ? Cl1 O2 O5 65.9(6) . 6 ? O5 O3 Cl1 86.6(8) 6 . ? O7 Cl2 O5 111.2(7) . 6 ? O7 Cl2 O5 111.2(7) . . ? O5 Cl2 O5 105.7(12) 6 . ? O7 Cl2 O6 113.6(13) . . ? O5 Cl2 O6 107.4(8) 6 . ? O5 Cl2 O6 107.4(8) . . ? Cl2 O5 O2 142.0(11) . 6 ? O1 C10 O1 38.9(6) . 6 ? O1 C10 O1' 38.9(6) . 6 ? O1 C10 O1' 0.0(7) 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 N1 Cd1 N1 C1 -127.2(5) 2_656 . . . ? N1 Cd1 N1 C1 52.8(5) 6 . . . ? N1 Cd1 N1 C1 -156(12) 5_656 . . . ? O1' Cd1 N1 C1 135.7(4) 6 . . . ? O1 Cd1 N1 C1 135.7(4) 6 . . . ? O1' Cd1 N1 C1 -44.3(4) 2_656 . . . ? O1 Cd1 N1 C1 -44.3(4) 2_656 . . . ? O1 Cd1 N1 C1 150.7(4) . . . . ? O1' Cd1 N1 C1 -29.3(4) 5_656 . . . ? O1 Cd1 N1 C1 -29.3(4) 5_656 . . . ? N1 Cd1 N1 C2 57.2(4) 2_656 . . . ? N1 Cd1 N1 C2 -122.8(4) 6 . . . ? N1 Cd1 N1 C2 29(12) 5_656 . . . ? O1' Cd1 N1 C2 -39.8(4) 6 . . . ? O1 Cd1 N1 C2 -39.8(4) 6 . . . ? O1' Cd1 N1 C2 140.2(4) 2_656 . . . ? O1 Cd1 N1 C2 140.2(4) 2_656 . . . ? O1 Cd1 N1 C2 -24.8(4) . . . . ? O1' Cd1 N1 C2 155.2(4) 5_656 . . . ? O1 Cd1 N1 C2 155.2(4) 5_656 . . . ? C2 N1 C1 N2 0.2(6) . . . . ? Cd1 N1 C1 N2 -176.0(3) . . . . ? C3 N2 C1 N1 -0.3(6) . . . . ? C4 N2 C1 N1 178.3(4) . . . . ? C1 N1 C2 C3 0.0(6) . . . . ? Cd1 N1 C2 C3 176.4(3) . . . . ? N1 C2 C3 N2 -0.2(6) . . . . ? C1 N2 C3 C2 0.3(6) . . . . ? C4 N2 C3 C2 -178.3(4) . . . . ? C1 N2 C4 C5 -39.7(7) . . . . ? C3 N2 C4 C5 138.7(6) . . . . ? C1 N2 C4 C9 140.0(5) . . . . ? C3 N2 C4 C9 -41.6(7) . . . . ? C9 C4 C5 C6 -1.2(9) . . . . ? N2 C4 C5 C6 178.5(5) . . . . ? C4 C5 C6 C7 1.1(10) . . . . ? C5 C6 C7 C8 0.0(9) . . . . ? C5 C6 C7 C7 179.9(6) . . . 7_557 ? C6 C7 C8 C9 -1.1(7) . . . . ? C7 C7 C8 C9 179.0(5) 7_557 . . . ? C5 C4 C9 C8 0.1(7) . . . . ? N2 C4 C9 C8 -179.6(4) . . . . ? C7 C8 C9 C4 1.1(7) . . . . ? O4 Cl1 O1 O1' 102.9(4) . . . 6 ? O1 Cl1 O1 O1' 0.000(2) 6 . . 6 ? O3 Cl1 O1 O1' -99.0(2) . . . 6 ? O2 Cl1 O1 O1' 175.3(5) 6 . . 6 ? O2 Cl1 O1 O1' 4.3(4) . . . 6 ? O5 Cl1 O1 O1' -53.6(7) 6 . . 6 ? O4 Cl1 O1 O1 102.9(4) . . . 6 ? O1' Cl1 O1 O1 0.000(2) 6 . . 6 ? O3 Cl1 O1 O1 -99.0(2) . . . 6 ? O2 Cl1 O1 O1 175.3(5) 6 . . 6 ? O2 Cl1 O1 O1 4.3(4) . . . 6 ? O5 Cl1 O1 O1 -53.6(7) 6 . . 6 ? O4 Cl1 O1 C10 31.0(6) . . . . ? O1 Cl1 O1 C10 -71.9(4) 6 . . . ? O1' Cl1 O1 C10 -71.9(4) 6 . . . ? O3 Cl1 O1 C10 -170.8(4) . . . . ? O2 Cl1 O1 C10 103.4(6) 6 . . . ? O2 Cl1 O1 C10 -67.6(6) . . . . ? O5 Cl1 O1 C10 -125.5(7) 6 . . . ? O4 Cl1 O1 O2 -72.4(6) . . . 6 ? O1 Cl1 O1 O2 -175.3(5) 6 . . 6 ? O1' Cl1 O1 O2 -175.3(5) 6 . . 6 ? O3 Cl1 O1 O2 85.8(5) . . . 6 ? O2 Cl1 O1 O2 -171.0(9) . . . 6 ? O5 Cl1 O1 O2 131.1(8) 6 . . 6 ? O4 Cl1 O1 Cd1 146.7(5) . . . . ? O1 Cl1 O1 Cd1 43.8(7) 6 . . . ? O1' Cl1 O1 Cd1 43.8(7) 6 . . . ? O3 Cl1 O1 Cd1 -55.2(7) . . . . ? O2 Cl1 O1 Cd1 -140.9(9) 6 . . . ? O2 Cl1 O1 Cd1 48.1(8) . . . . ? O5 Cl1 O1 Cd1 -9.8(11) 6 . . . ? N1 Cd1 O1 O1' 135.80(10) 2_656 . . 6 ? N1 Cd1 O1 O1' -44.20(10) 6 . . 6 ? N1 Cd1 O1 O1' -135.92(10) . . . 6 ? N1 Cd1 O1 O1' 44.08(10) 5_656 . . 6 ? O1 Cd1 O1 O1' 0.000(2) 6 . . 6 ? O1' Cd1 O1 O1' 179.997(2) 2_656 . . 6 ? O1 Cd1 O1 O1' 179.997(2) 2_656 . . 6 ? O1' Cd1 O1 O1' 42(5) 5_656 . . 6 ? O1 Cd1 O1 O1' 42(5) 5_656 . . 6 ? N1 Cd1 O1 O1 135.80(10) 2_656 . . 6 ? N1 Cd1 O1 O1 -44.20(10) 6 . . 6 ? N1 Cd1 O1 O1 -135.92(10) . . . 6 ? N1 Cd1 O1 O1 44.08(10) 5_656 . . 6 ? O1' Cd1 O1 O1 0.000(2) 6 . . 6 ? O1' Cd1 O1 O1 179.997(2) 2_656 . . 6 ? O1 Cd1 O1 O1 179.997(2) 2_656 . . 6 ? O1' Cd1 O1 O1 42(5) 5_656 . . 6 ? O1 Cd1 O1 O1 42(5) 5_656 . . 6 ? N1 Cd1 O1 C10 -160.4(5) 2_656 . . . ? N1 Cd1 O1 C10 19.6(5) 6 . . . ? N1 Cd1 O1 C10 -72.1(4) . . . . ? N1 Cd1 O1 C10 107.9(4) 5_656 . . . ? O1' Cd1 O1 C10 63.8(4) 6 . . . ? O1 Cd1 O1 C10 63.8(4) 6 . . . ? O1' Cd1 O1 C10 -116.2(4) 2_656 . . . ? O1 Cd1 O1 C10 -116.2(4) 2_656 . . . ? O1' Cd1 O1 C10 106(5) 5_656 . . . ? O1 Cd1 O1 C10 106(5) 5_656 . . . ? N1 Cd1 O1 Cl1 93.9(7) 2_656 . . . ? N1 Cd1 O1 Cl1 -86.1(7) 6 . . . ? N1 Cd1 O1 Cl1 -177.8(7) . . . . ? N1 Cd1 O1 Cl1 2.2(7) 5_656 . . . ? O1' Cd1 O1 Cl1 -41.9(7) 6 . . . ? O1 Cd1 O1 Cl1 -41.9(7) 6 . . . ? O1' Cd1 O1 Cl1 138.1(7) 2_656 . . . ? O1 Cd1 O1 Cl1 138.1(7) 2_656 . . . ? O1' Cd1 O1 Cl1 0(6) 5_656 . . . ? O1 Cd1 O1 Cl1 0(6) 5_656 . . . ? N1 Cd1 O1 O2 -20.7(9) 2_656 . . 6 ? N1 Cd1 O1 O2 159.3(9) 6 . . 6 ? N1 Cd1 O1 O2 67.6(9) . . . 6 ? N1 Cd1 O1 O2 -112.4(9) 5_656 . . 6 ? O1' Cd1 O1 O2 -156.5(9) 6 . . 6 ? O1 Cd1 O1 O2 -156.5(9) 6 . . 6 ? O1' Cd1 O1 O2 23.5(9) 2_656 . . 6 ? O1 Cd1 O1 O2 23.5(9) 2_656 . . 6 ? O1' Cd1 O1 O2 -114(5) 5_656 . . 6 ? O1 Cd1 O1 O2 -114(5) 5_656 . . 6 ? O4 Cl1 O2 O1' -127.4(7) . . . 6 ? O1 Cl1 O2 O1' -2.9(3) . . . 6 ? O1 Cl1 O2 O1' 0.000(2) 6 . . 6 ? O3 Cl1 O2 O1' 114.0(5) . . . 6 ? O2 Cl1 O2 O1' -29(3) 6 . . 6 ? O5 Cl1 O2 O1' 137.8(7) 6 . . 6 ? O4 Cl1 O2 O1 -127.4(7) . . . 6 ? O1 Cl1 O2 O1 -2.9(3) . . . 6 ? O1' Cl1 O2 O1 0.000(2) 6 . . 6 ? O3 Cl1 O2 O1 114.0(5) . . . 6 ? O2 Cl1 O2 O1 -29(3) 6 . . 6 ? O5 Cl1 O2 O1 137.8(7) 6 . . 6 ? O4 Cl1 O2 O5 94.9(8) . . . 6 ? O1 Cl1 O2 O5 -140.7(6) . . . 6 ? O1 Cl1 O2 O5 -137.8(7) 6 . . 6 ? O1' Cl1 O2 O5 -137.8(7) 6 . . 6 ? O3 Cl1 O2 O5 -23.8(7) . . . 6 ? O2 Cl1 O2 O5 -166(2) 6 . . 6 ? O4 Cl1 O3 O5 -64.2(6) . . . 6 ? O1 Cl1 O3 O5 136.4(7) . . . 6 ? O1 Cl1 O3 O5 95.2(7) 6 . . 6 ? O1' Cl1 O3 O5 95.2(7) 6 . . 6 ? O2 Cl1 O3 O5 -159.9(7) 6 . . 6 ? O2 Cl1 O3 O5 31.5(8) . . . 6 ? O7 Cl2 O5 O2 125.0(17) . . . 6 ? O5 Cl2 O5 O2 4(2) 6 . . 6 ? O6 Cl2 O5 O2 -110.2(17) . . . 6 ? O1' O1 C10 O1 0.000(3) 6 . . 6 ? Cl1 O1 C10 O1 72.7(4) . . . 6 ? O2 O1 C10 O1 134.8(5) 6 . . 6 ? Cd1 O1 C10 O1 -69.2(5) . . . 6 ? O1 O1 C10 O1' 0.000(3) 6 . . 6 ? Cl1 O1 C10 O1' 72.7(4) . . . 6 ? O2 O1 C10 O1' 134.8(5) 6 . . 6 ? Cd1 O1 C10 O1' -69.2(5) . . . 6 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.907 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.134 data_2 _database_code_depnum_ccdc_archive 'CCDC 893930' #TrackingRef 'crystallographic data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Cd Cl2 N8 O4' _chemical_formula_weight 819.96 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 p2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 10.558(2) _cell_length_b 25.831(5) _cell_length_c 16.593(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.93(3) _cell_angle_gamma 90.00 _cell_volume 4492.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5162 _cell_measurement_theta_min 1.4661 _cell_measurement_theta_max 27.8884 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113.15 _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 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30520 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7805 _reflns_number_gt 5086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0651P)^2^+7.1188P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7805 _refine_ls_number_parameters 462 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.99954(4) 0.248489(16) 0.74747(2) 0.02389(16) Uani 1 1 d . . . N1 N 0.9799(5) 0.2139(2) 0.6183(3) 0.0347(12) Uani 1 1 d . . . N2 N 1.0266(5) 0.1904(2) 0.4969(3) 0.0408(14) Uani 1 1 d . . . N3 N 0.9576(5) 0.3321(2) 0.7040(4) 0.0430(14) Uani 1 1 d . . . N4 N 0.8464(6) 0.3982(2) 0.6515(4) 0.0537(16) Uani 1 1 d . . . N5 N 1.0223(5) 0.27785(19) 0.8813(3) 0.0331(12) Uani 1 1 d . . . N6 N 0.9783(5) 0.2890(2) 1.0053(3) 0.0484(16) Uani 1 1 d . . . N7 N 1.0389(5) 0.16747(18) 0.7974(3) 0.0279(11) Uani 1 1 d . . . N8 N 1.1405(4) 0.10203(19) 0.8596(3) 0.0321(12) Uani 1 1 d . . . Cl1 Cl 1.2500 0.26739(8) 0.7500 0.0291(5) Uani 1 2 d S . . Cl2 Cl 0.7500 0.23198(8) 0.7500 0.0283(5) Uani 1 2 d S . . C1 C 1.0548(6) 0.2214(3) 0.5627(4) 0.0358(15) Uani 1 1 d . . . H1 H 1.1207 0.2455 0.5675 0.043 Uiso 1 1 calc R . . C2 C 0.8954(7) 0.1766(3) 0.5864(4) 0.0498(19) Uani 1 1 d . . . H2 H 0.8295 0.1631 0.6125 0.060 Uiso 1 1 calc R . . C3 C 0.9214(7) 0.1621(3) 0.5116(4) 0.052(2) Uani 1 1 d . . . H3 H 0.8772 0.1380 0.4772 0.062 Uiso 1 1 calc R . . C4 C 1.0930(6) 0.1889(3) 0.4264(4) 0.0373(16) Uani 1 1 d . . . C5 C 1.0990(8) 0.1447(3) 0.3846(5) 0.066(3) Uani 1 1 d . . . H5 H 1.0616 0.1147 0.4015 0.079 Uiso 1 1 calc R . . C6 C 1.1626(9) 0.1444(3) 0.3149(5) 0.071(3) Uani 1 1 d . . . H6 H 1.1685 0.1134 0.2870 0.086 Uiso 1 1 calc R . . C7 C 1.2153(6) 0.1873(3) 0.2868(4) 0.0405(17) Uani 1 1 d . . . C8 C 1.2096(11) 0.2305(4) 0.3310(6) 0.099(4) Uani 1 1 d . . . H8 H 1.2514 0.2601 0.3160 0.119 Uiso 1 1 calc R . . C9 C 1.1424(9) 0.2328(3) 0.3996(5) 0.081(3) Uani 1 1 d . . . H9 H 1.1326 0.2641 0.4258 0.097 Uiso 1 1 calc R . . C10 C 0.8501(6) 0.3477(2) 0.6647(4) 0.0340(15) Uani 1 1 d . . . H10 H 0.7828 0.3255 0.6475 0.041 Uiso 1 1 calc R . . C11 C 1.0316(10) 0.3746(3) 0.7150(8) 0.116(5) Uani 1 1 d . . . H11 H 1.1153 0.3752 0.7399 0.139 Uiso 1 1 calc R . . C12 C 0.9653(10) 0.4160(3) 0.6841(8) 0.126(5) Uani 1 1 d . . . H12 H 0.9939 0.4501 0.6846 0.152 Uiso 1 1 calc R . . C13 C 0.7436(8) 0.4281(3) 0.6080(5) 0.071(2) Uani 1 1 d U . . C14 C 0.6823(9) 0.4089(3) 0.5406(6) 0.092(3) Uani 1 1 d U . . H14 H 0.7049 0.3768 0.5214 0.111 Uiso 1 1 calc R . . C15 C 0.5833(9) 0.4372(3) 0.4985(6) 0.092(3) Uani 1 1 d U . . H15 H 0.5380 0.4230 0.4522 0.111 Uiso 1 1 calc R . . C16 C 0.5520(8) 0.4842(3) 0.5229(6) 0.075(2) Uani 1 1 d U . . C17 C 0.6256(11) 0.5032(4) 0.5864(7) 0.118(3) Uani 1 1 d U . . H17 H 0.6109 0.5369 0.6028 0.142 Uiso 1 1 calc R . . C18 C 0.7248(10) 0.4748(4) 0.6301(6) 0.114(3) Uani 1 1 d U . . H18 H 0.7755 0.4895 0.6739 0.136 Uiso 1 1 calc R . . C19 C 0.9427(6) 0.2664(3) 0.9336(4) 0.0404(16) Uani 1 1 d . . . H19 H 0.8712 0.2454 0.9223 0.049 Uiso 1 1 calc R . . C20 C 1.1141(6) 0.3102(3) 0.9216(4) 0.0447(18) Uani 1 1 d . . . H20 H 1.1818 0.3254 0.8993 0.054 Uiso 1 1 calc R . . C21 C 1.0877(7) 0.3158(4) 0.9992(4) 0.065(3) Uani 1 1 d . . . H21 H 1.1352 0.3343 1.0403 0.078 Uiso 1 1 calc R . . C22 C 0.9134(8) 0.2864(3) 1.0758(4) 0.061(2) Uani 1 1 d . . . C23 C 0.7868(10) 0.2717(5) 1.0697(5) 0.101(4) Uani 1 1 d . . . H23 H 0.7436 0.2634 1.0192 0.121 Uiso 1 1 calc R . . C24 C 0.7231(10) 0.2693(5) 1.1385(5) 0.101(4) Uani 1 1 d . . . H24 H 0.6388 0.2581 1.1333 0.121 Uiso 1 1 calc R . . C25 C 0.7826(9) 0.2830(4) 1.2141(5) 0.083(3) Uani 1 1 d . . . C26 C 0.9055(10) 0.3018(5) 1.2163(5) 0.110(4) Uani 1 1 d . . . H26 H 0.9470 0.3136 1.2655 0.132 Uiso 1 1 calc R . . C27 C 0.9703(9) 0.3037(5) 1.1471(5) 0.115(5) Uani 1 1 d . . . H27 H 1.0526 0.3171 1.1509 0.138 Uiso 1 1 calc R . . C28 C 1.1493(6) 0.1508(2) 0.8319(4) 0.0331(15) Uani 1 1 d . . . H28 H 1.2243 0.1701 0.8366 0.040 Uiso 1 1 calc R . . C29 C 0.9566(5) 0.1266(2) 0.8034(4) 0.0347(15) Uani 1 1 d . . . H29 H 0.8704 0.1269 0.7834 0.042 Uiso 1 1 calc R . . C30 C 1.0177(6) 0.0861(2) 0.8420(4) 0.0440(18) Uani 1 1 d . . . H30 H 0.9832 0.0543 0.8541 0.053 Uiso 1 1 calc R . . C31 C 1.2442(5) 0.0725(2) 0.8998(3) 0.0255(13) Uani 1 1 d . . . C32 C 1.2324(8) 0.0479(4) 0.9703(5) 0.079(3) Uani 1 1 d . . . H32 H 1.1566 0.0507 0.9933 0.095 Uiso 1 1 calc R . . C33 C 1.3302(7) 0.0191(3) 1.0081(5) 0.073(3) Uani 1 1 d . . . H33 H 1.3177 0.0012 1.0551 0.087 Uiso 1 1 calc R . . C34 C 1.4456(5) 0.0154(2) 0.9795(3) 0.0287(14) Uani 1 1 d . . . C35 C 1.4555(7) 0.0404(4) 0.9078(5) 0.070(3) Uani 1 1 d . . . H35 H 1.5313 0.0378 0.8848 0.084 Uiso 1 1 calc R . . C36 C 1.3564(6) 0.0693(3) 0.8684(4) 0.066(3) Uani 1 1 d . . . H36 H 1.3669 0.0866 0.8205 0.080 Uiso 1 1 calc R . . Cl3 Cl 0.7500 0.00668(10) 0.7500 0.0589(8) Uani 1 2 d S . . O1 O 0.8582(6) -0.0245(2) 0.7705(6) 0.131(3) Uani 1 1 d . . . O2 O 0.7689(5) 0.0398(2) 0.6827(3) 0.0696(16) Uani 1 1 d . . . Cl4 Cl 0.2500 0.39103(13) 0.2500 0.0880(11) Uani 1 2 d S . . O3 O 0.2485(8) 0.3595(3) 0.3202(6) 0.146(3) Uani 1 1 d . . . O4 O 0.1366(9) 0.4221(3) 0.2450(5) 0.140(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0201(3) 0.0308(3) 0.0207(2) 0.00218(16) 0.00255(17) 0.00302(16) N1 0.030(3) 0.052(3) 0.022(3) -0.006(2) 0.005(2) -0.005(2) N2 0.051(4) 0.043(3) 0.029(3) -0.007(2) 0.008(3) -0.002(3) N3 0.030(3) 0.036(3) 0.061(4) 0.012(3) 0.000(3) 0.007(3) N4 0.041(4) 0.034(3) 0.081(5) 0.001(3) -0.011(3) 0.003(3) N5 0.027(3) 0.042(3) 0.030(3) -0.005(2) 0.004(2) -0.001(2) N6 0.032(3) 0.099(5) 0.018(3) -0.009(3) 0.015(2) -0.010(3) N7 0.026(3) 0.031(3) 0.027(3) 0.005(2) 0.005(2) -0.001(2) N8 0.023(3) 0.035(3) 0.037(3) 0.017(2) 0.000(2) 0.009(2) Cl1 0.0158(11) 0.0397(12) 0.0317(11) 0.000 0.0021(8) 0.000 Cl2 0.0182(11) 0.0346(11) 0.0330(11) 0.000 0.0067(9) 0.000 C1 0.028(4) 0.053(4) 0.028(3) -0.005(3) 0.009(3) -0.003(3) C2 0.048(5) 0.074(5) 0.031(4) -0.011(3) 0.020(3) -0.009(4) C3 0.047(5) 0.072(5) 0.038(4) -0.005(3) 0.011(3) -0.030(4) C4 0.037(4) 0.048(4) 0.029(3) -0.004(3) 0.011(3) -0.008(3) C5 0.104(7) 0.054(5) 0.049(5) -0.016(4) 0.049(5) -0.030(5) C6 0.122(8) 0.054(5) 0.049(5) -0.013(4) 0.054(5) -0.008(5) C7 0.047(5) 0.050(4) 0.028(3) 0.004(3) 0.019(3) -0.002(3) C8 0.148(10) 0.075(6) 0.093(7) -0.036(6) 0.090(7) -0.064(7) C9 0.115(8) 0.067(6) 0.074(6) -0.035(5) 0.065(6) -0.030(6) C10 0.025(4) 0.028(3) 0.047(4) 0.001(3) -0.003(3) 0.001(3) C11 0.086(7) 0.056(6) 0.183(12) 0.028(7) -0.077(7) -0.032(5) C12 0.093(8) 0.033(5) 0.230(14) 0.041(7) -0.073(9) -0.006(5) C13 0.088(5) 0.031(4) 0.081(5) 0.000(3) -0.048(4) 0.019(4) C14 0.102(6) 0.044(4) 0.116(6) -0.021(4) -0.046(5) 0.034(4) C15 0.100(6) 0.049(4) 0.110(6) -0.018(4) -0.057(5) 0.025(4) C16 0.085(5) 0.039(4) 0.090(5) -0.009(4) -0.039(4) 0.018(4) C17 0.138(6) 0.070(5) 0.124(6) -0.039(5) -0.073(5) 0.062(5) C18 0.137(6) 0.073(5) 0.108(6) -0.035(5) -0.075(5) 0.048(5) C19 0.040(4) 0.060(4) 0.020(3) -0.001(3) 0.000(3) -0.006(3) C20 0.028(4) 0.073(5) 0.033(4) -0.006(3) 0.001(3) -0.018(3) C21 0.028(4) 0.131(8) 0.038(4) -0.035(4) 0.016(3) -0.021(4) C22 0.046(5) 0.107(7) 0.036(4) -0.009(4) 0.026(4) -0.013(4) C23 0.080(8) 0.186(11) 0.039(5) -0.011(6) 0.021(5) -0.052(7) C24 0.085(8) 0.172(10) 0.047(5) -0.019(6) 0.021(5) -0.057(7) C25 0.066(7) 0.156(10) 0.028(4) -0.009(5) 0.007(4) -0.020(6) C26 0.095(8) 0.209(13) 0.032(5) -0.031(6) 0.036(5) -0.056(8) C27 0.072(7) 0.246(14) 0.035(5) -0.035(7) 0.036(5) -0.065(8) C28 0.035(4) 0.031(3) 0.032(3) 0.003(3) 0.000(3) -0.001(3) C29 0.007(3) 0.038(4) 0.057(4) 0.008(3) -0.006(3) 0.006(3) C30 0.018(4) 0.038(4) 0.074(5) 0.012(3) -0.005(3) -0.010(3) C31 0.020(3) 0.032(3) 0.026(3) 0.007(2) 0.007(3) 0.004(2) C32 0.054(6) 0.114(7) 0.076(6) 0.048(5) 0.039(5) 0.057(5) C33 0.054(5) 0.100(7) 0.072(6) 0.047(5) 0.040(4) 0.050(5) C34 0.027(4) 0.031(3) 0.027(3) 0.015(2) -0.001(3) 0.010(3) C35 0.028(4) 0.136(8) 0.047(5) 0.053(5) 0.008(4) 0.020(5) C36 0.027(4) 0.133(8) 0.042(4) 0.057(5) 0.016(3) 0.019(4) Cl3 0.0355(16) 0.0435(15) 0.094(2) 0.000 -0.0057(15) 0.000 O1 0.056(4) 0.060(4) 0.257(10) -0.023(5) -0.058(5) 0.018(3) O2 0.068(4) 0.098(5) 0.047(3) -0.009(3) 0.023(3) -0.004(3) Cl4 0.125(3) 0.059(2) 0.075(2) 0.000 -0.009(2) 0.000 O3 0.142(7) 0.137(7) 0.156(8) 0.094(6) 0.011(6) 0.018(6) O4 0.210(9) 0.114(6) 0.092(6) 0.019(5) 0.000(6) 0.076(6) _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 N7 2.271(5) . ? Cd1 N3 2.304(5) . ? Cd1 N1 2.308(5) . ? Cd1 N5 2.331(5) . ? Cd1 Cl2 2.6743(7) . ? Cd1 Cl1 2.6843(8) . ? N1 C1 1.300(7) . ? N1 C2 1.376(8) . ? N2 C1 1.358(8) . ? N2 C3 1.376(8) . ? N2 C4 1.434(7) . ? N3 C10 1.303(7) . ? N3 C11 1.346(9) . ? N4 C10 1.324(8) . ? N4 C12 1.384(10) . ? N4 C13 1.450(9) . ? N5 C19 1.313(7) . ? N5 C20 1.389(8) . ? N6 C19 1.338(8) . ? N6 C21 1.360(9) . ? N6 C22 1.427(8) . ? N7 C28 1.308(7) . ? N7 C29 1.379(7) . ? N8 C28 1.348(7) . ? N8 C30 1.358(7) . ? N8 C31 1.432(7) . ? Cl1 Cd1 2.6843(8) 2_756 ? Cl2 Cd1 2.6743(7) 2_656 ? C1 H1 0.9300 . ? C2 C3 1.355(9) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.342(9) . ? C4 C9 1.346(10) . ? C5 C6 1.405(9) . ? C5 H5 0.9300 . ? C6 C7 1.348(9) . ? C6 H6 0.9300 . ? C7 C8 1.341(10) . ? C7 C7 1.497(11) 2_755 ? C8 C9 1.413(10) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.346(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.284(11) . ? C13 C14 1.319(11) . ? C14 C15 1.393(10) . ? C14 H14 0.9300 . ? C15 C16 1.333(10) . ? C15 H15 0.9300 . ? C16 C17 1.326(11) . ? C16 C16 1.499(14) 3_666 ? C17 C18 1.407(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.359(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.337(11) . ? C22 C23 1.382(11) . ? C23 C24 1.393(11) . ? C23 H23 0.9300 . ? C24 C25 1.381(12) . ? C24 H24 0.9300 . ? C25 C26 1.381(12) . ? C25 C25 1.446(15) 2_657 ? C26 C27 1.407(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.349(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.349(9) . ? C31 C36 1.353(8) . ? C32 C33 1.364(9) . ? C32 H32 0.9300 . ? C33 C34 1.363(9) . ? C33 H33 0.9300 . ? C34 C35 1.368(8) . ? C34 C34 1.493(10) 3_857 ? C35 C36 1.384(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? Cl3 O1 1.406(6) 2_656 ? Cl3 O1 1.406(6) . ? Cl3 O2 1.440(6) 2_656 ? Cl3 O2 1.440(6) . ? Cl4 O3 1.422(7) 2 ? Cl4 O3 1.422(7) . ? Cl4 O4 1.436(8) 2 ? Cl4 O4 1.436(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Cd1 N3 176.77(19) . . ? N7 Cd1 N1 88.49(18) . . ? N3 Cd1 N1 94.6(2) . . ? N7 Cd1 N5 87.65(17) . . ? N3 Cd1 N5 89.23(19) . . ? N1 Cd1 N5 176.15(17) . . ? N7 Cd1 Cl2 89.11(13) . . ? N3 Cd1 Cl2 90.11(14) . . ? N1 Cd1 Cl2 88.53(13) . . ? N5 Cd1 Cl2 91.45(13) . . ? N7 Cd1 Cl1 91.46(13) . . ? N3 Cd1 Cl1 89.21(14) . . ? N1 Cd1 Cl1 93.62(13) . . ? N5 Cd1 Cl1 86.44(13) . . ? Cl2 Cd1 Cl1 177.79(4) . . ? C1 N1 C2 104.6(5) . . ? C1 N1 Cd1 127.4(4) . . ? C2 N1 Cd1 127.7(4) . . ? C1 N2 C3 105.9(5) . . ? C1 N2 C4 126.2(5) . . ? C3 N2 C4 127.9(5) . . ? C10 N3 C11 105.8(6) . . ? C10 N3 Cd1 124.7(4) . . ? C11 N3 Cd1 129.4(5) . . ? C10 N4 C12 104.8(6) . . ? C10 N4 C13 127.7(6) . . ? C12 N4 C13 127.4(6) . . ? C19 N5 C20 106.5(5) . . ? C19 N5 Cd1 123.7(4) . . ? C20 N5 Cd1 129.8(4) . . ? C19 N6 C21 107.8(5) . . ? C19 N6 C22 126.7(6) . . ? C21 N6 C22 125.5(6) . . ? C28 N7 C29 104.7(5) . . ? C28 N7 Cd1 125.2(4) . . ? C29 N7 Cd1 130.0(4) . . ? C28 N8 C30 108.3(5) . . ? C28 N8 C31 125.2(5) . . ? C30 N8 C31 126.6(5) . . ? Cd1 Cl1 Cd1 159.04(9) 2_756 . ? Cd1 Cl2 Cd1 161.65(9) . 2_656 ? N1 C1 N2 113.0(6) . . ? N1 C1 H1 123.5 . . ? N2 C1 H1 123.5 . . ? C3 C2 N1 110.7(6) . . ? C3 C2 H2 124.7 . . ? N1 C2 H2 124.7 . . ? C2 C3 N2 105.8(6) . . ? C2 C3 H3 127.1 . . ? N2 C3 H3 127.1 . . ? C5 C4 C9 120.0(6) . . ? C5 C4 N2 120.2(6) . . ? C9 C4 N2 119.6(6) . . ? C4 C5 C6 119.2(7) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 122.5(7) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C8 C7 C6 116.6(6) . . ? C8 C7 C7 120.3(5) . 2_755 ? C6 C7 C7 123.0(4) . 2_755 ? C7 C8 C9 122.3(7) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C4 C9 C8 119.0(7) . . ? C4 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N3 C10 N4 113.1(6) . . ? N3 C10 H10 123.4 . . ? N4 C10 H10 123.4 . . ? C12 C11 N3 109.3(8) . . ? C12 C11 H11 125.4 . . ? N3 C11 H11 125.4 . . ? C11 C12 N4 106.9(7) . . ? C11 C12 H12 126.6 . . ? N4 C12 H12 126.6 . . ? C18 C13 C14 121.2(7) . . ? C18 C13 N4 119.3(7) . . ? C14 C13 N4 118.9(7) . . ? C13 C14 C15 119.3(8) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 121.7(8) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C17 C16 C15 115.8(7) . . ? C17 C16 C16 121.6(9) . 3_666 ? C15 C16 C16 122.4(10) . 3_666 ? C16 C17 C18 123.1(8) . . ? C16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C13 C18 C17 118.3(8) . . ? C13 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? N5 C19 N6 110.8(6) . . ? N5 C19 H19 124.6 . . ? N6 C19 H19 124.6 . . ? C21 C20 N5 107.9(6) . . ? C21 C20 H20 126.0 . . ? N5 C20 H20 126.0 . . ? C20 C21 N6 106.9(6) . . ? C20 C21 H21 126.6 . . ? N6 C21 H21 126.6 . . ? C27 C22 C23 118.9(7) . . ? C27 C22 N6 120.1(7) . . ? C23 C22 N6 120.6(7) . . ? C22 C23 C24 120.7(8) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 121.4(9) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C24 115.9(8) . . ? C26 C25 C25 121.2(9) . 2_657 ? C24 C25 C25 122.6(11) . 2_657 ? C25 C26 C27 122.6(8) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C22 C27 C26 120.0(8) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? N7 C28 N8 111.2(5) . . ? N7 C28 H28 124.4 . . ? N8 C28 H28 124.4 . . ? C30 C29 N7 111.0(5) . . ? C30 C29 H29 124.5 . . ? N7 C29 H29 124.5 . . ? C29 C30 N8 104.9(5) . . ? C29 C30 H30 127.5 . . ? N8 C30 H30 127.5 . . ? C32 C31 C36 118.8(6) . . ? C32 C31 N8 120.6(5) . . ? C36 C31 N8 120.6(5) . . ? C31 C32 C33 120.8(7) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 122.5(7) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 115.8(6) . . ? C33 C34 C34 123.3(7) . 3_857 ? C35 C34 C34 120.9(7) . 3_857 ? C34 C35 C36 122.2(6) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C31 C36 C35 119.8(6) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? O1 Cl3 O1 110.0(5) 2_656 . ? O1 Cl3 O2 110.1(4) 2_656 2_656 ? O1 Cl3 O2 109.7(4) . 2_656 ? O1 Cl3 O2 109.7(4) 2_656 . ? O1 Cl3 O2 110.1(4) . . ? O2 Cl3 O2 107.0(5) 2_656 . ? O3 Cl4 O3 110.2(9) 2 . ? O3 Cl4 O4 106.0(5) 2 2 ? O3 Cl4 O4 111.4(5) . 2 ? O3 Cl4 O4 111.4(5) 2 . ? O3 Cl4 O4 106.0(5) . . ? O4 Cl4 O4 112.0(8) 2 . ? 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 N7 Cd1 N1 C1 -113.1(5) . . . . ? N3 Cd1 N1 C1 67.7(6) . . . . ? N5 Cd1 N1 C1 -113(3) . . . . ? Cl2 Cd1 N1 C1 157.7(5) . . . . ? Cl1 Cd1 N1 C1 -21.8(5) . . . . ? N7 Cd1 N1 C2 59.0(6) . . . . ? N3 Cd1 N1 C2 -120.2(6) . . . . ? N5 Cd1 N1 C2 60(3) . . . . ? Cl2 Cd1 N1 C2 -30.2(6) . . . . ? Cl1 Cd1 N1 C2 150.3(6) . . . . ? N7 Cd1 N3 C10 -101(3) . . . . ? N1 Cd1 N3 C10 63.4(6) . . . . ? N5 Cd1 N3 C10 -116.6(6) . . . . ? Cl2 Cd1 N3 C10 -25.2(5) . . . . ? Cl1 Cd1 N3 C10 156.9(5) . . . . ? N7 Cd1 N3 C11 76(3) . . . . ? N1 Cd1 N3 C11 -119.2(9) . . . . ? N5 Cd1 N3 C11 60.9(9) . . . . ? Cl2 Cd1 N3 C11 152.3(9) . . . . ? Cl1 Cd1 N3 C11 -25.6(9) . . . . ? N7 Cd1 N5 C19 -67.1(5) . . . . ? N3 Cd1 N5 C19 112.0(5) . . . . ? N1 Cd1 N5 C19 -68(3) . . . . ? Cl2 Cd1 N5 C19 21.9(5) . . . . ? Cl1 Cd1 N5 C19 -158.7(5) . . . . ? N7 Cd1 N5 C20 114.5(6) . . . . ? N3 Cd1 N5 C20 -66.3(6) . . . . ? N1 Cd1 N5 C20 114(3) . . . . ? Cl2 Cd1 N5 C20 -156.4(5) . . . . ? Cl1 Cd1 N5 C20 22.9(5) . . . . ? N3 Cd1 N7 C28 -86(3) . . . . ? N1 Cd1 N7 C28 109.3(5) . . . . ? N5 Cd1 N7 C28 -70.7(5) . . . . ? Cl2 Cd1 N7 C28 -162.2(5) . . . . ? Cl1 Cd1 N7 C28 15.7(5) . . . . ? N3 Cd1 N7 C29 90(3) . . . . ? N1 Cd1 N7 C29 -74.9(5) . . . . ? N5 Cd1 N7 C29 105.2(5) . . . . ? Cl2 Cd1 N7 C29 13.7(5) . . . . ? Cl1 Cd1 N7 C29 -168.4(5) . . . . ? N7 Cd1 Cl1 Cd1 21.10(12) . . . 2_756 ? N3 Cd1 Cl1 Cd1 -162.06(15) . . . 2_756 ? N1 Cd1 Cl1 Cd1 -67.48(13) . . . 2_756 ? N5 Cd1 Cl1 Cd1 108.66(12) . . . 2_756 ? Cl2 Cd1 Cl1 Cd1 126.0(14) . . . 2_756 ? N7 Cd1 Cl2 Cd1 158.63(12) . . . 2_656 ? N3 Cd1 Cl2 Cd1 -18.23(15) . . . 2_656 ? N1 Cd1 Cl2 Cd1 -112.85(13) . . . 2_656 ? N5 Cd1 Cl2 Cd1 71.00(12) . . . 2_656 ? Cl1 Cd1 Cl2 Cd1 53.7(14) . . . 2_656 ? C2 N1 C1 N2 -1.4(8) . . . . ? Cd1 N1 C1 N2 172.1(4) . . . . ? C3 N2 C1 N1 2.2(8) . . . . ? C4 N2 C1 N1 -178.9(6) . . . . ? C1 N1 C2 C3 0.1(8) . . . . ? Cd1 N1 C2 C3 -173.4(5) . . . . ? N1 C2 C3 N2 1.2(9) . . . . ? C1 N2 C3 C2 -2.0(8) . . . . ? C4 N2 C3 C2 179.1(6) . . . . ? C1 N2 C4 C5 149.5(8) . . . . ? C3 N2 C4 C5 -31.8(11) . . . . ? C1 N2 C4 C9 -34.5(11) . . . . ? C3 N2 C4 C9 144.2(8) . . . . ? C9 C4 C5 C6 2.9(13) . . . . ? N2 C4 C5 C6 178.8(7) . . . . ? C4 C5 C6 C7 -1.8(15) . . . . ? C5 C6 C7 C8 3.1(14) . . . . ? C5 C6 C7 C7 179.1(9) . . . 2_755 ? C6 C7 C8 C9 -5.5(16) . . . . ? C7 C7 C8 C9 178.3(10) 2_755 . . . ? C5 C4 C9 C8 -5.2(15) . . . . ? N2 C4 C9 C8 178.8(9) . . . . ? C7 C8 C9 C4 6.7(18) . . . . ? C11 N3 C10 N4 -2.5(10) . . . . ? Cd1 N3 C10 N4 175.5(4) . . . . ? C12 N4 C10 N3 1.7(10) . . . . ? C13 N4 C10 N3 178.3(8) . . . . ? C10 N3 C11 C12 2.2(14) . . . . ? Cd1 N3 C11 C12 -175.7(8) . . . . ? N3 C11 C12 N4 -1.2(16) . . . . ? C10 N4 C12 C11 -0.3(13) . . . . ? C13 N4 C12 C11 -176.9(10) . . . . ? C10 N4 C13 C18 147.7(10) . . . . ? C12 N4 C13 C18 -36.4(16) . . . . ? C10 N4 C13 C14 -40.8(14) . . . . ? C12 N4 C13 C14 135.0(12) . . . . ? C18 C13 C14 C15 -8.8(18) . . . . ? N4 C13 C14 C15 180.0(9) . . . . ? C13 C14 C15 C16 2.6(18) . . . . ? C14 C15 C16 C17 3.9(18) . . . . ? C14 C15 C16 C16 178.4(12) . . . 3_666 ? C15 C16 C17 C18 -5(2) . . . . ? C16 C16 C17 C18 -179.3(13) 3_666 . . . ? C14 C13 C18 C17 7.9(19) . . . . ? N4 C13 C18 C17 179.2(10) . . . . ? C16 C17 C18 C13 -1(2) . . . . ? C20 N5 C19 N6 -0.6(8) . . . . ? Cd1 N5 C19 N6 -179.2(4) . . . . ? C21 N6 C19 N5 -1.0(9) . . . . ? C22 N6 C19 N5 178.2(7) . . . . ? C19 N5 C20 C21 1.9(8) . . . . ? Cd1 N5 C20 C21 -179.5(5) . . . . ? N5 C20 C21 N6 -2.5(9) . . . . ? C19 N6 C21 C20 2.1(9) . . . . ? C22 N6 C21 C20 -177.1(7) . . . . ? C19 N6 C22 C27 169.0(10) . . . . ? C21 N6 C22 C27 -11.9(14) . . . . ? C19 N6 C22 C23 -18.4(13) . . . . ? C21 N6 C22 C23 160.7(10) . . . . ? C27 C22 C23 C24 -7.3(18) . . . . ? N6 C22 C23 C24 -179.9(10) . . . . ? C22 C23 C24 C25 2.2(19) . . . . ? C23 C24 C25 C26 3.3(18) . . . . ? C23 C24 C25 C25 177.2(9) . . . 2_657 ? C24 C25 C26 C27 -4.1(19) . . . . ? C25 C25 C26 C27 -178.1(10) 2_657 . . . ? C23 C22 C27 C26 6.5(18) . . . . ? N6 C22 C27 C26 179.2(10) . . . . ? C25 C26 C27 C22 -1(2) . . . . ? C29 N7 C28 N8 -0.5(7) . . . . ? Cd1 N7 C28 N8 176.2(4) . . . . ? C30 N8 C28 N7 0.1(7) . . . . ? C31 N8 C28 N7 179.6(5) . . . . ? C28 N7 C29 C30 0.7(7) . . . . ? Cd1 N7 C29 C30 -175.8(5) . . . . ? N7 C29 C30 N8 -0.7(8) . . . . ? C28 N8 C30 C29 0.3(7) . . . . ? C31 N8 C30 C29 -179.1(6) . . . . ? C28 N8 C31 C32 130.8(8) . . . . ? C30 N8 C31 C32 -49.8(10) . . . . ? C28 N8 C31 C36 -48.3(9) . . . . ? C30 N8 C31 C36 131.0(8) . . . . ? C36 C31 C32 C33 -2.0(14) . . . . ? N8 C31 C32 C33 178.9(8) . . . . ? C31 C32 C33 C34 3.2(15) . . . . ? C32 C33 C34 C35 -3.4(13) . . . . ? C32 C33 C34 C34 179.3(9) . . . 3_857 ? C33 C34 C35 C36 2.6(13) . . . . ? C34 C34 C35 C36 -179.9(9) 3_857 . . . ? C32 C31 C36 C35 1.3(13) . . . . ? N8 C31 C36 C35 -179.6(7) . . . . ? C34 C35 C36 C31 -1.7(14) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.534 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.096