# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zhai, Quan-Guo' _publ_contact_author_email zhaiqg@snnu.edu.cn _publ_section_title ; Solvothermal Synthesis, Crystal Structures and Photoluminescence Properties of the Novel Cd/X/a,o-Bis(benzotriazole)alkane Hybrid Family (X = Cl, Br and I) ; loop_ _publ_author_name 'Quan-Guo Zhai' 'Xia Gao' 'Shuni Li' 'Yucheng Jiang' 'Mancheng Hu' data_01 _database_code_depnum_ccdc_archive 'CCDC 787187' #=================================END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Cd2 I4 N12' _chemical_formula_sum 'C28 H24 Cd2 I4 N12' _chemical_formula_weight 1260.99 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' I I -0.4742 1.8119 '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 C2/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 14.4305(15) _cell_length_b 9.9821(9) _cell_length_c 25.489(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.9170(10) _cell_angle_gamma 90.00 _cell_volume 3671.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3675 _cell_measurement_theta_min 2.398 _cell_measurement_theta_max 25.551 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 4.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2832 _exptl_absorpt_correction_T_max 0.3616 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8897 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3208 _reflns_number_gt 2426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0326P)^2^+320.7378P] 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 3208 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2025 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _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 1.01307(9) 0.19687(14) 0.37523(5) 0.0409(4) Uani 1 1 d . . . I1 I 1.18913(9) 0.28518(15) 0.37871(6) 0.0576(4) Uani 1 1 d . . . I2 I 0.88258(10) 0.32023(16) 0.31597(6) 0.0610(5) Uani 1 1 d . . . N1 N 0.9338(11) 0.3021(16) 0.5305(6) 0.044(4) Uani 1 1 d . . . N2 N 0.9851(11) 0.2998(17) 0.4881(6) 0.048(4) Uani 1 1 d . . . N3 N 0.9580(11) 0.1995(16) 0.4587(6) 0.045(4) Uani 1 1 d . . . N4 N 1.0205(10) -0.0213(15) 0.3527(6) 0.039(3) Uani 1 1 d . . . N5 N 0.9792(10) -0.1124(15) 0.3812(6) 0.041(4) Uani 1 1 d . . . N6 N 1.0022(10) -0.2327(14) 0.3623(6) 0.038(3) Uani 1 1 d . . . C1 C 0.8862(13) 0.1331(19) 0.4843(7) 0.041(4) Uani 1 1 d . . . C2 C 0.8700(12) 0.2059(19) 0.5308(7) 0.041(4) Uani 1 1 d . . . C3 C 0.8004(13) 0.1655(19) 0.5660(7) 0.043(4) Uani 1 1 d . . . H3 H 0.7896 0.2116 0.5970 0.051 Uiso 1 1 calc R . . C4 C 0.7498(13) 0.055(2) 0.5517(8) 0.048(5) Uani 1 1 d . . . H4 H 0.7046 0.0238 0.5743 0.058 Uiso 1 1 calc R . . C5 C 0.7633(14) -0.014(2) 0.5041(8) 0.048(5) Uani 1 1 d . . . H5 H 0.7258 -0.0873 0.4959 0.057 Uiso 1 1 calc R . . C6 C 0.8306(13) 0.0239(19) 0.4693(7) 0.045(5) Uani 1 1 d . . . H6 H 0.8387 -0.0204 0.4377 0.055 Uiso 1 1 calc R . . C7 C 1.0591(12) -0.2226(18) 0.3207(7) 0.038(4) Uani 1 1 d . . . C8 C 1.0685(13) -0.0827(18) 0.3135(7) 0.039(4) Uani 1 1 d . . . C9 C 1.1196(13) -0.030(2) 0.2733(7) 0.045(5) Uani 1 1 d . . . H9 H 1.1259 0.0615 0.2678 0.053 Uiso 1 1 calc R . . C10 C 1.1611(14) -0.125(2) 0.2415(8) 0.052(5) Uani 1 1 d . . . H10 H 1.1980 -0.0950 0.2143 0.062 Uiso 1 1 calc R . . C11 C 1.1507(14) -0.258(2) 0.2480(8) 0.050(5) Uani 1 1 d . . . H11 H 1.1799 -0.3154 0.2246 0.060 Uiso 1 1 calc R . . C12 C 1.0996(13) -0.313(2) 0.2868(7) 0.045(4) Uani 1 1 d . . . H12 H 1.0924 -0.4054 0.2905 0.054 Uiso 1 1 calc R . . C13 C 0.9534(13) 0.3984(18) 0.5723(7) 0.044(5) Uani 1 1 d . . . H13A H 0.8968 0.4155 0.5912 0.053 Uiso 1 1 calc R . . H13B H 0.9730 0.4822 0.5568 0.053 Uiso 1 1 calc R . . C14 C 1.0260(14) 0.3525(18) 0.6101(8) 0.047(5) Uani 1 1 d . . . H14A H 1.0826 0.3344 0.5914 0.057 Uiso 1 1 calc R . . H14B H 1.0388 0.4232 0.6353 0.057 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 0.0435(8) 0.0325(7) 0.0469(8) -0.0050(6) 0.0063(6) -0.0044(6) I1 0.0417(7) 0.0598(9) 0.0716(9) -0.0125(7) 0.0091(6) -0.0138(7) I2 0.0573(9) 0.0547(9) 0.0706(9) -0.0104(7) -0.0154(7) 0.0094(7) N1 0.050(9) 0.037(8) 0.045(9) 0.001(7) 0.007(7) 0.005(8) N2 0.052(10) 0.042(9) 0.049(9) 0.005(8) 0.009(8) -0.004(8) N3 0.048(9) 0.038(9) 0.048(9) 0.001(7) 0.008(7) -0.004(8) N4 0.036(8) 0.036(8) 0.045(9) -0.005(7) -0.005(7) -0.002(7) N5 0.039(9) 0.038(9) 0.046(9) -0.003(7) 0.000(7) -0.001(7) N6 0.039(8) 0.029(8) 0.044(9) -0.007(6) 0.000(7) -0.001(6) C1 0.040(10) 0.040(10) 0.043(10) 0.000(8) 0.006(8) -0.001(8) C2 0.042(10) 0.037(10) 0.045(10) 0.001(8) 0.005(8) 0.000(9) C3 0.043(11) 0.041(11) 0.045(10) 0.001(8) 0.009(8) -0.002(9) C4 0.042(11) 0.052(12) 0.050(12) 0.007(10) 0.007(9) -0.008(10) C5 0.045(12) 0.042(11) 0.057(12) 0.002(9) 0.002(9) -0.005(9) C6 0.046(11) 0.042(11) 0.048(11) 0.001(9) 0.005(9) -0.002(9) C7 0.037(9) 0.037(10) 0.040(10) -0.005(8) -0.005(8) -0.001(8) C8 0.040(10) 0.037(10) 0.041(10) -0.004(8) -0.002(8) 0.001(8) C9 0.039(11) 0.047(11) 0.047(11) -0.002(9) -0.003(9) -0.002(9) C10 0.041(11) 0.063(14) 0.051(12) 0.003(10) 0.004(9) 0.005(10) C11 0.043(11) 0.060(14) 0.047(12) -0.009(10) -0.003(9) 0.009(10) C12 0.042(11) 0.044(11) 0.050(11) -0.004(9) -0.003(9) 0.005(9) C13 0.050(11) 0.031(10) 0.053(11) -0.003(8) 0.013(9) 0.005(8) C14 0.057(12) 0.028(9) 0.057(12) -0.002(8) 0.006(10) -0.005(9) _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 N4 2.255(15) . ? Cd1 N3 2.282(15) . ? Cd1 I1 2.6893(19) . ? Cd1 I2 2.693(2) . ? N1 N2 1.32(2) . ? N1 C2 1.33(2) . ? N1 C13 1.46(2) . ? N2 N3 1.31(2) . ? N3 C1 1.40(2) . ? N4 N5 1.31(2) . ? N4 C8 1.37(2) . ? N5 N6 1.34(2) . ? N6 C7 1.36(2) . ? N6 C14 1.45(2) 5_756 ? C1 C6 1.40(3) . ? C1 C2 1.41(2) . ? C2 C3 1.42(2) . ? C3 C4 1.37(3) . ? C3 H3 0.9300 . ? C4 C5 1.41(3) . ? C4 H4 0.9300 . ? C5 C6 1.38(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.39(2) . ? C7 C8 1.42(3) . ? C8 C9 1.38(3) . ? C9 C10 1.39(3) . ? C9 H9 0.9300 . ? C10 C11 1.35(3) . ? C10 H10 0.9300 . ? C11 C12 1.36(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.48(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N6 1.45(2) 5_756 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 N4 Cd1 N3 105.5(6) . . ? N4 Cd1 I1 106.0(4) . . ? N3 Cd1 I1 108.0(4) . . ? N4 Cd1 I2 109.6(4) . . ? N3 Cd1 I2 105.5(4) . . ? I1 Cd1 I2 121.36(7) . . ? N2 N1 C2 113.0(16) . . ? N2 N1 C13 120.3(16) . . ? C2 N1 C13 126.6(15) . . ? N3 N2 N1 108.4(15) . . ? N2 N3 C1 108.2(14) . . ? N2 N3 Cd1 116.0(11) . . ? C1 N3 Cd1 134.4(13) . . ? N5 N4 C8 109.5(15) . . ? N5 N4 Cd1 120.3(11) . . ? C8 N4 Cd1 130.1(12) . . ? N4 N5 N6 107.7(14) . . ? N5 N6 C7 111.9(14) . . ? N5 N6 C14 119.5(14) . 5_756 ? C7 N6 C14 128.3(15) . 5_756 ? N3 C1 C6 131.8(17) . . ? N3 C1 C2 106.4(16) . . ? C6 C1 C2 121.7(17) . . ? N1 C2 C1 104.0(15) . . ? N1 C2 C3 135.0(18) . . ? C1 C2 C3 121.0(18) . . ? C4 C3 C2 116.2(17) . . ? C4 C3 H3 121.9 . . ? C2 C3 H3 121.9 . . ? C3 C4 C5 122.8(18) . . ? C3 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C6 C5 C4 121.8(19) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 116.5(18) . . ? C5 C6 H6 121.7 . . ? C1 C6 H6 121.7 . . ? N6 C7 C12 134.8(17) . . ? N6 C7 C8 103.6(15) . . ? C12 C7 C8 121.4(17) . . ? N4 C8 C9 131.1(18) . . ? N4 C8 C7 107.2(16) . . ? C9 C8 C7 121.7(17) . . ? C8 C9 C10 114.6(19) . . ? C8 C9 H9 122.7 . . ? C10 C9 H9 122.7 . . ? C11 C10 C9 123(2) . . ? C11 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C10 C11 C12 123(2) . . ? C10 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C7 115.4(19) . . ? C11 C12 H12 122.3 . . ? C7 C12 H12 122.3 . . ? N1 C13 C14 113.4(15) . . ? N1 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N1 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N6 C14 C13 111.7(16) 5_756 . ? N6 C14 H14A 109.3 5_756 . ? C13 C14 H14A 109.3 . . ? N6 C14 H14B 109.3 5_756 . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? 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 C2 N1 N2 N3 -1(2) . . . . ? C13 N1 N2 N3 175.5(15) . . . . ? N1 N2 N3 C1 -1(2) . . . . ? N1 N2 N3 Cd1 167.5(11) . . . . ? N4 Cd1 N3 N2 150.4(13) . . . . ? I1 Cd1 N3 N2 37.4(14) . . . . ? I2 Cd1 N3 N2 -93.7(13) . . . . ? N4 Cd1 N3 C1 -44.9(18) . . . . ? I1 Cd1 N3 C1 -157.9(16) . . . . ? I2 Cd1 N3 C1 71.0(18) . . . . ? N3 Cd1 N4 N5 13.3(14) . . . . ? I1 Cd1 N4 N5 127.7(12) . . . . ? I2 Cd1 N4 N5 -99.8(12) . . . . ? N3 Cd1 N4 C8 -162.0(15) . . . . ? I1 Cd1 N4 C8 -47.7(15) . . . . ? I2 Cd1 N4 C8 84.9(15) . . . . ? C8 N4 N5 N6 2.2(19) . . . . ? Cd1 N4 N5 N6 -174.0(10) . . . . ? N4 N5 N6 C7 0(2) . . . . ? N4 N5 N6 C14 173.4(15) . . . 5_756 ? N2 N3 C1 C6 177(2) . . . . ? Cd1 N3 C1 C6 12(3) . . . . ? N2 N3 C1 C2 2(2) . . . . ? Cd1 N3 C1 C2 -163.1(13) . . . . ? N2 N1 C2 C1 2(2) . . . . ? C13 N1 C2 C1 -173.8(17) . . . . ? N2 N1 C2 C3 180(2) . . . . ? C13 N1 C2 C3 3(3) . . . . ? N3 C1 C2 N1 -3(2) . . . . ? C6 C1 C2 N1 -178.1(18) . . . . ? N3 C1 C2 C3 179.5(17) . . . . ? C6 C1 C2 C3 4(3) . . . . ? N1 C2 C3 C4 -178(2) . . . . ? C1 C2 C3 C4 -1(3) . . . . ? C2 C3 C4 C5 -2(3) . . . . ? C3 C4 C5 C6 2(3) . . . . ? C4 C5 C6 C1 1(3) . . . . ? N3 C1 C6 C5 -178(2) . . . . ? C2 C1 C6 C5 -4(3) . . . . ? N5 N6 C7 C12 -177.7(19) . . . . ? C14 N6 C7 C12 9(3) 5_756 . . . ? N5 N6 C7 C8 -2(2) . . . . ? C14 N6 C7 C8 -174.7(17) 5_756 . . . ? N5 N4 C8 C9 177.8(19) . . . . ? Cd1 N4 C8 C9 -7(3) . . . . ? N5 N4 C8 C7 -3(2) . . . . ? Cd1 N4 C8 C7 172.4(12) . . . . ? N6 C7 C8 N4 3.0(19) . . . . ? C12 C7 C8 N4 179.6(16) . . . . ? N6 C7 C8 C9 -177.9(16) . . . . ? C12 C7 C8 C9 -1(3) . . . . ? N4 C8 C9 C10 178.1(18) . . . . ? C7 C8 C9 C10 -1(3) . . . . ? C8 C9 C10 C11 2(3) . . . . ? C9 C10 C11 C12 -1(3) . . . . ? C10 C11 C12 C7 -1(3) . . . . ? N6 C7 C12 C11 177.4(19) . . . . ? C8 C7 C12 C11 2(3) . . . . ? N2 N1 C13 C14 -85(2) . . . . ? C2 N1 C13 C14 91(2) . . . . ? N1 C13 C14 N6 -63(2) . . . 5_756 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.022 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.249 # Attachment '02.cif' data_02 _database_code_depnum_ccdc_archive 'CCDC 787188' #TrackingRef '02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Br6 Cd3 N12' _chemical_formula_sum 'C28 H24 Br6 Cd3 N12' _chemical_formula_weight 1345.25 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' Br Br -0.2901 2.4595 '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 C2/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 18.1301(19) _cell_length_b 8.2353(7) _cell_length_c 24.658(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.996(2) _cell_angle_gamma 90.00 _cell_volume 3601.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3399 _cell_measurement_theta_min 2.297 _cell_measurement_theta_max 27.806 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 8.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1792 _exptl_absorpt_correction_T_max 0.3114 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8535 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3142 _reflns_number_gt 2395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0531P)^2^+0.0000P] 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 3142 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.01026(2) 1.00293(5) 0.419096(19) 0.03437(16) Uani 1 1 d . . . Cd2 Cd 0.0000 0.99803(8) 0.2500 0.0393(2) Uani 1 2 d S . . Br1 Br -0.01986(4) 1.21306(8) 0.32443(3) 0.0421(2) Uani 1 1 d . . . Br2 Br -0.03680(4) 0.76110(9) 0.35843(3) 0.0557(2) Uani 1 1 d . . . Br3 Br -0.05685(4) 1.18637(8) 0.47844(3) 0.0451(2) Uani 1 1 d . . . N1 N 0.2443(2) 1.0794(5) 0.42204(19) 0.0259(11) Uani 1 1 d . . . N2 N 0.1821(3) 0.9910(5) 0.4205(2) 0.0277(11) Uani 1 1 d . . . N3 N 0.1290(2) 1.0896(6) 0.42716(19) 0.0274(11) Uani 1 1 d . . . N4 N 0.2329(2) 0.9180(5) 0.31657(19) 0.0236(10) Uani 1 1 d . . . N5 N 0.1679(3) 0.9975(5) 0.3018(2) 0.0284(11) Uani 1 1 d . . . N6 N 0.1140(2) 0.8904(6) 0.28515(18) 0.0267(11) Uani 1 1 d . . . C1 C 0.1566(3) 1.2467(7) 0.4332(2) 0.0235(12) Uani 1 1 d . . . C2 C 0.2310(3) 1.2401(6) 0.4301(2) 0.0238(12) Uani 1 1 d . . . C3 C 0.2775(3) 1.3757(7) 0.4370(2) 0.0319(14) Uani 1 1 d . . . H3 H 0.3286 1.3687 0.4365 0.038 Uiso 1 1 calc R . . C4 C 0.2435(4) 1.5210(7) 0.4444(2) 0.0370(16) Uani 1 1 d . . . H4 H 0.2722 1.6156 0.4488 0.044 Uiso 1 1 calc R . . C5 C 0.1657(4) 1.5299(8) 0.4455(3) 0.0432(18) Uani 1 1 d . . . H5 H 0.1443 1.6304 0.4498 0.052 Uiso 1 1 calc R . . C6 C 0.1219(4) 1.3947(7) 0.4406(3) 0.0389(16) Uani 1 1 d . . . H6 H 0.0710 1.4002 0.4420 0.047 Uiso 1 1 calc R . . C7 C 0.1452(3) 0.7375(6) 0.2907(2) 0.0240(13) Uani 1 1 d . . . C8 C 0.2223(3) 0.7553(6) 0.3099(2) 0.0223(12) Uani 1 1 d . . . C9 C 0.2715(3) 0.6241(7) 0.3171(2) 0.0281(13) Uani 1 1 d . . . H9 H 0.3232 0.6384 0.3289 0.034 Uiso 1 1 calc R . . C10 C 0.2411(4) 0.4750(7) 0.3063(2) 0.0343(15) Uani 1 1 d . . . H10 H 0.2724 0.3845 0.3103 0.041 Uiso 1 1 calc R . . C11 C 0.1621(4) 0.4547(8) 0.2888(3) 0.0418(17) Uani 1 1 d . . . H11 H 0.1427 0.3501 0.2833 0.050 Uiso 1 1 calc R . . C12 C 0.1135(4) 0.5821(7) 0.2799(3) 0.0368(15) Uani 1 1 d . . . H12 H 0.0620 0.5673 0.2673 0.044 Uiso 1 1 calc R . . C13 C 0.3091(3) 1.0039(7) 0.4065(3) 0.0303(14) Uani 1 1 d . . . H13A H 0.3142 0.8934 0.4203 0.036 Uiso 1 1 calc R . . H13B H 0.3544 1.0630 0.4233 0.036 Uiso 1 1 calc R . . C14 C 0.3003(3) 1.0029(7) 0.3428(2) 0.0299(14) Uani 1 1 d . . . H14A H 0.2982 1.1138 0.3293 0.036 Uiso 1 1 calc R . . H14B H 0.3439 0.9507 0.3332 0.036 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 0.0228(2) 0.0390(3) 0.0429(3) -0.0073(2) 0.0103(2) -0.0055(2) Cd2 0.0228(3) 0.0314(4) 0.0569(5) 0.000 -0.0071(3) 0.000 Br1 0.0393(4) 0.0449(4) 0.0405(4) 0.0039(3) 0.0043(3) 0.0041(3) Br2 0.0555(5) 0.0524(5) 0.0577(5) -0.0195(4) 0.0083(4) -0.0204(4) Br3 0.0473(4) 0.0440(4) 0.0496(5) 0.0083(3) 0.0229(3) 0.0168(3) N1 0.022(2) 0.024(3) 0.032(3) 0.001(2) 0.005(2) -0.002(2) N2 0.025(3) 0.027(3) 0.031(3) 0.001(2) 0.004(2) -0.002(2) N3 0.021(3) 0.033(3) 0.028(3) -0.001(2) 0.005(2) -0.002(2) N4 0.019(2) 0.021(3) 0.029(3) 0.000(2) 0.003(2) 0.002(2) N5 0.026(3) 0.023(3) 0.036(3) 0.001(2) 0.006(2) 0.003(2) N6 0.021(2) 0.028(3) 0.028(3) 0.001(2) -0.002(2) 0.001(2) C1 0.021(3) 0.029(3) 0.019(3) -0.001(2) 0.002(2) -0.001(2) C2 0.028(3) 0.024(3) 0.020(3) 0.005(2) 0.006(2) -0.002(2) C3 0.034(3) 0.037(4) 0.025(3) 0.000(3) 0.007(3) -0.011(3) C4 0.054(4) 0.029(4) 0.030(4) -0.006(3) 0.013(3) -0.017(3) C5 0.059(5) 0.028(4) 0.046(4) -0.002(3) 0.018(4) 0.005(3) C6 0.034(3) 0.037(4) 0.048(4) -0.001(3) 0.014(3) 0.006(3) C7 0.023(3) 0.026(3) 0.022(3) 0.002(2) 0.001(2) 0.001(2) C8 0.030(3) 0.020(3) 0.017(3) 0.006(2) 0.005(2) 0.002(2) C9 0.025(3) 0.032(3) 0.025(3) 0.003(3) 0.000(2) 0.009(3) C10 0.045(4) 0.029(4) 0.027(3) 0.003(3) 0.005(3) 0.012(3) C11 0.063(5) 0.026(4) 0.038(4) -0.005(3) 0.013(3) -0.008(3) C12 0.033(4) 0.032(4) 0.042(4) -0.001(3) 0.001(3) -0.002(3) C13 0.021(3) 0.030(3) 0.038(4) -0.001(3) 0.002(3) -0.001(3) C14 0.026(3) 0.025(3) 0.041(4) -0.001(3) 0.013(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.236(4) . ? Cd1 Br2 2.5301(8) . ? Cd1 Br3 2.5776(8) . ? Cd1 Br1 2.8655(8) . ? Cd1 Br3 2.9393(8) 5_576 ? Cd2 N6 2.251(4) 2 ? Cd2 N6 2.251(4) . ? Cd2 Br1 2.6285(8) . ? Cd2 Br1 2.6285(8) 2 ? Cd2 Br2 3.4845(9) . ? Br3 Cd1 2.9393(8) 5_576 ? N1 N2 1.337(6) . ? N1 C2 1.367(7) . ? N1 C13 1.448(7) . ? N2 N3 1.296(6) . ? N3 C1 1.385(7) . ? N4 N5 1.331(6) . ? N4 C8 1.359(7) . ? N4 C14 1.439(7) . ? N5 N6 1.317(6) . ? N6 C7 1.375(7) . ? C1 C2 1.369(8) . ? C1 C6 1.401(8) . ? C2 C3 1.388(7) . ? C3 C4 1.376(8) . ? C3 H3 0.9300 . ? C4 C5 1.418(10) . ? C4 H4 0.9300 . ? C5 C6 1.359(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.386(8) . ? C7 C12 1.405(8) . ? C8 C9 1.389(7) . ? C9 C10 1.349(8) . ? C9 H9 0.9300 . ? C10 C11 1.417(9) . ? C10 H10 0.9300 . ? C11 C12 1.357(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.546(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 Br2 120.24(12) . . ? N3 Cd1 Br3 108.76(12) . . ? Br2 Cd1 Br3 131.00(3) . . ? N3 Cd1 Br1 84.07(12) . . ? Br2 Cd1 Br1 90.57(3) . . ? Br3 Cd1 Br1 94.36(3) . . ? N3 Cd1 Br3 89.62(12) . 5_576 ? Br2 Cd1 Br3 95.28(3) . 5_576 ? Br3 Cd1 Br3 84.73(2) . 5_576 ? Br1 Cd1 Br3 172.98(3) . 5_576 ? N6 Cd2 N6 133.6(2) 2 . ? N6 Cd2 Br1 106.61(12) 2 . ? N6 Cd2 Br1 104.16(12) . . ? N6 Cd2 Br1 104.16(12) 2 2 ? N6 Cd2 Br1 106.61(12) . 2 ? Br1 Cd2 Br1 95.29(4) . 2 ? N6 Cd2 Br2 76.58(12) 2 . ? N6 Cd2 Br2 77.95(12) . . ? Br1 Cd2 Br2 76.44(2) . . ? Br1 Cd2 Br2 171.45(3) 2 . ? Cd2 Br1 Cd1 97.55(3) . . ? Cd1 Br2 Cd2 85.30(2) . . ? Cd1 Br3 Cd1 95.27(2) . 5_576 ? N2 N1 C2 111.0(4) . . ? N2 N1 C13 119.0(4) . . ? C2 N1 C13 129.1(5) . . ? N3 N2 N1 107.5(4) . . ? N2 N3 C1 109.7(4) . . ? N2 N3 Cd1 121.0(3) . . ? C1 N3 Cd1 128.9(3) . . ? N5 N4 C8 110.8(4) . . ? N5 N4 C14 120.3(4) . . ? C8 N4 C14 128.3(5) . . ? N6 N5 N4 108.3(4) . . ? N5 N6 C7 108.6(4) . . ? N5 N6 Cd2 114.8(3) . . ? C7 N6 Cd2 136.4(4) . . ? C2 C1 N3 107.2(5) . . ? C2 C1 C6 121.1(5) . . ? N3 C1 C6 131.7(5) . . ? N1 C2 C1 104.6(5) . . ? N1 C2 C3 132.5(5) . . ? C1 C2 C3 122.8(5) . . ? C4 C3 C2 116.0(6) . . ? C4 C3 H3 122.0 . . ? C2 C3 H3 122.0 . . ? C3 C4 C5 121.5(6) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 121.5(6) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 117.0(6) . . ? C5 C6 H6 121.5 . . ? C1 C6 H6 121.5 . . ? N6 C7 C8 107.5(5) . . ? N6 C7 C12 132.2(5) . . ? C8 C7 C12 120.2(5) . . ? N4 C8 C7 104.7(5) . . ? N4 C8 C9 132.8(5) . . ? C7 C8 C9 122.5(5) . . ? C10 C9 C8 117.2(5) . . ? C10 C9 H9 121.4 . . ? C8 C9 H9 121.4 . . ? C9 C10 C11 120.9(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 122.6(6) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C7 116.6(6) . . ? C11 C12 H12 121.7 . . ? C7 C12 H12 121.7 . . ? N1 C13 C14 110.7(5) . . ? N1 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N4 C14 C13 110.9(4) . . ? N4 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? 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 N6 Cd2 Br1 Cd1 92.57(12) 2 . . . ? N6 Cd2 Br1 Cd1 -52.30(12) . . . . ? Br1 Cd2 Br1 Cd1 -160.93(3) 2 . . . ? Br2 Cd2 Br1 Cd1 21.30(2) . . . . ? N3 Cd1 Br1 Cd2 91.26(12) . . . . ? Br2 Cd1 Br1 Cd2 -29.10(3) . . . . ? Br3 Cd1 Br1 Cd2 -160.30(2) . . . . ? Br3 Cd1 Br1 Cd2 117.5(2) 5_576 . . . ? N3 Cd1 Br2 Cd2 -62.07(14) . . . . ? Br3 Cd1 Br2 Cd2 117.68(3) . . . . ? Br1 Cd1 Br2 Cd2 21.40(2) . . . . ? Br3 Cd1 Br2 Cd2 -154.723(19) 5_576 . . . ? N6 Cd2 Br2 Cd1 -135.25(12) 2 . . . ? N6 Cd2 Br2 Cd1 83.83(12) . . . . ? Br1 Cd2 Br2 Cd1 -24.15(2) . . . . ? Br1 Cd2 Br2 Cd1 -39.26(14) 2 . . . ? N3 Cd1 Br3 Cd1 -87.80(13) . . . 5_576 ? Br2 Cd1 Br3 Cd1 92.42(4) . . . 5_576 ? Br1 Cd1 Br3 Cd1 -173.02(3) . . . 5_576 ? Br3 Cd1 Br3 Cd1 0.0 5_576 . . 5_576 ? C2 N1 N2 N3 0.2(6) . . . . ? C13 N1 N2 N3 -169.8(5) . . . . ? N1 N2 N3 C1 -0.1(6) . . . . ? N1 N2 N3 Cd1 173.7(3) . . . . ? Br2 Cd1 N3 N2 -27.0(4) . . . . ? Br3 Cd1 N3 N2 153.2(4) . . . . ? Br1 Cd1 N3 N2 -114.2(4) . . . . ? Br3 Cd1 N3 N2 68.9(4) 5_576 . . . ? Br2 Cd1 N3 C1 145.4(4) . . . . ? Br3 Cd1 N3 C1 -34.4(5) . . . . ? Br1 Cd1 N3 C1 58.2(4) . . . . ? Br3 Cd1 N3 C1 -118.7(4) 5_576 . . . ? C8 N4 N5 N6 -0.2(6) . . . . ? C14 N4 N5 N6 -172.5(5) . . . . ? N4 N5 N6 C7 1.5(6) . . . . ? N4 N5 N6 Cd2 -174.2(3) . . . . ? N6 Cd2 N6 N5 -180.0(4) 2 . . . ? Br1 Cd2 N6 N5 -49.6(4) . . . . ? Br1 Cd2 N6 N5 50.5(4) 2 . . . ? Br2 Cd2 N6 N5 -122.1(4) . . . . ? N6 Cd2 N6 C7 5.8(5) 2 . . . ? Br1 Cd2 N6 C7 136.2(5) . . . . ? Br1 Cd2 N6 C7 -123.7(5) 2 . . . ? Br2 Cd2 N6 C7 63.7(5) . . . . ? N2 N3 C1 C2 -0.1(6) . . . . ? Cd1 N3 C1 C2 -173.2(4) . . . . ? N2 N3 C1 C6 179.0(6) . . . . ? Cd1 N3 C1 C6 5.8(9) . . . . ? N2 N1 C2 C1 -0.3(6) . . . . ? C13 N1 C2 C1 168.5(5) . . . . ? N2 N1 C2 C3 176.7(6) . . . . ? C13 N1 C2 C3 -14.5(10) . . . . ? N3 C1 C2 N1 0.3(6) . . . . ? C6 C1 C2 N1 -178.9(5) . . . . ? N3 C1 C2 C3 -177.1(5) . . . . ? C6 C1 C2 C3 3.7(9) . . . . ? N1 C2 C3 C4 -179.8(6) . . . . ? C1 C2 C3 C4 -3.2(8) . . . . ? C2 C3 C4 C5 0.7(9) . . . . ? C3 C4 C5 C6 1.5(10) . . . . ? C4 C5 C6 C1 -1.2(10) . . . . ? C2 C1 C6 C5 -1.3(9) . . . . ? N3 C1 C6 C5 179.7(6) . . . . ? N5 N6 C7 C8 -2.3(6) . . . . ? Cd2 N6 C7 C8 172.2(4) . . . . ? N5 N6 C7 C12 179.1(6) . . . . ? Cd2 N6 C7 C12 -6.5(10) . . . . ? N5 N4 C8 C7 -1.2(6) . . . . ? C14 N4 C8 C7 170.4(5) . . . . ? N5 N4 C8 C9 176.9(6) . . . . ? C14 N4 C8 C9 -11.5(10) . . . . ? N6 C7 C8 N4 2.1(6) . . . . ? C12 C7 C8 N4 -179.1(5) . . . . ? N6 C7 C8 C9 -176.3(5) . . . . ? C12 C7 C8 C9 2.5(9) . . . . ? N4 C8 C9 C10 -179.8(6) . . . . ? C7 C8 C9 C10 -2.0(8) . . . . ? C8 C9 C10 C11 -0.6(9) . . . . ? C9 C10 C11 C12 2.8(10) . . . . ? C10 C11 C12 C7 -2.2(10) . . . . ? N6 C7 C12 C11 178.1(6) . . . . ? C8 C7 C12 C11 -0.4(9) . . . . ? N2 N1 C13 C14 82.3(6) . . . . ? C2 N1 C13 C14 -85.7(7) . . . . ? N5 N4 C14 C13 89.5(6) . . . . ? C8 N4 C14 C13 -81.3(7) . . . . ? N1 C13 C14 N4 -58.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.938 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.149 # Attachment '03.cif' data_03 _database_code_depnum_ccdc_archive 'CCDC 787189' #TrackingRef '03.cif' #=================================END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Cd5 Cl10 N12' _chemical_formula_sum 'C28 H24 Cd5 Cl10 N12' _chemical_formula_weight 1445.09 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 25.887(2) _cell_length_b 6.7510(10) _cell_length_c 25.753(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.269(2) _cell_angle_gamma 90.00 _cell_volume 4361.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3700 _cell_measurement_theta_min 2.448 _cell_measurement_theta_max 28.272 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 3.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4150 _exptl_absorpt_correction_T_max 0.5668 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9989 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3744 _reflns_number_gt 2313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0769P)^2^+58.6689P] 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 3744 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 0.62870(3) 0.75345(13) 0.87821(3) 0.0312(3) Uani 1 1 d . . . Cd2 Cd 0.68696(3) 0.25102(12) 0.93589(3) 0.0321(3) Uani 1 1 d . . . Cd3 Cd 0.7500 0.7500 1.0000 0.0316(3) Uani 1 2 d S . . Cl1 Cl 0.65590(10) 0.5880(4) 0.97604(10) 0.0319(6) Uani 1 1 d . . . Cl2 Cl 0.66405(12) 0.4224(4) 0.84526(11) 0.0410(7) Uani 1 1 d . . . Cl3 Cl 0.78438(10) 0.4134(4) 0.96572(10) 0.0293(5) Uani 1 1 d . . . Cl4 Cl 0.59656(11) 0.0832(5) 0.91492(12) 0.0427(7) Uani 1 1 d . . . Cl5 Cl 0.72675(10) -0.0842(4) 0.90439(10) 0.0312(6) Uani 1 1 d . . . N1 N 0.4705(4) 0.5042(18) 0.8303(5) 0.063(3) Uani 1 1 d . . . N2 N 0.5202(4) 0.5489(16) 0.8278(4) 0.053(3) Uani 1 1 d . . . N3 N 0.5416(4) 0.6447(15) 0.8695(4) 0.046(3) Uani 1 1 d . . . N4 N 0.5811(5) 1.0168(18) 0.7206(4) 0.064(3) Uani 1 1 d . . . N5 N 0.5775(4) 0.9614(18) 0.7705(5) 0.059(3) Uani 1 1 d . . . N6 N 0.6186(4) 0.8630(17) 0.7909(4) 0.048(3) Uani 1 1 d . . . C1 C 0.4398(6) 0.368(2) 0.7939(6) 0.074(5) Uani 1 1 d . . . H1A H 0.4440 0.3949 0.7581 0.089 Uiso 1 1 calc R . . H1B H 0.4024 0.3844 0.7933 0.089 Uiso 1 1 calc R . . C2 C 0.5434(6) 1.155(2) 0.6908(6) 0.059(4) Uani 1 1 d . . . H2A H 0.5087 1.1303 0.6975 0.071 Uiso 1 1 calc R . . H2B H 0.5403 1.1362 0.6528 0.071 Uiso 1 1 calc R . . C3 C 0.5090(5) 0.6647(19) 0.9034(6) 0.053(3) Uani 1 1 d . . . C4 C 0.4617(6) 0.567(2) 0.8782(6) 0.063(4) Uani 1 1 d . . . C5 C 0.4167(7) 0.560(3) 0.8986(8) 0.088(5) Uani 1 1 d . . . H5 H 0.3849 0.4999 0.8808 0.105 Uiso 1 1 calc R . . C6 C 0.4242(8) 0.651(3) 0.9487(9) 0.104(7) Uani 1 1 d . . . H6 H 0.3963 0.6471 0.9656 0.124 Uiso 1 1 calc R . . C7 C 0.4713(6) 0.747(2) 0.9747(6) 0.076(5) Uani 1 1 d . . . H7 H 0.4733 0.8085 1.0075 0.091 Uiso 1 1 calc R . . C8 C 0.5135(5) 0.754(2) 0.9537(5) 0.058(3) Uani 1 1 d . . . H8 H 0.5449 0.8154 0.9718 0.069 Uiso 1 1 calc R . . C9 C 0.6522(5) 0.8511(19) 0.7572(5) 0.048(3) Uani 1 1 d . . . C10 C 0.6285(6) 0.953(2) 0.7115(5) 0.057(4) Uani 1 1 d . . . C11 C 0.6514(7) 0.975(3) 0.6674(6) 0.084(5) Uani 1 1 d . . . H11 H 0.6353 1.0480 0.6371 0.101 Uiso 1 1 calc R . . C12 C 0.6984(7) 0.882(3) 0.6730(6) 0.090(6) Uani 1 1 d . . . H12 H 0.7148 0.8878 0.6447 0.108 Uiso 1 1 calc R . . C13 C 0.7243(5) 0.776(2) 0.7196(5) 0.066(4) Uani 1 1 d . . . H13 H 0.7573 0.7188 0.7215 0.080 Uiso 1 1 calc R . . C14 C 0.7017(5) 0.758(2) 0.7619(5) 0.051(3) Uani 1 1 d . . . H14 H 0.7182 0.6866 0.7924 0.061 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 0.0308(4) 0.0292(4) 0.0329(4) 0.0006(4) 0.0064(3) -0.0016(4) Cd2 0.0349(5) 0.0222(4) 0.0365(4) 0.0012(4) 0.0035(3) -0.0023(4) Cd3 0.0351(6) 0.0208(5) 0.0349(6) -0.0003(5) 0.0010(4) -0.0026(6) Cl1 0.0303(14) 0.0280(13) 0.0372(14) 0.0008(12) 0.0079(11) -0.0028(12) Cl2 0.0540(18) 0.0338(15) 0.0367(14) 0.0019(13) 0.0138(13) 0.0028(14) Cl3 0.0302(13) 0.0256(12) 0.0310(12) -0.0013(11) 0.0053(10) -0.0014(11) Cl4 0.0370(16) 0.0349(15) 0.0583(18) -0.0040(14) 0.0158(14) -0.0056(13) Cl5 0.0353(14) 0.0263(13) 0.0306(13) -0.0001(11) 0.0054(11) -0.0005(12) N1 0.045(7) 0.065(8) 0.077(8) -0.021(7) 0.008(6) -0.018(6) N2 0.054(7) 0.055(7) 0.053(7) -0.009(6) 0.016(6) -0.006(6) N3 0.050(6) 0.042(6) 0.053(6) 0.001(5) 0.023(5) 0.005(5) N4 0.065(8) 0.068(8) 0.053(7) 0.020(6) 0.004(6) 0.017(7) N5 0.048(7) 0.067(8) 0.062(7) 0.002(6) 0.017(6) 0.010(6) N6 0.041(6) 0.061(7) 0.044(6) -0.001(5) 0.017(5) -0.005(5) C1 0.062(10) 0.070(12) 0.080(11) -0.001(9) -0.003(8) -0.023(9) C2 0.054(9) 0.061(9) 0.066(9) 0.027(8) 0.020(7) 0.014(7) C3 0.053(8) 0.038(7) 0.069(9) 0.001(7) 0.020(7) -0.012(6) C4 0.061(9) 0.055(9) 0.079(10) -0.001(8) 0.028(8) -0.012(8) C5 0.063(11) 0.085(13) 0.124(15) -0.011(12) 0.039(11) -0.017(9) C6 0.093(15) 0.090(14) 0.157(19) -0.010(14) 0.088(14) 0.007(12) C7 0.097(13) 0.070(11) 0.082(10) -0.011(10) 0.062(10) -0.008(11) C8 0.069(9) 0.053(8) 0.056(7) -0.008(8) 0.023(7) -0.027(8) C9 0.051(8) 0.050(8) 0.044(7) 0.010(6) 0.015(6) 0.001(6) C10 0.060(9) 0.062(9) 0.047(7) 0.007(7) 0.014(7) -0.003(7) C11 0.083(12) 0.122(16) 0.052(9) 0.028(9) 0.024(9) 0.013(11) C12 0.076(12) 0.139(17) 0.065(10) 0.009(11) 0.038(9) 0.009(12) C13 0.061(9) 0.076(12) 0.073(10) 0.013(9) 0.037(8) 0.001(8) C14 0.048(7) 0.055(8) 0.053(7) 0.008(7) 0.020(6) 0.009(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 N6 2.320(10) . ? Cd1 N3 2.328(11) . ? Cd1 Cl4 2.633(3) 1_565 ? Cd1 Cl2 2.633(3) . ? Cd1 Cl1 2.686(3) . ? Cd1 Cl5 2.693(3) 1_565 ? Cd2 Cl4 2.535(3) . ? Cd2 Cl2 2.541(3) . ? Cd2 Cl3 2.683(3) . ? Cd2 Cl5 2.693(3) . ? Cd2 Cl3 2.697(3) 7_657 ? Cd2 Cl1 2.702(3) . ? Cd3 Cl1 2.602(3) . ? Cd3 Cl1 2.602(3) 7_667 ? Cd3 Cl5 2.636(2) 7_657 ? Cd3 Cl5 2.636(2) 1_565 ? Cd3 Cl3 2.669(3) . ? Cd3 Cl3 2.669(3) 7_667 ? Cl3 Cd2 2.697(3) 7_657 ? Cl4 Cd1 2.633(3) 1_545 ? Cl5 Cd3 2.636(2) 1_545 ? Cl5 Cd1 2.693(3) 1_545 ? N1 N2 1.338(14) . ? N1 C4 1.376(18) . ? N1 C1 1.411(17) . ? N2 N3 1.260(13) . ? N3 C3 1.362(16) . ? N4 N5 1.366(15) . ? N4 C10 1.373(17) . ? N4 C2 1.429(16) . ? N5 N6 1.256(14) . ? N6 C9 1.374(15) . ? C1 C2 1.53(2) 2_646 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C1 1.53(2) 2_666 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.403(18) . ? C3 C8 1.407(17) . ? C4 C5 1.39(2) . ? C5 C6 1.40(2) . ? C5 H5 0.9300 . ? C6 C7 1.40(2) . ? C6 H6 0.9300 . ? C7 C8 1.332(17) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.370(16) . ? C9 C14 1.407(17) . ? C10 C11 1.413(19) . ? C11 C12 1.35(2) . ? C11 H11 0.9300 . ? C12 C13 1.42(2) . ? C12 H12 0.9300 . ? C13 C14 1.362(15) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? 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 N6 Cd1 N3 97.6(4) . . ? N6 Cd1 Cl4 96.2(3) . 1_565 ? N3 Cd1 Cl4 85.2(3) . 1_565 ? N6 Cd1 Cl2 85.6(3) . . ? N3 Cd1 Cl2 96.1(3) . . ? Cl4 Cd1 Cl2 177.57(9) 1_565 . ? N6 Cd1 Cl1 169.2(3) . . ? N3 Cd1 Cl1 89.0(3) . . ? Cl4 Cd1 Cl1 92.73(9) 1_565 . ? Cl2 Cd1 Cl1 85.29(8) . . ? N6 Cd1 Cl5 89.2(3) . 1_565 ? N3 Cd1 Cl5 169.3(3) . 1_565 ? Cl4 Cd1 Cl5 85.86(9) 1_565 1_565 ? Cl2 Cd1 Cl5 92.58(9) . 1_565 ? Cl1 Cd1 Cl5 85.49(8) . 1_565 ? Cl4 Cd2 Cl2 90.79(10) . . ? Cl4 Cd2 Cl3 175.37(9) . . ? Cl2 Cd2 Cl3 93.84(9) . . ? Cl4 Cd2 Cl5 87.81(9) . . ? Cl2 Cd2 Cl5 97.24(9) . . ? Cl3 Cd2 Cl5 91.57(8) . . ? Cl4 Cd2 Cl3 92.40(9) . 7_657 ? Cl2 Cd2 Cl3 176.52(9) . 7_657 ? Cl3 Cd2 Cl3 82.97(8) . 7_657 ? Cl5 Cd2 Cl3 84.26(8) . 7_657 ? Cl4 Cd2 Cl1 96.41(9) . . ? Cl2 Cd2 Cl1 86.78(9) . . ? Cl3 Cd2 Cl1 83.90(8) . . ? Cl5 Cd2 Cl1 174.15(8) . . ? Cl3 Cd2 Cl1 91.49(8) 7_657 . ? Cl1 Cd3 Cl1 180.0 . 7_667 ? Cl1 Cd3 Cl5 91.61(8) . 7_657 ? Cl1 Cd3 Cl5 88.39(8) 7_667 7_657 ? Cl1 Cd3 Cl5 88.39(8) . 1_565 ? Cl1 Cd3 Cl5 91.61(8) 7_667 1_565 ? Cl5 Cd3 Cl5 180.000(1) 7_657 1_565 ? Cl1 Cd3 Cl3 86.14(8) . . ? Cl1 Cd3 Cl3 93.86(8) 7_667 . ? Cl5 Cd3 Cl3 85.95(8) 7_657 . ? Cl5 Cd3 Cl3 94.05(8) 1_565 . ? Cl1 Cd3 Cl3 93.86(8) . 7_667 ? Cl1 Cd3 Cl3 86.14(8) 7_667 7_667 ? Cl5 Cd3 Cl3 94.05(8) 7_657 7_667 ? Cl5 Cd3 Cl3 85.95(8) 1_565 7_667 ? Cl3 Cd3 Cl3 180.000(1) . 7_667 ? Cd3 Cl1 Cd1 93.52(8) . . ? Cd3 Cl1 Cd2 95.46(8) . . ? Cd1 Cl1 Cd2 91.44(8) . . ? Cd2 Cl2 Cd1 96.40(9) . . ? Cd3 Cl3 Cd2 94.36(8) . . ? Cd3 Cl3 Cd2 94.39(8) . 7_657 ? Cd2 Cl3 Cd2 97.03(8) . 7_657 ? Cd2 Cl4 Cd1 95.59(10) . 1_545 ? Cd3 Cl5 Cd2 95.26(8) 1_545 . ? Cd3 Cl5 Cd1 92.59(8) 1_545 1_545 ? Cd2 Cl5 Cd1 90.61(8) . 1_545 ? N2 N1 C4 110.3(11) . . ? N2 N1 C1 120.4(13) . . ? C4 N1 C1 127.3(13) . . ? N3 N2 N1 107.6(10) . . ? N2 N3 C3 112.6(11) . . ? N2 N3 Cd1 117.2(8) . . ? C3 N3 Cd1 130.2(9) . . ? N5 N4 C10 110.3(10) . . ? N5 N4 C2 119.2(12) . . ? C10 N4 C2 129.3(12) . . ? N6 N5 N4 106.9(10) . . ? N5 N6 C9 111.7(11) . . ? N5 N6 Cd1 117.0(8) . . ? C9 N6 Cd1 131.1(8) . . ? N1 C1 C2 111.3(12) . 2_646 ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 2_646 . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 2_646 . ? H1A C1 H1B 108.0 . . ? N4 C2 C1 111.2(12) . 2_666 ? N4 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 2_666 . ? N4 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 2_666 . ? H2A C2 H2B 108.0 . . ? N3 C3 C4 105.4(12) . . ? N3 C3 C8 135.2(12) . . ? C4 C3 C8 119.3(13) . . ? N1 C4 C5 131.8(15) . . ? N1 C4 C3 103.9(12) . . ? C5 C4 C3 124.1(15) . . ? C4 C5 C6 113.1(16) . . ? C4 C5 H5 123.4 . . ? C6 C5 H5 123.4 . . ? C5 C6 C7 123.6(15) . . ? C5 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C8 C7 C6 121.7(15) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C3 118.1(13) . . ? C7 C8 H8 121.0 . . ? C3 C8 H8 121.0 . . ? C10 C9 N6 107.1(12) . . ? C10 C9 C14 120.3(12) . . ? N6 C9 C14 132.5(11) . . ? C9 C10 N4 104.0(11) . . ? C9 C10 C11 123.7(14) . . ? N4 C10 C11 132.3(13) . . ? C12 C11 C10 114.4(15) . . ? C12 C11 H11 122.8 . . ? C10 C11 H11 122.8 . . ? C11 C12 C13 123.5(15) . . ? C11 C12 H12 118.2 . . ? C13 C12 H12 118.2 . . ? C14 C13 C12 121.1(14) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C9 116.8(12) . . ? C13 C14 H14 121.6 . . ? C9 C14 H14 121.6 . . ? 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 Cl1 Cd3 Cl1 Cd1 -119(100) 7_667 . . . ? Cl5 Cd3 Cl1 Cd1 179.58(8) 7_657 . . . ? Cl5 Cd3 Cl1 Cd1 -0.42(8) 1_565 . . . ? Cl3 Cd3 Cl1 Cd1 -94.58(8) . . . . ? Cl3 Cd3 Cl1 Cd1 85.42(8) 7_667 . . . ? Cl1 Cd3 Cl1 Cd2 -27(100) 7_667 . . . ? Cl5 Cd3 Cl1 Cd2 -88.63(8) 7_657 . . . ? Cl5 Cd3 Cl1 Cd2 91.37(8) 1_565 . . . ? Cl3 Cd3 Cl1 Cd2 -2.80(7) . . . . ? Cl3 Cd3 Cl1 Cd2 177.20(7) 7_667 . . . ? N6 Cd1 Cl1 Cd3 61.3(14) . . . . ? N3 Cd1 Cl1 Cd3 -170.4(3) . . . . ? Cl4 Cd1 Cl1 Cd3 -85.21(9) 1_565 . . . ? Cl2 Cd1 Cl1 Cd3 93.38(9) . . . . ? Cl5 Cd1 Cl1 Cd3 0.41(8) 1_565 . . . ? N6 Cd1 Cl1 Cd2 -34.3(14) . . . . ? N3 Cd1 Cl1 Cd2 94.0(3) . . . . ? Cl4 Cd1 Cl1 Cd2 179.23(8) 1_565 . . . ? Cl2 Cd1 Cl1 Cd2 -2.18(8) . . . . ? Cl5 Cd1 Cl1 Cd2 -95.15(8) 1_565 . . . ? Cl4 Cd2 Cl1 Cd3 178.15(8) . . . . ? Cl2 Cd2 Cl1 Cd3 -91.42(9) . . . . ? Cl3 Cd2 Cl1 Cd3 2.79(7) . . . . ? Cl5 Cd2 Cl1 Cd3 42.2(8) . . . . ? Cl3 Cd2 Cl1 Cd3 85.56(8) 7_657 . . . ? Cl4 Cd2 Cl1 Cd1 -88.18(9) . . . . ? Cl2 Cd2 Cl1 Cd1 2.25(8) . . . . ? Cl3 Cd2 Cl1 Cd1 96.47(8) . . . . ? Cl5 Cd2 Cl1 Cd1 135.8(8) . . . . ? Cl3 Cd2 Cl1 Cd1 179.23(7) 7_657 . . . ? Cl4 Cd2 Cl2 Cd1 94.06(10) . . . . ? Cl3 Cd2 Cl2 Cd1 -85.97(10) . . . . ? Cl5 Cd2 Cl2 Cd1 -178.04(8) . . . . ? Cl3 Cd2 Cl2 Cd1 -62.6(15) 7_657 . . . ? Cl1 Cd2 Cl2 Cd1 -2.31(9) . . . . ? N6 Cd1 Cl2 Cd2 176.6(3) . . . . ? N3 Cd1 Cl2 Cd2 -86.2(3) . . . . ? Cl4 Cd1 Cl2 Cd2 38(2) 1_565 . . . ? Cl1 Cd1 Cl2 Cd2 2.33(9) . . . . ? Cl5 Cd1 Cl2 Cd2 87.58(9) 1_565 . . . ? Cl1 Cd3 Cl3 Cd2 2.81(7) . . . . ? Cl1 Cd3 Cl3 Cd2 -177.19(7) 7_667 . . . ? Cl5 Cd3 Cl3 Cd2 94.70(8) 7_657 . . . ? Cl5 Cd3 Cl3 Cd2 -85.30(8) 1_565 . . . ? Cl3 Cd3 Cl3 Cd2 49(100) 7_667 . . . ? Cl1 Cd3 Cl3 Cd2 -94.60(8) . . . 7_657 ? Cl1 Cd3 Cl3 Cd2 85.40(8) 7_667 . . 7_657 ? Cl5 Cd3 Cl3 Cd2 -2.71(7) 7_657 . . 7_657 ? Cl5 Cd3 Cl3 Cd2 177.29(7) 1_565 . . 7_657 ? Cl3 Cd3 Cl3 Cd2 -49(100) 7_667 . . 7_657 ? Cl4 Cd2 Cl3 Cd3 -96.8(11) . . . . ? Cl2 Cd2 Cl3 Cd3 83.63(9) . . . . ? Cl5 Cd2 Cl3 Cd3 -179.01(7) . . . . ? Cl3 Cd2 Cl3 Cd3 -94.98(9) 7_657 . . . ? Cl1 Cd2 Cl3 Cd3 -2.72(7) . . . . ? Cl4 Cd2 Cl3 Cd2 -1.8(12) . . . 7_657 ? Cl2 Cd2 Cl3 Cd2 178.61(9) . . . 7_657 ? Cl5 Cd2 Cl3 Cd2 -84.02(8) . . . 7_657 ? Cl3 Cd2 Cl3 Cd2 0.0 7_657 . . 7_657 ? Cl1 Cd2 Cl3 Cd2 92.27(8) . . . 7_657 ? Cl2 Cd2 Cl4 Cd1 94.42(10) . . . 1_545 ? Cl3 Cd2 Cl4 Cd1 -85.1(11) . . . 1_545 ? Cl5 Cd2 Cl4 Cd1 -2.79(9) . . . 1_545 ? Cl3 Cd2 Cl4 Cd1 -86.96(9) 7_657 . . 1_545 ? Cl1 Cd2 Cl4 Cd1 -178.73(8) . . . 1_545 ? Cl4 Cd2 Cl5 Cd3 -89.94(9) . . . 1_545 ? Cl2 Cd2 Cl5 Cd3 179.54(8) . . . 1_545 ? Cl3 Cd2 Cl5 Cd3 85.47(8) . . . 1_545 ? Cl3 Cd2 Cl5 Cd3 2.70(7) 7_657 . . 1_545 ? Cl1 Cd2 Cl5 Cd3 46.4(8) . . . 1_545 ? Cl4 Cd2 Cl5 Cd1 2.72(8) . . . 1_545 ? Cl2 Cd2 Cl5 Cd1 -87.80(9) . . . 1_545 ? Cl3 Cd2 Cl5 Cd1 178.13(7) . . . 1_545 ? Cl3 Cd2 Cl5 Cd1 95.36(8) 7_657 . . 1_545 ? Cl1 Cd2 Cl5 Cd1 139.0(8) . . . 1_545 ? C4 N1 N2 N3 -3.7(16) . . . . ? C1 N1 N2 N3 -168.9(12) . . . . ? N1 N2 N3 C3 2.2(15) . . . . ? N1 N2 N3 Cd1 -178.9(8) . . . . ? N6 Cd1 N3 N2 43.1(9) . . . . ? Cl4 Cd1 N3 N2 138.8(9) 1_565 . . . ? Cl2 Cd1 N3 N2 -43.3(9) . . . . ? Cl1 Cd1 N3 N2 -128.4(9) . . . . ? Cl5 Cd1 N3 N2 172.5(9) 1_565 . . . ? N6 Cd1 N3 C3 -138.2(11) . . . . ? Cl4 Cd1 N3 C3 -42.6(11) 1_565 . . . ? Cl2 Cd1 N3 C3 135.4(11) . . . . ? Cl1 Cd1 N3 C3 50.3(11) . . . . ? Cl5 Cd1 N3 C3 -9(2) 1_565 . . . ? C10 N4 N5 N6 -2.4(16) . . . . ? C2 N4 N5 N6 -171.1(12) . . . . ? N4 N5 N6 C9 1.5(15) . . . . ? N4 N5 N6 Cd1 177.4(8) . . . . ? N3 Cd1 N6 N5 44.0(10) . . . . ? Cl4 Cd1 N6 N5 -42.0(9) 1_565 . . . ? Cl2 Cd1 N6 N5 139.6(9) . . . . ? Cl1 Cd1 N6 N5 171.7(10) . . . . ? Cl5 Cd1 N6 N5 -127.8(9) 1_565 . . . ? N3 Cd1 N6 C9 -141.1(11) . . . . ? Cl4 Cd1 N6 C9 132.9(11) 1_565 . . . ? Cl2 Cd1 N6 C9 -45.5(11) . . . . ? Cl1 Cd1 N6 C9 -13(2) . . . . ? Cl5 Cd1 N6 C9 47.2(11) 1_565 . . . ? N2 N1 C1 C2 77.4(18) . . . 2_646 ? C4 N1 C1 C2 -85.1(19) . . . 2_646 ? N5 N4 C2 C1 84.2(16) . . . 2_666 ? C10 N4 C2 C1 -82.0(19) . . . 2_666 ? N2 N3 C3 C4 0.0(15) . . . . ? Cd1 N3 C3 C4 -178.7(9) . . . . ? N2 N3 C3 C8 179.5(15) . . . . ? Cd1 N3 C3 C8 1(2) . . . . ? N2 N1 C4 C5 178.0(17) . . . . ? C1 N1 C4 C5 -18(3) . . . . ? N2 N1 C4 C3 3.6(16) . . . . ? C1 N1 C4 C3 167.5(14) . . . . ? N3 C3 C4 N1 -2.2(15) . . . . ? C8 C3 C4 N1 178.3(13) . . . . ? N3 C3 C4 C5 -177.1(15) . . . . ? C8 C3 C4 C5 3(2) . . . . ? N1 C4 C5 C6 -176.8(17) . . . . ? C3 C4 C5 C6 -3(3) . . . . ? C4 C5 C6 C7 3(3) . . . . ? C5 C6 C7 C8 -2(3) . . . . ? C6 C7 C8 C3 2(3) . . . . ? N3 C3 C8 C7 178.4(16) . . . . ? C4 C3 C8 C7 -2(2) . . . . ? N5 N6 C9 C10 -0.1(16) . . . . ? Cd1 N6 C9 C10 -175.2(9) . . . . ? N5 N6 C9 C14 -179.4(14) . . . . ? Cd1 N6 C9 C14 5(2) . . . . ? N6 C9 C10 N4 -1.4(15) . . . . ? C14 C9 C10 N4 178.1(13) . . . . ? N6 C9 C10 C11 179.6(14) . . . . ? C14 C9 C10 C11 -1(2) . . . . ? N5 N4 C10 C9 2.3(16) . . . . ? C2 N4 C10 C9 169.5(14) . . . . ? N5 N4 C10 C11 -178.7(17) . . . . ? C2 N4 C10 C11 -12(3) . . . . ? C9 C10 C11 C12 2(3) . . . . ? N4 C10 C11 C12 -177.1(17) . . . . ? C10 C11 C12 C13 -2(3) . . . . ? C11 C12 C13 C14 2(3) . . . . ? C12 C13 C14 C9 -1(2) . . . . ? C10 C9 C14 C13 1(2) . . . . ? N6 C9 C14 C13 179.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.750 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.187 # Attachment '04.cif' data_04 _database_code_depnum_ccdc_archive 'CCDC 787190' #TrackingRef '04.cif' #=================================END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H14 Cd I2 N6' _chemical_formula_sum 'C15 H14 Cd I2 N6' _chemical_formula_weight 644.52 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' I I -0.4742 1.8119 '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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9448(11) _cell_length_b 23.481(3) _cell_length_c 9.1979(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.1790(10) _cell_angle_gamma 90.00 _cell_volume 1988.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4065 _cell_measurement_theta_min 2.376 _cell_measurement_theta_max 26.333 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 4.211 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2371 _exptl_absorpt_correction_T_max 0.3648 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9840 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3497 _reflns_number_gt 2714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0161P)^2^+3.6009P] 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 3497 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.70571(4) 0.146882(17) 0.31503(5) 0.04190(13) Uani 1 1 d . . . I1 I 0.55738(5) 0.231809(18) 0.13048(5) 0.06263(15) Uani 1 1 d . . . I2 I 0.77845(5) 0.052104(19) 0.19104(6) 0.07013(17) Uani 1 1 d . . . N1 N 0.6113(5) 0.10784(18) 0.4819(5) 0.0391(11) Uani 1 1 d . . . N2 N 0.4845(5) 0.12258(19) 0.4803(5) 0.0415(11) Uani 1 1 d . . . N3 N 0.4533(5) 0.08880(19) 0.5811(5) 0.0397(11) Uani 1 1 d . . . N4 N 1.1142(4) 0.17094(18) 0.6989(5) 0.0377(11) Uani 1 1 d . . . N5 N 1.0004(5) 0.14373(19) 0.5965(6) 0.0461(12) Uani 1 1 d . . . N6 N 0.9135(5) 0.18171(19) 0.5023(6) 0.0461(12) Uani 1 1 d . . . C1 C 0.5625(6) 0.0511(2) 0.6509(6) 0.0379(13) Uani 1 1 d . . . C2 C 0.6658(6) 0.0637(2) 0.5874(6) 0.0367(13) Uani 1 1 d . . . C3 C 0.7956(6) 0.0329(2) 0.6328(7) 0.0465(14) Uani 1 1 d . . . H3 H 0.8656 0.0408 0.5913 0.056 Uiso 1 1 calc R . . C4 C 0.8149(7) -0.0094(3) 0.7406(8) 0.0575(17) Uani 1 1 d . . . H4 H 0.9004 -0.0304 0.7746 0.069 Uiso 1 1 calc R . . C5 C 0.7080(7) -0.0216(3) 0.8011(8) 0.0593(17) Uani 1 1 d . . . H5 H 0.7244 -0.0514 0.8723 0.071 Uiso 1 1 calc R . . C6 C 0.5816(7) 0.0080(2) 0.7610(7) 0.0474(15) Uani 1 1 d . . . H6 H 0.5127 0.0000 0.8040 0.057 Uiso 1 1 calc R . . C7 C 0.9715(5) 0.2353(2) 0.5454(6) 0.0392(13) Uani 1 1 d . . . C8 C 1.1024(6) 0.2283(2) 0.6715(6) 0.0378(13) Uani 1 1 d . . . C9 C 1.1905(6) 0.2748(3) 0.7441(7) 0.0498(16) Uani 1 1 d . . . H9 H 1.2779 0.2703 0.8291 0.060 Uiso 1 1 calc R . . C10 C 1.1409(7) 0.3265(3) 0.6829(8) 0.0602(18) Uani 1 1 d . . . H10 H 1.1971 0.3584 0.7262 0.072 Uiso 1 1 calc R . . C11 C 1.0075(7) 0.3341(3) 0.5562(8) 0.0610(18) Uani 1 1 d . . . H11 H 0.9768 0.3707 0.5209 0.073 Uiso 1 1 calc R . . C12 C 0.9220(6) 0.2886(2) 0.4836(7) 0.0504(16) Uani 1 1 d . . . H12 H 0.8354 0.2933 0.3976 0.060 Uiso 1 1 calc R . . C13 C 0.3231(6) 0.0986(3) 0.6155(6) 0.0441(14) Uani 1 1 d . . . H13A H 0.2795 0.0624 0.6231 0.053 Uiso 1 1 calc R . . H13B H 0.2530 0.1202 0.5306 0.053 Uiso 1 1 calc R . . C14 C 0.3607(6) 0.1310(2) 0.7678(6) 0.0398(13) Uani 1 1 d . . . H14A H 0.3989 0.1681 0.7570 0.048 Uiso 1 1 calc R . . H14B H 0.4363 0.1106 0.8505 0.048 Uiso 1 1 calc R . . C15 C 1.2314(6) 0.1389(2) 0.8149(6) 0.0427(14) Uani 1 1 d . . . H15A H 1.1951 0.1018 0.8291 0.051 Uiso 1 1 calc R . . H15B H 1.2626 0.1587 0.9148 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 0.0343(2) 0.0429(2) 0.0442(3) 0.00057(19) 0.01001(19) -0.00258(18) I1 0.0635(3) 0.0606(3) 0.0466(2) 0.0048(2) 0.0013(2) 0.0143(2) I2 0.0761(3) 0.0605(3) 0.0932(4) -0.0198(3) 0.0540(3) -0.0084(2) N1 0.042(3) 0.037(3) 0.042(3) 0.000(2) 0.020(2) -0.002(2) N2 0.040(3) 0.041(3) 0.046(3) -0.003(2) 0.018(2) 0.000(2) N3 0.034(2) 0.043(3) 0.041(3) -0.007(2) 0.014(2) -0.002(2) N4 0.028(2) 0.042(3) 0.042(3) -0.003(2) 0.012(2) -0.001(2) N5 0.034(3) 0.041(3) 0.056(3) -0.001(2) 0.009(2) -0.002(2) N6 0.032(2) 0.041(3) 0.056(3) -0.005(2) 0.005(2) -0.003(2) C1 0.041(3) 0.034(3) 0.039(3) -0.010(3) 0.015(3) 0.000(2) C2 0.037(3) 0.036(3) 0.037(3) -0.010(2) 0.014(3) -0.005(2) C3 0.040(3) 0.040(3) 0.060(4) -0.004(3) 0.019(3) 0.002(3) C4 0.049(4) 0.049(4) 0.070(5) -0.001(3) 0.018(4) 0.013(3) C5 0.075(5) 0.045(4) 0.057(4) 0.009(3) 0.024(4) 0.011(3) C6 0.055(4) 0.047(4) 0.046(4) -0.002(3) 0.026(3) -0.002(3) C7 0.029(3) 0.038(3) 0.049(3) -0.010(3) 0.012(3) -0.003(2) C8 0.036(3) 0.037(3) 0.043(3) -0.003(2) 0.017(3) 0.001(2) C9 0.039(3) 0.054(4) 0.049(4) -0.010(3) 0.009(3) -0.007(3) C10 0.055(4) 0.042(4) 0.077(5) -0.014(3) 0.017(4) -0.014(3) C11 0.064(4) 0.037(3) 0.079(5) 0.001(3) 0.024(4) 0.004(3) C12 0.042(3) 0.043(3) 0.061(4) 0.000(3) 0.012(3) 0.004(3) C13 0.035(3) 0.057(4) 0.043(3) -0.004(3) 0.018(3) 0.001(3) C14 0.034(3) 0.044(3) 0.038(3) -0.003(3) 0.011(3) 0.005(2) C15 0.042(3) 0.046(3) 0.041(3) 0.000(3) 0.017(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.273(4) . ? Cd1 N6 2.284(4) . ? Cd1 I1 2.6728(6) . ? Cd1 I2 2.7202(6) . ? N1 N2 1.302(6) . ? N1 C2 1.382(7) . ? N2 N3 1.343(6) . ? N3 C1 1.360(6) . ? N3 C13 1.462(7) . ? N4 N5 1.331(6) . ? N4 C8 1.366(6) . ? N4 C15 1.458(6) . ? N5 N6 1.315(6) . ? N6 C7 1.378(6) . ? C1 C2 1.392(7) . ? C1 C6 1.393(8) . ? C2 C3 1.400(7) . ? C3 C4 1.363(8) . ? C3 H3 0.9300 . ? C4 C5 1.404(9) . ? C4 H4 0.9300 . ? C5 C6 1.360(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.386(7) . ? C7 C8 1.388(7) . ? C8 C9 1.401(7) . ? C9 C10 1.352(8) . ? C9 H9 0.9300 . ? C10 C11 1.407(8) . ? C10 H10 0.9300 . ? C11 C12 1.371(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.511(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.516(7) 1_455 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C14 1.516(7) 1_655 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? 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 N6 96.98(17) . . ? N1 Cd1 I1 117.40(11) . . ? N6 Cd1 I1 109.70(12) . . ? N1 Cd1 I2 101.32(11) . . ? N6 Cd1 I2 107.53(12) . . ? I1 Cd1 I2 120.96(2) . . ? N2 N1 C2 109.2(5) . . ? N2 N1 Cd1 122.0(3) . . ? C2 N1 Cd1 128.6(4) . . ? N1 N2 N3 108.1(4) . . ? N2 N3 C1 111.0(4) . . ? N2 N3 C13 120.7(4) . . ? C1 N3 C13 128.0(5) . . ? N5 N4 C8 110.6(4) . . ? N5 N4 C15 120.1(4) . . ? C8 N4 C15 129.3(4) . . ? N6 N5 N4 108.2(4) . . ? N5 N6 C7 109.2(4) . . ? N5 N6 Cd1 115.9(3) . . ? C7 N6 Cd1 134.8(4) . . ? N3 C1 C2 104.3(5) . . ? N3 C1 C6 132.9(5) . . ? C2 C1 C6 122.7(5) . . ? N1 C2 C1 107.4(5) . . ? N1 C2 C3 132.1(5) . . ? C1 C2 C3 120.5(5) . . ? C4 C3 C2 117.0(6) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C3 C4 C5 121.2(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 123.3(6) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C5 C6 C1 115.3(6) . . ? C5 C6 H6 122.4 . . ? C1 C6 H6 122.4 . . ? N6 C7 C12 131.4(5) . . ? N6 C7 C8 106.9(5) . . ? C12 C7 C8 121.7(5) . . ? N4 C8 C7 105.0(4) . . ? N4 C8 C9 133.2(5) . . ? C7 C8 C9 121.7(5) . . ? C10 C9 C8 116.0(5) . . ? C10 C9 H9 122.0 . . ? C8 C9 H9 122.0 . . ? C9 C10 C11 122.6(6) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 121.5(6) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C7 116.4(5) . . ? C11 C12 H12 121.8 . . ? C7 C12 H12 121.8 . . ? N3 C13 C14 110.5(4) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 112.8(4) . 1_455 ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 1_455 . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 1_455 . ? H14A C14 H14B 107.8 . . ? N4 C15 C14 112.6(4) . 1_655 ? N4 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 1_655 . ? N4 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 1_655 . ? H15A C15 H15B 107.8 . . ? 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 N6 Cd1 N1 N2 122.0(4) . . . . ? I1 Cd1 N1 N2 5.5(4) . . . . ? I2 Cd1 N1 N2 -128.5(4) . . . . ? N6 Cd1 N1 C2 -64.0(4) . . . . ? I1 Cd1 N1 C2 179.5(4) . . . . ? I2 Cd1 N1 C2 45.5(4) . . . . ? C2 N1 N2 N3 -0.6(5) . . . . ? Cd1 N1 N2 N3 174.5(3) . . . . ? N1 N2 N3 C1 0.2(6) . . . . ? N1 N2 N3 C13 174.4(4) . . . . ? C8 N4 N5 N6 -0.1(6) . . . . ? C15 N4 N5 N6 -177.9(5) . . . . ? N4 N5 N6 C7 -0.6(6) . . . . ? N4 N5 N6 Cd1 -179.2(3) . . . . ? N1 Cd1 N6 N5 60.8(4) . . . . ? I1 Cd1 N6 N5 -176.7(4) . . . . ? I2 Cd1 N6 N5 -43.4(4) . . . . ? N1 Cd1 N6 C7 -117.3(6) . . . . ? I1 Cd1 N6 C7 5.1(6) . . . . ? I2 Cd1 N6 C7 138.5(5) . . . . ? N2 N3 C1 C2 0.3(6) . . . . ? C13 N3 C1 C2 -173.3(5) . . . . ? N2 N3 C1 C6 -179.7(5) . . . . ? C13 N3 C1 C6 6.7(9) . . . . ? N2 N1 C2 C1 0.8(6) . . . . ? Cd1 N1 C2 C1 -173.8(3) . . . . ? N2 N1 C2 C3 180.0(5) . . . . ? Cd1 N1 C2 C3 5.4(8) . . . . ? N3 C1 C2 N1 -0.7(5) . . . . ? C6 C1 C2 N1 179.3(5) . . . . ? N3 C1 C2 C3 -180.0(5) . . . . ? C6 C1 C2 C3 0.0(8) . . . . ? N1 C2 C3 C4 -179.1(5) . . . . ? C1 C2 C3 C4 -0.1(8) . . . . ? C2 C3 C4 C5 0.8(9) . . . . ? C3 C4 C5 C6 -1.7(10) . . . . ? C4 C5 C6 C1 1.6(9) . . . . ? N3 C1 C6 C5 179.2(6) . . . . ? C2 C1 C6 C5 -0.8(8) . . . . ? N5 N6 C7 C12 179.9(6) . . . . ? Cd1 N6 C7 C12 -1.9(10) . . . . ? N5 N6 C7 C8 1.1(6) . . . . ? Cd1 N6 C7 C8 179.3(4) . . . . ? N5 N4 C8 C7 0.8(6) . . . . ? C15 N4 C8 C7 178.3(5) . . . . ? N5 N4 C8 C9 179.8(6) . . . . ? C15 N4 C8 C9 -2.6(10) . . . . ? N6 C7 C8 N4 -1.1(6) . . . . ? C12 C7 C8 N4 179.9(5) . . . . ? N6 C7 C8 C9 179.7(5) . . . . ? C12 C7 C8 C9 0.7(9) . . . . ? N4 C8 C9 C10 -179.5(6) . . . . ? C7 C8 C9 C10 -0.6(9) . . . . ? C8 C9 C10 C11 1.3(10) . . . . ? C9 C10 C11 C12 -2.3(11) . . . . ? C10 C11 C12 C7 2.2(10) . . . . ? N6 C7 C12 C11 179.8(6) . . . . ? C8 C7 C12 C11 -1.5(9) . . . . ? N2 N3 C13 C14 -98.8(6) . . . . ? C1 N3 C13 C14 74.3(7) . . . . ? N3 C13 C14 C15 -176.1(5) . . . 1_455 ? N5 N4 C15 C14 99.6(6) . . . 1_655 ? C8 N4 C15 C14 -77.8(7) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.606 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.108 # Attachment '05.cif' data_05 _database_code_depnum_ccdc_archive 'CCDC 787191' #TrackingRef '05.cif' #=================================END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 Br2 Cd N6' _chemical_formula_sum 'C16 H16 Br2 Cd N6' _chemical_formula_weight 564.57 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' Br Br -0.2901 2.4595 '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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5203(9) _cell_length_b 23.232(3) _cell_length_c 8.5244(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.5780(10) _cell_angle_gamma 90.00 _cell_volume 1937.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4379 _cell_measurement_theta_min 2.259 _cell_measurement_theta_max 28.135 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 5.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2215 _exptl_absorpt_correction_T_max 0.2462 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9818 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3417 _reflns_number_gt 2842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0299P)^2^+3.5835P] 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 3417 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.53836(3) 0.564874(14) 0.66819(4) 0.03014(11) Uani 1 1 d . . . Br1 Br 0.52946(6) 0.55773(2) 0.35771(6) 0.04005(15) Uani 1 1 d . . . Br2 Br 0.77426(5) 0.55560(2) 0.89380(7) 0.04557(16) Uani 1 1 d . . . N1 N 0.2026(4) 0.58447(16) 0.8405(5) 0.0297(9) Uani 1 1 d . . . N2 N 0.3346(4) 0.58134(17) 0.8604(5) 0.0311(9) Uani 1 1 d . . . N3 N 0.3405(4) 0.57386(16) 0.7108(5) 0.0307(9) Uani 1 1 d . . . N4 N 0.4503(4) 0.75497(16) 0.6507(5) 0.0398(10) Uani 1 1 d . . . N5 N 0.4242(4) 0.69874(17) 0.6645(5) 0.0421(10) Uani 1 1 d . . . N6 N 0.5239(4) 0.66884(17) 0.6459(5) 0.0408(10) Uani 1 1 d . . . C1 C 0.2108(5) 0.57227(19) 0.5917(6) 0.0317(11) Uani 1 1 d . . . C2 C 0.1205(5) 0.57943(19) 0.6748(6) 0.0290(10) Uani 1 1 d . . . C3 C -0.0214(5) 0.5788(2) 0.5903(7) 0.0415(13) Uani 1 1 d . . . H3 H -0.0815 0.5822 0.6470 0.050 Uiso 1 1 calc R . . C4 C -0.0658(6) 0.5728(3) 0.4190(7) 0.0542(15) Uani 1 1 d . . . H4 H -0.1593 0.5730 0.3565 0.065 Uiso 1 1 calc R . . C5 C 0.0261(6) 0.5662(3) 0.3340(7) 0.0546(15) Uani 1 1 d . . . H5 H -0.0085 0.5624 0.2172 0.066 Uiso 1 1 calc R . . C6 C 0.1633(5) 0.5654(2) 0.4183(6) 0.0445(13) Uani 1 1 d . . . H6 H 0.2232 0.5603 0.3618 0.053 Uiso 1 1 calc R . . C7 C 0.6153(5) 0.7062(2) 0.6193(6) 0.0380(12) Uani 1 1 d . . . C8 C 0.5680(5) 0.7620(2) 0.6214(6) 0.0374(12) Uani 1 1 d . . . C9 C 0.6389(6) 0.8101(2) 0.5971(8) 0.0564(16) Uani 1 1 d . . . H9 H 0.6070 0.8474 0.5971 0.068 Uiso 1 1 calc R . . C10 C 0.7581(7) 0.7986(3) 0.5731(8) 0.0654(18) Uani 1 1 d . . . H10 H 0.8101 0.8292 0.5594 0.078 Uiso 1 1 calc R . . C11 C 0.8042(7) 0.7423(3) 0.5685(9) 0.0651(18) Uani 1 1 d . . . H11 H 0.8843 0.7367 0.5482 0.078 Uiso 1 1 calc R . . C12 C 0.7371(6) 0.6960(3) 0.5922(8) 0.0548(15) Uani 1 1 d . . . H12 H 0.7698 0.6589 0.5909 0.066 Uiso 1 1 calc R . . C13 C 0.1651(5) 0.5954(2) 0.9874(6) 0.0337(11) Uani 1 1 d . . . H13A H 0.2431 0.5875 1.0897 0.040 Uiso 1 1 calc R . . H13B H 0.0918 0.5695 0.9843 0.040 Uiso 1 1 calc R . . C14 C 0.1189(5) 0.6576(2) 0.9907(7) 0.0404(12) Uani 1 1 d . . . H14A H 0.0369 0.6641 0.8920 0.049 Uiso 1 1 calc R . . H14B H 0.0952 0.6628 1.0894 0.049 Uiso 1 1 calc R . . C15 C 0.2243(5) 0.7973(2) 0.4937(7) 0.0412(12) Uani 1 1 d . . . H15A H 0.1822 0.7596 0.4799 0.049 Uiso 1 1 calc R . . H15B H 0.2523 0.8038 0.3987 0.049 Uiso 1 1 calc R . . C16 C 0.3496(5) 0.7977(2) 0.6540(7) 0.0445(13) Uani 1 1 d . . . H16A H 0.3909 0.8356 0.6698 0.053 Uiso 1 1 calc R . . H16B H 0.3225 0.7900 0.7491 0.053 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 0.02178(18) 0.03410(19) 0.0331(2) -0.00143(15) 0.00838(14) 0.00267(14) Br1 0.0474(3) 0.0357(3) 0.0384(3) 0.0009(2) 0.0175(2) -0.0026(2) Br2 0.0316(3) 0.0444(3) 0.0467(3) -0.0041(2) -0.0020(2) 0.0021(2) N1 0.026(2) 0.035(2) 0.030(2) -0.0008(17) 0.0128(17) -0.0005(17) N2 0.025(2) 0.035(2) 0.034(2) 0.0001(17) 0.0125(17) 0.0016(17) N3 0.024(2) 0.031(2) 0.038(2) 0.0003(17) 0.0120(18) -0.0003(16) N4 0.042(3) 0.026(2) 0.047(3) -0.0028(18) 0.011(2) 0.0061(18) N5 0.042(3) 0.030(2) 0.054(3) -0.003(2) 0.018(2) 0.0026(19) N6 0.039(3) 0.030(2) 0.053(3) 0.0033(19) 0.017(2) 0.0068(19) C1 0.024(2) 0.031(2) 0.041(3) 0.001(2) 0.014(2) 0.0011(19) C2 0.029(3) 0.030(2) 0.029(3) 0.0028(19) 0.012(2) 0.002(2) C3 0.027(3) 0.054(3) 0.048(3) 0.006(3) 0.019(2) 0.006(2) C4 0.028(3) 0.076(4) 0.050(4) 0.010(3) 0.004(3) 0.005(3) C5 0.046(3) 0.081(4) 0.030(3) -0.002(3) 0.007(3) -0.006(3) C6 0.039(3) 0.059(3) 0.035(3) -0.005(3) 0.013(2) -0.003(3) C7 0.032(3) 0.031(3) 0.045(3) 0.006(2) 0.008(2) 0.005(2) C8 0.035(3) 0.033(3) 0.037(3) 0.004(2) 0.005(2) 0.001(2) C9 0.060(4) 0.033(3) 0.070(4) 0.013(3) 0.016(3) 0.005(3) C10 0.057(4) 0.055(4) 0.079(5) 0.023(3) 0.020(4) -0.013(3) C11 0.054(4) 0.063(4) 0.086(5) 0.019(4) 0.036(4) 0.006(3) C12 0.047(4) 0.047(3) 0.072(4) 0.010(3) 0.023(3) 0.012(3) C13 0.034(3) 0.036(3) 0.037(3) -0.003(2) 0.020(2) -0.003(2) C14 0.038(3) 0.043(3) 0.047(3) -0.005(2) 0.023(3) 0.001(2) C15 0.042(3) 0.032(3) 0.049(3) 0.001(2) 0.017(3) 0.000(2) C16 0.049(3) 0.032(3) 0.049(3) -0.002(2) 0.015(3) 0.009(2) _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 2.250(4) . ? Cd1 N6 2.423(4) . ? Cd1 Br2 2.5286(6) . ? Cd1 Br1 2.6190(6) . ? Cd1 Br1 2.9249(7) 3_666 ? Br1 Cd1 2.9249(7) 3_666 ? N1 N2 1.338(5) . ? N1 C2 1.363(6) . ? N1 C13 1.467(6) . ? N2 N3 1.311(5) . ? N3 C1 1.369(6) . ? N4 N5 1.349(5) . ? N4 C8 1.360(6) . ? N4 C16 1.460(6) . ? N5 N6 1.315(5) . ? N6 C7 1.374(6) . ? C1 C6 1.385(7) . ? C1 C2 1.388(6) . ? C2 C3 1.398(7) . ? C3 C4 1.367(8) . ? C3 H3 0.9300 . ? C4 C5 1.414(8) . ? C4 H4 0.9300 . ? C5 C6 1.356(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.393(6) . ? C7 C12 1.402(7) . ? C8 C9 1.399(7) . ? C9 C10 1.369(8) . ? C9 H9 0.9300 . ? C10 C11 1.401(9) . ? C10 H10 0.9300 . ? C11 C12 1.341(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.528(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.519(7) 4_576 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.510(7) . ? C15 C14 1.519(7) 4_575 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? 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 N6 83.39(14) . . ? N3 Cd1 Br2 126.33(10) . . ? N6 Cd1 Br2 99.23(10) . . ? N3 Cd1 Br1 118.53(10) . . ? N6 Cd1 Br1 90.35(10) . . ? Br2 Cd1 Br1 115.06(2) . . ? N3 Cd1 Br1 83.57(9) . 3_666 ? N6 Cd1 Br1 163.37(10) . 3_666 ? Br2 Cd1 Br1 96.795(19) . 3_666 ? Br1 Cd1 Br1 86.844(17) . 3_666 ? Cd1 Br1 Cd1 93.156(17) . 3_666 ? N2 N1 C2 111.1(4) . . ? N2 N1 C13 119.6(4) . . ? C2 N1 C13 129.2(4) . . ? N3 N2 N1 107.6(4) . . ? N2 N3 C1 109.5(4) . . ? N2 N3 Cd1 123.2(3) . . ? C1 N3 Cd1 127.3(3) . . ? N5 N4 C8 111.2(4) . . ? N5 N4 C16 119.0(4) . . ? C8 N4 C16 129.6(4) . . ? N6 N5 N4 107.7(4) . . ? N5 N6 C7 108.9(4) . . ? N5 N6 Cd1 123.2(3) . . ? C7 N6 Cd1 127.9(3) . . ? N3 C1 C6 131.6(4) . . ? N3 C1 C2 107.5(4) . . ? C6 C1 C2 120.8(4) . . ? N1 C2 C1 104.3(4) . . ? N1 C2 C3 133.2(4) . . ? C1 C2 C3 122.5(4) . . ? C4 C3 C2 115.6(5) . . ? C4 C3 H3 122.2 . . ? C2 C3 H3 122.2 . . ? C3 C4 C5 121.9(5) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 121.7(5) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 117.4(5) . . ? C5 C6 H6 121.3 . . ? C1 C6 H6 121.3 . . ? N6 C7 C8 108.1(4) . . ? N6 C7 C12 131.2(5) . . ? C8 C7 C12 120.7(5) . . ? N4 C8 C7 104.1(4) . . ? N4 C8 C9 134.0(5) . . ? C7 C8 C9 121.9(5) . . ? C10 C9 C8 115.8(5) . . ? C10 C9 H9 122.1 . . ? C8 C9 H9 122.1 . . ? C9 C10 C11 122.1(6) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C12 C11 C10 122.5(6) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C11 C12 C7 117.0(5) . . ? C11 C12 H12 121.5 . . ? C7 C12 H12 121.5 . . ? N1 C13 C14 111.5(4) . . ? N1 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N1 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 114.7(4) 4_576 . ? C15 C14 H14A 108.6 4_576 . ? C13 C14 H14A 108.6 . . ? C15 C14 H14B 108.6 4_576 . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C14 113.6(4) . 4_575 ? C16 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 4_575 . ? C16 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 4_575 . ? H15A C15 H15B 107.7 . . ? N4 C16 C15 112.1(4) . . ? N4 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? N4 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? 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 N3 Cd1 Br1 Cd1 -80.93(11) . . . 3_666 ? N6 Cd1 Br1 Cd1 -163.60(10) . . . 3_666 ? Br2 Cd1 Br1 Cd1 96.03(2) . . . 3_666 ? Br1 Cd1 Br1 Cd1 0.0 3_666 . . 3_666 ? C2 N1 N2 N3 -0.5(5) . . . . ? C13 N1 N2 N3 -177.3(4) . . . . ? N1 N2 N3 C1 0.2(5) . . . . ? N1 N2 N3 Cd1 -179.5(3) . . . . ? N6 Cd1 N3 N2 -88.8(3) . . . . ? Br2 Cd1 N3 N2 7.8(4) . . . . ? Br1 Cd1 N3 N2 -175.6(3) . . . . ? Br1 Cd1 N3 N2 101.5(3) 3_666 . . . ? N6 Cd1 N3 C1 91.6(4) . . . . ? Br2 Cd1 N3 C1 -171.8(3) . . . . ? Br1 Cd1 N3 C1 4.8(4) . . . . ? Br1 Cd1 N3 C1 -78.1(4) 3_666 . . . ? C8 N4 N5 N6 0.4(6) . . . . ? C16 N4 N5 N6 175.5(4) . . . . ? N4 N5 N6 C7 -0.2(5) . . . . ? N4 N5 N6 Cd1 177.7(3) . . . . ? N3 Cd1 N6 N5 1.3(4) . . . . ? Br2 Cd1 N6 N5 -124.5(4) . . . . ? Br1 Cd1 N6 N5 120.0(4) . . . . ? Br1 Cd1 N6 N5 39.9(6) 3_666 . . . ? N3 Cd1 N6 C7 178.7(4) . . . . ? Br2 Cd1 N6 C7 52.9(4) . . . . ? Br1 Cd1 N6 C7 -62.6(4) . . . . ? Br1 Cd1 N6 C7 -142.7(3) 3_666 . . . ? N2 N3 C1 C6 180.0(5) . . . . ? Cd1 N3 C1 C6 -0.4(7) . . . . ? N2 N3 C1 C2 0.2(5) . . . . ? Cd1 N3 C1 C2 179.8(3) . . . . ? N2 N1 C2 C1 0.6(5) . . . . ? C13 N1 C2 C1 177.0(4) . . . . ? N2 N1 C2 C3 178.5(5) . . . . ? C13 N1 C2 C3 -5.0(8) . . . . ? N3 C1 C2 N1 -0.5(5) . . . . ? C6 C1 C2 N1 179.7(4) . . . . ? N3 C1 C2 C3 -178.7(4) . . . . ? C6 C1 C2 C3 1.5(7) . . . . ? N1 C2 C3 C4 -180.0(5) . . . . ? C1 C2 C3 C4 -2.3(7) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? C3 C4 C5 C6 0.2(10) . . . . ? C4 C5 C6 C1 -1.1(9) . . . . ? N3 C1 C6 C5 -179.5(5) . . . . ? C2 C1 C6 C5 0.3(8) . . . . ? N5 N6 C7 C8 -0.2(6) . . . . ? Cd1 N6 C7 C8 -177.9(3) . . . . ? N5 N6 C7 C12 -179.9(6) . . . . ? Cd1 N6 C7 C12 2.4(8) . . . . ? N5 N4 C8 C7 -0.5(6) . . . . ? C16 N4 C8 C7 -174.9(5) . . . . ? N5 N4 C8 C9 179.6(6) . . . . ? C16 N4 C8 C9 5.2(10) . . . . ? N6 C7 C8 N4 0.4(6) . . . . ? C12 C7 C8 N4 -179.9(5) . . . . ? N6 C7 C8 C9 -179.7(5) . . . . ? C12 C7 C8 C9 0.0(8) . . . . ? N4 C8 C9 C10 179.1(6) . . . . ? C7 C8 C9 C10 -0.8(8) . . . . ? C8 C9 C10 C11 1.7(10) . . . . ? C9 C10 C11 C12 -2.1(11) . . . . ? C10 C11 C12 C7 1.2(10) . . . . ? N6 C7 C12 C11 179.5(6) . . . . ? C8 C7 C12 C11 -0.2(9) . . . . ? N2 N1 C13 C14 103.6(5) . . . . ? C2 N1 C13 C14 -72.6(6) . . . . ? N1 C13 C14 C15 -58.4(6) . . . 4_576 ? N5 N4 C16 C15 -72.3(6) . . . . ? C8 N4 C16 C15 101.7(6) . . . . ? C14 C15 C16 N4 -178.4(4) 4_575 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.150 # Attachment '06.cif' data_06 _database_code_depnum_ccdc_archive 'CCDC 787192' #TrackingRef '06.cif' #=================================END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Br2 Cd N6' _chemical_formula_sum 'C18 H20 Br2 Cd N6' _chemical_formula_weight 592.61 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 10.2326(11) _cell_length_b 12.4020(17) _cell_length_c 16.713(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.9780(10) _cell_angle_gamma 90.00 _cell_volume 2119.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4443 _cell_measurement_theta_min 2.299 _cell_measurement_theta_max 26.875 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 4.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2369 _exptl_absorpt_correction_T_max 0.3564 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10827 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3732 _reflns_number_gt 2952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0292P)^2^+0.7275P] 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 3732 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.54408(2) 0.63696(2) 1.555074(15) 0.03514(9) Uani 1 1 d . . . Br1 Br 0.55506(4) 0.40261(3) 1.58522(2) 0.04352(12) Uani 1 1 d . . . Br2 Br 0.41848(4) 0.67649(3) 1.67960(2) 0.05191(13) Uani 1 1 d . . . N1 N 0.6590(3) 0.9631(2) 1.46553(17) 0.0409(8) Uani 1 1 d . . . N2 N 0.5984(3) 0.8674(2) 1.45938(18) 0.0403(7) Uani 1 1 d . . . N3 N 0.5995(3) 0.8241(2) 1.53106(19) 0.0412(7) Uani 1 1 d . . . N4 N 0.9547(3) 0.6194(2) 1.62035(17) 0.0352(7) Uani 1 1 d . . . N5 N 0.8262(3) 0.6170(2) 1.63189(18) 0.0374(7) Uani 1 1 d . . . N6 N 0.7651(3) 0.6263(2) 1.56229(18) 0.0356(7) Uani 1 1 d . . . C1 C 0.6631(3) 0.8929(3) 1.5842(2) 0.0389(9) Uani 1 1 d . . . C2 C 0.7017(4) 0.9820(3) 1.5419(2) 0.0409(9) Uani 1 1 d . . . C3 C 0.7712(4) 1.0671(3) 1.5787(3) 0.0631(12) Uani 1 1 d . . . H3 H 0.7985 1.1269 1.5501 0.076 Uiso 1 1 calc R . . C4 C 0.7964(5) 1.0568(4) 1.6594(3) 0.0742(15) Uani 1 1 d . . . H4 H 0.8405 1.1120 1.6865 0.089 Uiso 1 1 calc R . . C5 C 0.7584(5) 0.9666(4) 1.7021(3) 0.0642(13) Uani 1 1 d . . . H5 H 0.7790 0.9632 1.7567 0.077 Uiso 1 1 calc R . . C6 C 0.6924(4) 0.8836(3) 1.6671(2) 0.0504(10) Uani 1 1 d . . . H6 H 0.6676 0.8234 1.6962 0.061 Uiso 1 1 calc R . . C7 C 0.8555(3) 0.6370(3) 1.5043(2) 0.0329(8) Uani 1 1 d . . . C8 C 0.9796(3) 0.6319(3) 1.5413(2) 0.0326(8) Uani 1 1 d . . . C9 C 1.0936(4) 0.6387(3) 1.4986(2) 0.0420(9) Uani 1 1 d . . . H9 H 1.1760 0.6344 1.5236 0.050 Uiso 1 1 calc R . . C10 C 1.0770(4) 0.6523(3) 1.4177(3) 0.0504(10) Uani 1 1 d . . . H10 H 1.1505 0.6579 1.3868 0.060 Uiso 1 1 calc R . . C11 C 0.9522(4) 0.6580(3) 1.3795(2) 0.0512(10) Uani 1 1 d . . . H11 H 0.9460 0.6677 1.3243 0.061 Uiso 1 1 calc R . . C12 C 0.8407(4) 0.6499(3) 1.4209(2) 0.0435(9) Uani 1 1 d . . . H12 H 0.7586 0.6527 1.3954 0.052 Uiso 1 1 calc R . . C13 C 0.6837(4) 1.0251(3) 1.3938(2) 0.0482(10) Uani 1 1 d . . . H13A H 0.6817 1.1013 1.4066 0.058 Uiso 1 1 calc R . . H13B H 0.6146 1.0111 1.3540 0.058 Uiso 1 1 calc R . . C14 C 0.8136(4) 0.9983(3) 1.3588(2) 0.0510(10) Uani 1 1 d . . . H14A H 0.8085 0.9272 1.3348 0.061 Uiso 1 1 calc R . . H14B H 0.8800 0.9961 1.4016 0.061 Uiso 1 1 calc R . . C15 C 0.8545(4) 1.0793(3) 1.2958(2) 0.0508(10) Uani 1 1 d . . . H15A H 0.9224 1.0476 1.2642 0.061 Uiso 1 1 calc R . . H15B H 0.7802 1.0948 1.2601 0.061 Uiso 1 1 calc R . . C16 C 0.9042(4) 1.1827(3) 1.3324(2) 0.0446(9) Uani 1 1 d . . . H16A H 0.9804 1.1668 1.3664 0.053 Uiso 1 1 calc R . . H16B H 0.8375 1.2118 1.3661 0.053 Uiso 1 1 calc R . . C17 C 0.9409(4) 1.2687(3) 1.2723(2) 0.0473(10) Uani 1 1 d . . . H17A H 1.0230 1.2490 1.2490 0.057 Uiso 1 1 calc R . . H17B H 0.8745 1.2711 1.2295 0.057 Uiso 1 1 calc R . . C18 C 1.0455(4) 0.6202(3) 1.6907(2) 0.0447(10) Uani 1 1 d . . . H18A H 1.1308 0.5955 1.6749 0.054 Uiso 1 1 calc R . . H18B H 1.0143 0.5704 1.7305 0.054 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 0.02877(15) 0.04425(17) 0.03262(16) -0.00328(12) 0.00446(11) -0.00592(11) Br1 0.0504(2) 0.0430(2) 0.0366(2) 0.00353(17) -0.00757(17) -0.00833(17) Br2 0.0557(3) 0.0549(3) 0.0466(3) 0.0022(2) 0.0236(2) 0.0028(2) N1 0.051(2) 0.0349(18) 0.0369(19) 0.0028(14) 0.0030(15) -0.0080(14) N2 0.0444(18) 0.0382(18) 0.0384(19) -0.0003(15) 0.0015(14) -0.0071(15) N3 0.0439(19) 0.0393(17) 0.0405(18) 0.0000(15) 0.0045(15) -0.0091(14) N4 0.0314(17) 0.0359(17) 0.0381(18) 0.0032(13) -0.0010(13) -0.0078(13) N5 0.0333(17) 0.0384(18) 0.0406(19) 0.0042(14) 0.0031(14) -0.0081(13) N6 0.0332(16) 0.0378(17) 0.0359(18) 0.0021(14) 0.0009(14) -0.0057(13) C1 0.040(2) 0.039(2) 0.038(2) -0.0043(17) 0.0039(17) -0.0030(16) C2 0.046(2) 0.037(2) 0.039(2) -0.0050(17) 0.0025(18) -0.0052(17) C3 0.083(3) 0.044(3) 0.062(3) -0.007(2) 0.001(3) -0.019(2) C4 0.094(4) 0.063(3) 0.065(3) -0.026(3) -0.013(3) -0.020(3) C5 0.080(3) 0.068(3) 0.043(3) -0.012(2) -0.005(2) -0.003(3) C6 0.064(3) 0.052(3) 0.036(2) -0.0024(19) 0.007(2) -0.005(2) C7 0.0307(19) 0.0303(18) 0.038(2) 0.0012(16) 0.0017(16) -0.0019(15) C8 0.0315(19) 0.0292(18) 0.037(2) 0.0015(16) 0.0015(15) -0.0062(15) C9 0.032(2) 0.039(2) 0.055(3) -0.0028(19) 0.0030(18) -0.0027(16) C10 0.048(3) 0.049(3) 0.055(3) -0.004(2) 0.019(2) -0.0078(19) C11 0.062(3) 0.055(3) 0.037(2) 0.0056(19) 0.011(2) -0.002(2) C12 0.044(2) 0.051(2) 0.035(2) 0.0050(18) -0.0004(18) -0.0024(18) C13 0.056(3) 0.047(2) 0.042(2) 0.0077(19) 0.0029(19) -0.0086(19) C14 0.069(3) 0.041(2) 0.044(2) -0.0057(19) 0.014(2) -0.006(2) C15 0.062(3) 0.049(3) 0.042(2) -0.0068(19) 0.009(2) -0.011(2) C16 0.050(2) 0.045(2) 0.038(2) -0.0003(18) 0.0023(18) -0.0070(18) C17 0.049(2) 0.055(3) 0.037(2) 0.0024(19) -0.0027(18) -0.012(2) C18 0.043(2) 0.049(2) 0.042(2) 0.0133(18) -0.0100(18) -0.0086(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 N6 2.265(3) . ? Cd1 N3 2.426(3) . ? Cd1 Br2 2.5315(5) . ? Cd1 Br1 2.5698(5) 3_668 ? Cd1 Br1 2.9513(6) . ? Br1 Cd1 2.5698(5) 3_668 ? N1 N2 1.341(4) . ? N1 C2 1.355(4) . ? N1 C13 1.455(5) . ? N2 N3 1.313(4) . ? N3 C1 1.378(4) . ? N4 N5 1.336(4) . ? N4 C8 1.363(4) . ? N4 C18 1.474(4) . ? N5 N6 1.307(4) . ? N6 C7 1.369(4) . ? C1 C2 1.378(5) . ? C1 C6 1.413(5) . ? C2 C3 1.403(5) . ? C3 C4 1.370(6) . ? C3 H3 0.9300 . ? C4 C5 1.390(6) . ? C4 H4 0.9300 . ? C5 C6 1.353(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.394(5) . ? C7 C12 1.406(5) . ? C8 C9 1.390(5) . ? C9 C10 1.369(6) . ? C9 H9 0.9300 . ? C10 C11 1.409(6) . ? C10 H10 0.9300 . ? C11 C12 1.359(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.507(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.524(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.502(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.520(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.514(5) 3_778 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C17 1.514(5) 3_778 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? 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 N6 Cd1 N3 79.96(10) . . ? N6 Cd1 Br2 120.13(8) . . ? N3 Cd1 Br2 94.53(8) . . ? N6 Cd1 Br1 113.55(8) . 3_668 ? N3 Cd1 Br1 96.83(7) . 3_668 ? Br2 Cd1 Br1 126.264(18) . 3_668 ? N6 Cd1 Br1 84.35(7) . . ? N3 Cd1 Br1 164.29(7) . . ? Br2 Cd1 Br1 93.887(15) . . ? Br1 Cd1 Br1 88.808(14) 3_668 . ? Cd1 Br1 Cd1 91.192(14) 3_668 . ? N2 N1 C2 111.1(3) . . ? N2 N1 C13 119.9(3) . . ? C2 N1 C13 128.7(3) . . ? N3 N2 N1 107.6(3) . . ? N2 N3 C1 108.9(3) . . ? N2 N3 Cd1 123.2(2) . . ? C1 N3 Cd1 126.4(2) . . ? N5 N4 C8 111.1(3) . . ? N5 N4 C18 118.8(3) . . ? C8 N4 C18 129.7(3) . . ? N6 N5 N4 108.2(3) . . ? N5 N6 C7 108.9(3) . . ? N5 N6 Cd1 119.9(2) . . ? C7 N6 Cd1 130.9(2) . . ? C2 C1 N3 107.7(3) . . ? C2 C1 C6 121.0(3) . . ? N3 C1 C6 131.4(3) . . ? N1 C2 C1 104.8(3) . . ? N1 C2 C3 133.3(4) . . ? C1 C2 C3 121.9(4) . . ? C4 C3 C2 115.9(4) . . ? C4 C3 H3 122.1 . . ? C2 C3 H3 122.1 . . ? C3 C4 C5 122.4(4) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 122.3(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 116.6(4) . . ? C5 C6 H6 121.7 . . ? C1 C6 H6 121.7 . . ? N6 C7 C8 108.0(3) . . ? N6 C7 C12 131.3(3) . . ? C8 C7 C12 120.7(3) . . ? N4 C8 C9 133.8(3) . . ? N4 C8 C7 103.7(3) . . ? C9 C8 C7 122.5(3) . . ? C10 C9 C8 115.9(4) . . ? C10 C9 H9 122.1 . . ? C8 C9 H9 122.1 . . ? C9 C10 C11 122.3(4) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C7 116.7(4) . . ? C11 C12 H12 121.6 . . ? C7 C12 H12 121.6 . . ? N1 C13 C14 112.6(3) . . ? N1 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N1 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 112.9(3) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 112.3(3) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 114.7(3) . . ? C15 C16 H16A 108.6 . . ? C17 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? C17 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 113.0(3) 3_778 . ? C18 C17 H17A 109.0 3_778 . ? C16 C17 H17A 109.0 . . ? C18 C17 H17B 109.0 3_778 . ? C16 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N4 C18 C17 112.2(3) . 3_778 ? N4 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 3_778 . ? N4 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 3_778 . ? H18A C18 H18B 107.9 . . ? 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 N6 Cd1 Br1 Cd1 -113.81(8) . . . 3_668 ? N3 Cd1 Br1 Cd1 -111.4(3) . . . 3_668 ? Br2 Cd1 Br1 Cd1 126.270(18) . . . 3_668 ? Br1 Cd1 Br1 Cd1 0.0 3_668 . . 3_668 ? C2 N1 N2 N3 0.8(4) . . . . ? C13 N1 N2 N3 174.1(3) . . . . ? N1 N2 N3 C1 -0.6(4) . . . . ? N1 N2 N3 Cd1 -167.4(2) . . . . ? N6 Cd1 N3 N2 100.1(3) . . . . ? Br2 Cd1 N3 N2 -140.0(3) . . . . ? Br1 Cd1 N3 N2 -12.7(3) 3_668 . . . ? Br1 Cd1 N3 N2 97.7(3) . . . . ? N6 Cd1 N3 C1 -64.3(3) . . . . ? Br2 Cd1 N3 C1 55.5(3) . . . . ? Br1 Cd1 N3 C1 -177.1(3) 3_668 . . . ? Br1 Cd1 N3 C1 -66.7(5) . . . . ? C8 N4 N5 N6 0.7(4) . . . . ? C18 N4 N5 N6 174.5(3) . . . . ? N4 N5 N6 C7 -1.1(4) . . . . ? N4 N5 N6 Cd1 -176.02(19) . . . . ? N3 Cd1 N6 N5 104.4(2) . . . . ? Br2 Cd1 N6 N5 14.9(3) . . . . ? Br1 Cd1 N6 N5 -162.5(2) 3_668 . . . ? Br1 Cd1 N6 N5 -76.3(2) . . . . ? N3 Cd1 N6 C7 -69.3(3) . . . . ? Br2 Cd1 N6 C7 -158.7(3) . . . . ? Br1 Cd1 N6 C7 23.8(3) 3_668 . . . ? Br1 Cd1 N6 C7 110.0(3) . . . . ? N2 N3 C1 C2 0.1(4) . . . . ? Cd1 N3 C1 C2 166.4(2) . . . . ? N2 N3 C1 C6 -178.7(4) . . . . ? Cd1 N3 C1 C6 -12.4(6) . . . . ? N2 N1 C2 C1 -0.7(4) . . . . ? C13 N1 C2 C1 -173.2(4) . . . . ? N2 N1 C2 C3 178.6(4) . . . . ? C13 N1 C2 C3 6.1(7) . . . . ? N3 C1 C2 N1 0.4(4) . . . . ? C6 C1 C2 N1 179.3(3) . . . . ? N3 C1 C2 C3 -179.0(4) . . . . ? C6 C1 C2 C3 -0.1(6) . . . . ? N1 C2 C3 C4 179.8(4) . . . . ? C1 C2 C3 C4 -1.0(7) . . . . ? C2 C3 C4 C5 1.4(8) . . . . ? C3 C4 C5 C6 -0.9(8) . . . . ? C4 C5 C6 C1 -0.2(7) . . . . ? C2 C1 C6 C5 0.7(6) . . . . ? N3 C1 C6 C5 179.4(4) . . . . ? N5 N6 C7 C8 1.1(4) . . . . ? Cd1 N6 C7 C8 175.3(2) . . . . ? N5 N6 C7 C12 -179.7(4) . . . . ? Cd1 N6 C7 C12 -5.5(6) . . . . ? N5 N4 C8 C9 -179.7(4) . . . . ? C18 N4 C8 C9 7.3(6) . . . . ? N5 N4 C8 C7 0.0(4) . . . . ? C18 N4 C8 C7 -172.9(3) . . . . ? N6 C7 C8 N4 -0.6(4) . . . . ? C12 C7 C8 N4 -180.0(3) . . . . ? N6 C7 C8 C9 179.1(3) . . . . ? C12 C7 C8 C9 -0.2(5) . . . . ? N4 C8 C9 C10 -179.5(4) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C8 C9 C10 C11 -0.5(6) . . . . ? C9 C10 C11 C12 -0.3(6) . . . . ? C10 C11 C12 C7 0.9(6) . . . . ? N6 C7 C12 C11 -179.8(4) . . . . ? C8 C7 C12 C11 -0.7(5) . . . . ? N2 N1 C13 C14 -89.6(4) . . . . ? C2 N1 C13 C14 82.3(5) . . . . ? N1 C13 C14 C15 -166.9(3) . . . . ? C13 C14 C15 C16 76.2(4) . . . . ? C14 C15 C16 C17 -177.4(4) . . . . ? C15 C16 C17 C18 164.2(3) . . . 3_778 ? N5 N4 C18 C17 -79.8(4) . . . 3_778 ? C8 N4 C18 C17 92.7(4) . . . 3_778 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.392 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.076 # Attachment '07.cif' data_07 _database_code_depnum_ccdc_archive 'CCDC 787193' #TrackingRef '07.cif' #=================================END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H80 Cd4 I8 N24' _chemical_formula_sum 'C72 H80 Cd4 I8 N24' _chemical_formula_weight 2746.40 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' I I -0.4742 1.8119 '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' 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 Cc 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' _cell_length_a 16.8129(18) _cell_length_b 57.479(4) _cell_length_c 9.5157(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.3920(10) _cell_angle_gamma 90.00 _cell_volume 9097.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4293 _cell_measurement_theta_min 2.126 _cell_measurement_theta_max 23.337 _exptl_crystal_description sheet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184 _exptl_absorpt_coefficient_mu 3.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3200 _exptl_absorpt_correction_T_max 0.3757 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23754 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -63 _diffrn_reflns_limit_k_max 68 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.02 _reflns_number_total 12293 _reflns_number_gt 6620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0573P)^2^+136.2904P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(9) _refine_ls_number_reflns 12293 _refine_ls_number_parameters 1191 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1780 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 -0.13147(16) 0.31179(4) -0.1567(3) 0.0475(8) Uani 1 1 d . . . Cd2 Cd 0.14779(16) 0.43632(4) 1.3729(3) 0.0485(7) Uani 1 1 d . . . Cd3 Cd 0.65113(16) 0.43664(4) 1.3641(3) 0.0500(8) Uani 1 1 d . . . Cd4 Cd 0.36749(17) 0.31482(4) -0.1667(3) 0.0514(8) Uani 1 1 d . . . I1 I -0.00510(15) 0.43642(3) 1.4184(3) 0.0626(7) Uani 1 1 d . . . I2 I 0.75014(17) 0.41330(4) 1.5653(3) 0.0637(7) Uani 1 1 d . . . I3 I 0.27553(18) 0.42074(5) 1.5519(3) 0.0735(7) Uani 1 1 d . . . I4 I 0.49753(16) 0.44724(5) 1.3796(3) 0.0782(8) Uani 1 1 d . . . I5 I -0.2416(2) 0.33233(5) -0.3516(3) 0.0945(11) Uani 1 1 d . . . I6 I 0.2574(2) 0.33520(5) -0.3585(3) 0.0890(10) Uani 1 1 d . . . I7 I 0.52083(18) 0.30959(6) -0.2023(4) 0.1171(14) Uani 1 1 d . . . I8 I 0.02332(18) 0.30762(6) -0.1910(3) 0.0960(10) Uani 1 1 d . . . N1 N -0.16(3) 0.240(11) -0.10(8) 0.08(7) Uani 0.489(10) 1 d P . 1 N2 N -0.140(5) 0.2623(15) -0.055(9) 0.08(2) Uani 0.489(10) 1 d P . 1 N3 N -0.196(12) 0.276(7) -0.14(5) 0.08(5) Uani 0.489(10) 1 d P . 1 N4 N 0.257(4) 0.2518(11) -0.045(7) 0.084(18) Uani 0.489(10) 1 d P . 1 N5 N 0.270(4) 0.2757(11) -0.053(8) 0.079(18) Uani 0.489(10) 1 d P . 1 N6 N 0.339(8) 0.278(4) -0.12(2) 0.08(4) Uani 0.489(10) 1 d P . 1 N1' N -0.241(4) 0.2480(10) -0.045(6) 0.080(16) Uani 0.511(10) 1 d P . 2 N2' N -0.234(4) 0.2720(10) -0.057(7) 0.079(17) Uani 0.511(10) 1 d P . 2 N3' N -0.167(13) 0.274(6) -0.12(4) 0.08(5) Uani 0.511(10) 1 d P . 2 N4' N 0.33(11) 0.24(3) -0.1(2) 0.08(17) Uani 0.511(10) 1 d P . 2 N5' N 0.354(5) 0.2644(15) -0.057(9) 0.08(2) Uani 0.511(10) 1 d P . 2 N6' N 0.304(8) 0.279(4) -0.14(2) 0.08(4) Uani 0.511(10) 1 d P . 2 N7 N -0.113(2) 0.3544(5) 0.223(3) 0.049(8) Uani 1 1 d . . . N8 N -0.083(2) 0.3424(5) 0.117(4) 0.052(9) Uani 1 1 d . . . N9 N -0.144(2) 0.3311(5) 0.046(4) 0.056(9) Uani 1 1 d . . . N10 N 0.128(2) 0.3947(5) 0.992(4) 0.049(8) Uani 1 1 d . . . N11 N 0.098(2) 0.4055(6) 1.095(4) 0.053(8) Uani 1 1 d . . . N12 N 0.160(2) 0.4185(5) 1.161(3) 0.045(7) Uani 1 1 d . . . N13 N 0.2577(16) 0.5001(4) 1.257(3) 0.053(7) Uani 1 1 d . . . N14 N 0.2464(17) 0.4780(4) 1.266(3) 0.057(7) Uani 1 1 d . . . N15 N 0.1818(19) 0.4743(5) 1.327(4) 0.054(8) Uani 1 1 d . . . N16 N 0.694(2) 0.5085(5) 1.291(4) 0.044(8) Uani 1 1 d . . . N17 N 0.6686(15) 0.4872(4) 1.261(3) 0.046(6) Uani 1 1 d . . . N18 N 0.7133(16) 0.4723(4) 1.348(3) 0.041(7) Uani 1 1 d . . . N19 N 0.624(2) 0.3942(5) 0.986(4) 0.050(8) Uani 1 1 d . . . N20 N 0.601(2) 0.4066(6) 1.082(4) 0.057(9) Uani 1 1 d . . . N21 N 0.6610(19) 0.4180(5) 1.160(4) 0.044(7) Uani 1 1 d . . . N22 N 0.387(2) 0.3589(5) 0.205(3) 0.046(7) Uani 1 1 d . . . N23 N 0.414(2) 0.3464(5) 0.100(4) 0.049(8) Uani 1 1 d . . . N24 N 0.356(2) 0.3351(5) 0.035(4) 0.052(8) Uani 1 1 d . . . C1 C -0.251(5) 0.2632(13) -0.225(8) 0.08(2) Uani 0.489(10) 1 d P . 1 C2 C -0.230(6) 0.2400(14) -0.200(10) 0.08(2) Uani 0.489(10) 1 d P . 1 C3 C -0.277(5) 0.2232(12) -0.278(8) 0.08(2) Uani 0.489(10) 1 d P . 1 H3 H -0.2648 0.2075 -0.2640 0.098 Uiso 0.489(10) 1 calc PR . 1 C4 C -0.340(5) 0.2301(12) -0.378(8) 0.08(2) Uani 0.489(10) 1 d P . 1 H4 H -0.3697 0.2186 -0.4309 0.097 Uiso 0.489(10) 1 d PR . 1 C5 C -0.362(5) 0.2528(12) -0.402(8) 0.08(2) Uani 0.489(10) 1 d P . 1 H5 H -0.4073 0.2557 -0.4694 0.100 Uiso 0.489(10) 1 d PR . 1 C6 C -0.323(4) 0.2717(12) -0.336(7) 0.08(2) Uani 0.489(10) 1 d P . 1 H6 H -0.3377 0.2872 -0.3546 0.097 Uiso 0.489(10) 1 d PR . 1 C7 C 0.369(6) 0.2562(18) -0.145(11) 0.08(3) Uani 0.489(10) 1 d P . 1 C8 C 0.32(15) 0.24(4) -0.1(3) 0.08(15) Uani 0.489(10) 1 d P . 1 C9 C 0.332(6) 0.2164(15) -0.117(10) 0.08(2) Uani 0.489(10) 1 d P . 1 H9 H 0.2979 0.2053 -0.0880 0.099 Uiso 0.489(10) 1 calc PR . 1 C10 C 0.398(15) 0.209(5) -0.18(2) 0.09(5) Uani 0.489(10) 1 d P . 1 H10 H 0.4079 0.1937 -0.1904 0.102 Uiso 0.489(10) 1 calc PR . 1 C11 C 0.450(9) 0.226(3) -0.222(18) 0.08(4) Uani 0.489(10) 1 d P . 1 H11 H 0.4945 0.2210 -0.2618 0.101 Uiso 0.489(10) 1 calc PR . 1 C12 C 0.435(5) 0.2494(12) -0.207(8) 0.08(2) Uani 0.489(10) 1 d P . 1 H12 H 0.4690 0.2604 -0.2373 0.101 Uiso 0.489(10) 1 calc PR . 1 C13 C -0.128(6) 0.2193(17) -0.055(10) 0.08(3) Uani 0.489(10) 1 d P . 1 H13A H -0.1663 0.2067 -0.0733 0.097 Uiso 0.489(10) 1 calc PR . 1 H13B H -0.1079 0.2196 0.0461 0.097 Uiso 0.489(10) 1 calc PR . 1 C14 C -0.058(6) 0.2156(17) -0.140(12) 0.08(3) Uani 0.489(10) 1 d P . 1 H14A H -0.0461 0.1991 -0.1454 0.101 Uiso 0.489(10) 1 calc PR . 1 H14B H -0.0730 0.2213 -0.2363 0.101 Uiso 0.489(10) 1 calc PR . 1 C15 C 0.018(4) 0.2284(11) -0.072(7) 0.08(2) Uani 0.489(10) 1 d P . 1 H15A H 0.0024 0.2417 -0.0206 0.099 Uiso 0.489(10) 1 calc PR . 1 H15B H 0.0489 0.2181 -0.0037 0.099 Uiso 0.489(10) 1 calc PR . 1 C16 C 0.072(4) 0.2366(11) -0.178(7) 0.09(2) Uani 0.489(10) 1 d P . 1 H16A H 0.0562 0.2290 -0.2683 0.104 Uiso 0.489(10) 1 calc PR . 1 H16B H 0.0656 0.2532 -0.1920 0.104 Uiso 0.489(10) 1 calc PR . 1 C17 C 0.161(4) 0.2314(11) -0.126(7) 0.09(2) Uani 0.489(10) 1 d P . 1 H17A H 0.1921 0.2360 -0.1995 0.103 Uiso 0.489(10) 1 calc PR . 1 H17B H 0.1671 0.2147 -0.1124 0.103 Uiso 0.489(10) 1 calc PR . 1 C18 C 0.194(5) 0.2438(12) 0.012(8) 0.08(2) Uani 0.489(10) 1 d P . 1 H18A H 0.1586 0.2560 0.0373 0.099 Uiso 0.489(10) 1 d PR . 1 H18B H 0.2083 0.2332 0.0911 0.099 Uiso 0.489(10) 1 d PR . 1 C1' C -0.134(5) 0.2530(18) -0.149(10) 0.08(2) Uani 0.511(10) 1 d P . 2 C2' C -0.18(4) 0.236(14) -0.10(9) 0.08(8) Uani 0.511(10) 1 d P . 2 C3' C -0.161(6) 0.2129(16) -0.117(10) 0.08(3) Uani 0.511(10) 1 d P . 2 H3' H -0.1920 0.2012 -0.0832 0.097 Uiso 0.511(10) 1 calc PR . 2 C4' C -0.096(7) 0.2072(16) -0.180(11) 0.08(3) Uani 0.511(10) 1 d P . 2 H4' H -0.0841 0.1915 -0.1919 0.095 Uiso 0.511(10) 1 calc PR . 2 C5' C -0.046(6) 0.2236(15) -0.228(10) 0.08(3) Uani 0.511(10) 1 d P . 2 H5' H -0.0019 0.2183 -0.2669 0.098 Uiso 0.511(10) 1 calc PR . 2 C6' C -0.058(4) 0.2472(11) -0.221(7) 0.08(2) Uani 0.511(10) 1 d P . 2 H6' H -0.0248 0.2583 -0.2551 0.097 Uiso 0.511(10) 1 calc PR . 2 C7' C 0.248(5) 0.2668(12) -0.237(8) 0.08(2) Uani 0.511(10) 1 d P . 2 C8' C 0.263(5) 0.2434(13) -0.209(10) 0.08(2) Uani 0.511(10) 1 d P . 2 C9' C 0.216(4) 0.2265(12) -0.287(8) 0.08(2) Uani 0.511(10) 1 d P . 2 H9' H 0.2263 0.2108 -0.2691 0.100 Uiso 0.511(10) 1 calc PR . 2 C10' C 0.155(5) 0.2333(11) -0.393(8) 0.08(2) Uani 0.511(10) 1 d P . 2 H10' H 0.1237 0.2221 -0.4455 0.099 Uiso 0.511(10) 1 calc PR . 2 C11' C 0.140(5) 0.2566(12) -0.421(8) 0.08(2) Uani 0.511(10) 1 d P . 2 H11' H 0.0994 0.2611 -0.4927 0.100 Uiso 0.511(10) 1 d PR . 2 C12' C 0.185(4) 0.2735(12) -0.341(8) 0.08(2) Uani 0.511(10) 1 d P . 2 H12' H 0.1737 0.2892 -0.3563 0.099 Uiso 0.511(10) 1 d PR . 2 C13' C -0.298(5) 0.2364(11) 0.014(8) 0.08(2) Uani 0.511(10) 1 d P . 2 H13C H -0.3140 0.2450 0.0926 0.098 Uiso 0.511(10) 1 d PR . 2 H13D H -0.2788 0.2212 0.0466 0.098 Uiso 0.511(10) 1 d PR . 2 C14' C 0.633(5) 0.2344(12) -0.109(8) 0.09(2) Uani 0.511(10) 1 d P . 2 H14C H 0.6397 0.2206 -0.1638 0.106 Uiso 0.511(10) 1 d PR . 2 H14D H 0.6330 0.2478 -0.1706 0.106 Uiso 0.511(10) 1 d PR . 2 C15' C 0.551(5) 0.2331(11) -0.054(8) 0.09(2) Uani 0.511(10) 1 d P . 2 H15C H 0.5526 0.2206 0.0144 0.106 Uiso 0.511(10) 1 d PR . 2 H15D H 0.5420 0.2476 -0.0063 0.106 Uiso 0.511(10) 1 d PR . 2 C16' C 0.483(8) 0.229(3) -0.175(15) 0.09(3) Uani 0.511(10) 1 d P . 2 H16C H 0.4574 0.2438 -0.2027 0.103 Uiso 0.511(10) 1 calc PR . 2 H16D H 0.5049 0.2229 -0.2562 0.103 Uiso 0.511(10) 1 calc PR . 2 C17' C 0.420(14) 0.212(4) -0.14(2) 0.09(4) Uani 0.511(10) 1 d P . 2 H17C H 0.4465 0.1988 -0.0877 0.103 Uiso 0.511(10) 1 calc PR . 2 H17D H 0.3876 0.2066 -0.2225 0.103 Uiso 0.511(10) 1 calc PR . 2 C18' C 0.364(6) 0.2231(16) -0.041(9) 0.08(2) Uani 0.511(10) 1 d P . 2 H18C H 0.3234 0.2119 -0.0237 0.101 Uiso 0.511(10) 1 calc PR . 2 H18D H 0.3950 0.2272 0.0501 0.101 Uiso 0.511(10) 1 calc PR . 2 C19 C -0.209(3) 0.3352(6) 0.111(4) 0.052(10) Uani 1 1 d . . . C20 C -0.191(3) 0.3510(6) 0.221(4) 0.045(9) Uani 1 1 d . . . C21 C -0.252(3) 0.3591(6) 0.293(4) 0.053(10) Uani 1 1 d . . . H21 H -0.2409 0.3696 0.3674 0.064 Uiso 1 1 calc R . . C22 C -0.330(3) 0.3514(6) 0.251(4) 0.060(10) Uani 1 1 d . . . H22 H -0.3707 0.3561 0.3022 0.072 Uiso 1 1 calc R . . C23 C -0.349(3) 0.3369(6) 0.135(4) 0.061(10) Uani 1 1 d . . . H23 H -0.4016 0.3317 0.1085 0.073 Uiso 1 1 calc R . . C24 C -0.289(3) 0.3304(6) 0.059(5) 0.058(10) Uani 1 1 d . . . H24 H -0.3020 0.3227 -0.0277 0.069 Uiso 1 1 calc R . . C25 C 0.230(3) 0.4136(6) 1.109(4) 0.050(10) Uani 1 1 d . . . C26 C 0.208(3) 0.3982(6) 0.993(5) 0.049(10) Uani 1 1 d . . . C27 C 0.258(3) 0.3907(7) 0.907(5) 0.056(10) Uani 1 1 d . . . H27 H 0.2414 0.3803 0.8335 0.067 Uiso 1 1 calc R . . C28 C 0.334(3) 0.3987(7) 0.931(4) 0.059(10) Uani 1 1 d . . . H28 H 0.3713 0.3937 0.8749 0.071 Uiso 1 1 calc R . . C29 C 0.357(3) 0.4156(6) 1.047(4) 0.062(10) Uani 1 1 d . . . H29 H 0.4098 0.4208 1.0610 0.074 Uiso 1 1 calc R . . C30 C 0.310(3) 0.4238(6) 1.129(4) 0.054(10) Uani 1 1 d . . . H30 H 0.3258 0.4352 1.1966 0.065 Uiso 1 1 calc R . . C31 C -0.050(3) 0.3678(6) 0.324(4) 0.051(9) Uani 1 1 d . . . H31A H -0.0068 0.3727 0.2734 0.061 Uiso 1 1 calc R . . H31B H -0.0743 0.3816 0.3582 0.061 Uiso 1 1 calc R . . C32 C -0.017(2) 0.3523(6) 0.448(4) 0.045(9) Uani 1 1 d . . . H32A H 0.0154 0.3400 0.4159 0.054 Uiso 1 1 calc R . . H32B H -0.0610 0.3452 0.4880 0.054 Uiso 1 1 calc R . . C33 C 0.034(2) 0.3666(6) 0.563(4) 0.044(9) Uani 1 1 d . . . H33A H 0.0660 0.3777 0.5176 0.053 Uiso 1 1 calc R . . H33B H 0.0714 0.3563 0.6206 0.053 Uiso 1 1 calc R . . C34 C -0.016(2) 0.3799(6) 0.661(4) 0.049(10) Uani 1 1 d . . . H34A H -0.0538 0.3902 0.6033 0.059 Uiso 1 1 calc R . . H34B H -0.0473 0.3689 0.7074 0.059 Uiso 1 1 calc R . . C35 C 0.036(3) 0.3939(6) 0.771(4) 0.052(10) Uani 1 1 d . . . H35A H 0.0755 0.4021 0.7248 0.062 Uiso 1 1 calc R . . H35B H 0.0027 0.4055 0.8083 0.062 Uiso 1 1 calc R . . C36 C 0.077(3) 0.3807(6) 0.886(4) 0.050(9) Uani 1 1 d . . . H36A H 0.1094 0.3690 0.8484 0.060 Uiso 1 1 calc R . . H36B H 0.0370 0.3727 0.9327 0.060 Uiso 1 1 calc R . . C37 C 0.1494(18) 0.4951(4) 1.356(3) 0.046(8) Uani 1 1 d . . . C38 C 0.201(3) 0.5120(6) 1.310(5) 0.053(10) Uani 1 1 d . . . C39 C 0.182(2) 0.5364(5) 1.325(4) 0.057(9) Uani 1 1 d . . . H39 H 0.2139 0.5480 1.2947 0.068 Uiso 1 1 calc R . . C40 C 0.118(2) 0.5416(5) 1.383(4) 0.057(10) Uani 1 1 d . . . H40 H 0.1037 0.5571 1.3912 0.068 Uiso 1 1 calc R . . C41 C 0.067(2) 0.5233(5) 1.438(4) 0.060(11) Uani 1 1 d . . . H41 H 0.0237 0.5274 1.4835 0.072 Uiso 1 1 calc R . . C42 C 0.0847(18) 0.5001(5) 1.419(3) 0.052(8) Uani 1 1 d . . . H42 H 0.0530 0.4883 1.4482 0.062 Uiso 1 1 calc R . . C43 C 0.7713(17) 0.4847(5) 1.430(3) 0.041(7) Uani 1 1 d . . . C44 C 0.7559(18) 0.5077(5) 1.394(3) 0.041(7) Uani 1 1 d . . . C45 C 0.8049(18) 0.5254(5) 1.463(3) 0.049(7) Uani 1 1 d . . . H45 H 0.7969 0.5411 1.4438 0.059 Uiso 1 1 calc R . . C46 C 0.8646(18) 0.5171(5) 1.561(3) 0.052(8) Uani 1 1 d . . . H46 H 0.8993 0.5281 1.6078 0.062 Uiso 1 1 calc R . . C47 C 0.8798(18) 0.4944(5) 1.598(3) 0.055(8) Uani 1 1 d . . . H47 H 0.9224 0.4906 1.6682 0.066 Uiso 1 1 calc R . . C48 C 0.8300(17) 0.4772(5) 1.530(3) 0.048(7) Uani 1 1 d . . . H48 H 0.8372 0.4615 1.5520 0.057 Uiso 1 1 calc R . . C49 C 0.3305(19) 0.5089(5) 1.205(4) 0.060(9) Uani 1 1 d . . . H49A H 0.3168 0.5226 1.1472 0.072 Uiso 1 1 calc R . . H49B H 0.3503 0.4972 1.1457 0.072 Uiso 1 1 calc R . . C50 C 0.3951(18) 0.5149(5) 1.322(3) 0.056(8) Uani 1 1 d . . . H50A H 0.4108 0.5012 1.3787 0.067 Uiso 1 1 calc R . . H50B H 0.3754 0.5264 1.3839 0.067 Uiso 1 1 calc R . . C51 C 0.4674(19) 0.5247(5) 1.264(4) 0.064(9) Uani 1 1 d . . . H51A H 0.4531 0.5391 1.2137 0.077 Uiso 1 1 calc R . . H51B H 0.4852 0.5137 1.1972 0.077 Uiso 1 1 calc R . . C52 C 0.535(2) 0.5290(5) 1.386(4) 0.056(9) Uani 1 1 d . . . H52A H 0.5536 0.5144 1.4301 0.068 Uiso 1 1 calc R . . H52B H 0.5162 0.5389 1.4571 0.068 Uiso 1 1 calc R . . C53 C 0.606(2) 0.5418(6) 1.314(4) 0.062(10) Uani 1 1 d . . . H53A H 0.5823 0.5551 1.2602 0.075 Uiso 1 1 calc R . . H53B H 0.6449 0.5479 1.3905 0.075 Uiso 1 1 calc R . . C54 C 0.6506(19) 0.5281(5) 1.220(3) 0.055(8) Uani 1 1 d . . . H54A H 0.6130 0.5223 1.1402 0.066 Uiso 1 1 calc R . . H54B H 0.6885 0.5382 1.1817 0.066 Uiso 1 1 calc R . . C55 C 0.733(2) 0.4107(6) 1.111(4) 0.045(9) Uani 1 1 d . . . C56 C 0.711(3) 0.3957(6) 0.999(5) 0.050(10) Uani 1 1 d . . . C57 C 0.759(2) 0.3864(6) 0.913(4) 0.048(9) Uani 1 1 d . . . H57 H 0.7395 0.3772 0.8355 0.057 Uiso 1 1 calc R . . C58 C 0.840(2) 0.3916(6) 0.949(4) 0.052(9) Uani 1 1 d . . . H58 H 0.8778 0.3851 0.8993 0.062 Uiso 1 1 calc R . . C59 C 0.862(2) 0.4068(6) 1.060(4) 0.055(10) Uani 1 1 d . . . H59 H 0.9167 0.4094 1.0848 0.066 Uiso 1 1 calc R . . C60 C 0.812(3) 0.4188(6) 1.140(4) 0.051(10) Uani 1 1 d . . . H60 H 0.8291 0.4306 1.2044 0.061 Uiso 1 1 calc R . . C61 C 0.290(2) 0.3382(6) 0.101(4) 0.047(9) Uani 1 1 d . . . C62 C 0.312(3) 0.3535(6) 0.212(5) 0.050(10) Uani 1 1 d . . . C63 C 0.245(3) 0.3615(7) 0.288(5) 0.056(10) Uani 1 1 d . . . H63 H 0.2557 0.3720 0.3627 0.068 Uiso 1 1 calc R . . C64 C 0.170(3) 0.3538(6) 0.248(4) 0.055(9) Uani 1 1 d . . . H64 H 0.1291 0.3591 0.2959 0.066 Uiso 1 1 calc R . . C65 C 0.152(3) 0.3380(6) 0.137(4) 0.056(10) Uani 1 1 d . . . H65 H 0.1003 0.3323 0.1144 0.068 Uiso 1 1 calc R . . C66 C 0.214(3) 0.3307(6) 0.060(5) 0.056(10) Uani 1 1 d . . . H66 H 0.2015 0.3210 -0.0186 0.067 Uiso 1 1 calc R . . C67 C 0.576(3) 0.3812(6) 0.879(5) 0.060(11) Uani 1 1 d . . . H67A H 0.5341 0.3732 0.9213 0.072 Uiso 1 1 calc R . . H67B H 0.6083 0.3696 0.8409 0.072 Uiso 1 1 calc R . . C68 C 0.538(3) 0.3965(7) 0.763(5) 0.058(11) Uani 1 1 d . . . H68A H 0.5798 0.4050 0.7253 0.070 Uiso 1 1 calc R . . H68B H 0.5046 0.4079 0.8030 0.070 Uiso 1 1 calc R . . C69 C 0.484(3) 0.3838(7) 0.635(5) 0.063(12) Uani 1 1 d . . . H69A H 0.4458 0.3737 0.6730 0.076 Uiso 1 1 calc R . . H69B H 0.4527 0.3954 0.5763 0.076 Uiso 1 1 calc R . . C70 C 0.530(3) 0.3700(7) 0.546(4) 0.057(11) Uani 1 1 d . . . H70A H 0.5641 0.3592 0.6057 0.069 Uiso 1 1 calc R . . H70B H 0.5650 0.3804 0.5021 0.069 Uiso 1 1 calc R . . C71 C 0.481(3) 0.3566(6) 0.433(4) 0.057(11) Uani 1 1 d . . . H71A H 0.4369 0.3492 0.4712 0.068 Uiso 1 1 calc R . . H71B H 0.5134 0.3445 0.3990 0.068 Uiso 1 1 calc R . . C72 C 0.446(3) 0.3726(6) 0.304(4) 0.056(10) Uani 1 1 d . . . H72A H 0.4191 0.3860 0.3377 0.067 Uiso 1 1 calc R . . H72B H 0.4887 0.3781 0.2545 0.067 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 0.0532(19) 0.0426(13) 0.0449(18) -0.0094(11) 0.0005(14) 0.0009(11) Cd2 0.0487(19) 0.0474(13) 0.0488(18) -0.0099(11) 0.0052(14) 0.0026(11) Cd3 0.0521(19) 0.0447(13) 0.0510(19) -0.0108(12) 0.0007(15) -0.0028(11) Cd4 0.053(2) 0.0439(13) 0.056(2) -0.0129(12) 0.0009(15) 0.0031(12) I1 0.0540(14) 0.0476(10) 0.0878(17) 0.0042(10) 0.0156(12) -0.0070(9) I2 0.0772(16) 0.0527(12) 0.0615(15) 0.0084(11) 0.0113(12) 0.0028(10) I3 0.0709(16) 0.0828(16) 0.0616(16) -0.0137(12) -0.0079(12) 0.0194(12) I4 0.0454(14) 0.0826(15) 0.105(2) -0.0331(14) 0.0043(13) -0.0010(12) I5 0.121(3) 0.0985(19) 0.0548(16) -0.0084(14) -0.0175(15) 0.0492(17) I6 0.106(2) 0.0958(19) 0.0582(16) -0.0117(13) -0.0134(14) 0.0453(16) I7 0.0517(17) 0.154(3) 0.141(3) -0.071(2) 0.0005(17) 0.0044(16) I8 0.0540(17) 0.130(2) 0.103(2) -0.0355(17) 0.0086(15) -0.0083(14) N1 0.1(2) 0.1(2) 0.09(8) 0.00(12) 0.02(15) 0.00(11) N2 0.09(6) 0.06(5) 0.08(6) 0.00(4) 0.02(4) -0.01(4) N3 0.09(14) 0.06(7) 0.08(9) 0.00(6) 0.01(14) -0.01(12) N4 0.09(5) 0.07(4) 0.09(5) -0.01(4) 0.01(4) 0.00(4) N5 0.08(5) 0.07(4) 0.08(5) -0.01(3) 0.01(4) -0.01(3) N6 0.09(9) 0.07(6) 0.08(10) -0.01(6) 0.01(8) 0.00(9) N1' 0.09(5) 0.07(4) 0.09(5) -0.01(3) 0.02(4) -0.01(3) N2' 0.09(5) 0.06(4) 0.08(5) -0.01(3) 0.02(4) -0.01(3) N3' 0.09(13) 0.06(8) 0.09(11) -0.01(7) 0.02(14) -0.01(12) N4' 0.1(4) 0.1(3) 0.09(13) -0.01(19) 0.0(2) 0.0(2) N5' 0.09(6) 0.07(5) 0.09(6) -0.01(4) 0.01(5) -0.01(5) N6' 0.09(10) 0.07(5) 0.08(8) -0.01(5) 0.01(8) -0.01(8) N7 0.06(2) 0.048(16) 0.032(18) -0.006(13) -0.002(16) 0.001(15) N8 0.06(2) 0.048(16) 0.046(19) -0.015(14) 0.007(17) 0.000(15) N9 0.07(3) 0.051(17) 0.05(2) -0.008(14) 0.004(19) -0.006(15) N10 0.05(2) 0.053(16) 0.039(18) -0.006(13) -0.008(15) 0.001(13) N11 0.05(2) 0.062(18) 0.045(19) -0.007(14) -0.001(16) -0.005(14) N12 0.043(19) 0.051(15) 0.040(18) -0.018(12) 0.004(14) 0.000(13) N13 0.053(18) 0.045(15) 0.065(19) 0.002(13) 0.018(15) -0.004(12) N14 0.055(19) 0.053(16) 0.07(2) -0.005(13) 0.017(15) 0.003(13) N15 0.05(2) 0.042(14) 0.07(2) 0.004(14) 0.014(17) -0.001(13) N16 0.042(18) 0.042(16) 0.052(19) 0.004(13) 0.020(16) -0.008(13) N17 0.046(16) 0.043(15) 0.051(17) 0.001(12) 0.005(13) -0.008(12) N18 0.034(17) 0.040(13) 0.047(17) -0.006(12) 0.003(14) -0.010(12) N19 0.042(19) 0.061(17) 0.045(19) -0.008(14) -0.004(15) 0.000(14) N20 0.05(2) 0.062(18) 0.05(2) -0.009(15) -0.005(16) -0.001(15) N21 0.035(18) 0.052(15) 0.044(18) -0.009(12) -0.001(14) -0.005(12) N22 0.044(19) 0.052(15) 0.040(18) -0.011(12) 0.002(14) -0.001(12) N23 0.044(19) 0.056(16) 0.044(17) -0.017(13) -0.002(14) 0.002(13) N24 0.05(2) 0.052(15) 0.05(2) -0.012(13) 0.003(16) -0.005(14) C1 0.09(6) 0.06(5) 0.08(6) -0.01(4) 0.02(5) -0.01(4) C2 0.09(6) 0.06(5) 0.09(6) -0.01(5) 0.02(5) 0.00(4) C3 0.09(6) 0.07(4) 0.09(5) -0.01(4) 0.02(5) -0.01(4) C4 0.09(6) 0.07(5) 0.09(5) -0.01(4) 0.02(4) -0.01(4) C5 0.09(6) 0.07(5) 0.09(6) -0.01(4) 0.01(5) -0.01(4) C6 0.09(6) 0.07(4) 0.09(5) 0.00(4) 0.02(5) 0.00(4) C7 0.09(7) 0.07(6) 0.09(7) -0.01(5) 0.01(6) 0.00(5) C8 0.1(4) 0.1(4) 0.09(17) 0.0(2) 0.0(2) 0.0(3) C9 0.09(7) 0.07(6) 0.09(7) -0.01(4) 0.01(6) 0.00(5) C10 0.09(12) 0.07(7) 0.09(11) -0.02(7) 0.00(8) 0.00(7) C11 0.09(11) 0.07(7) 0.09(11) -0.02(7) 0.01(7) 0.00(7) C12 0.09(6) 0.07(5) 0.09(6) -0.02(4) 0.01(5) 0.00(4) C13 0.09(8) 0.07(6) 0.09(7) -0.01(5) 0.02(6) -0.01(5) C14 0.10(8) 0.07(7) 0.09(7) -0.01(5) 0.01(6) 0.00(5) C15 0.09(6) 0.07(4) 0.09(5) 0.00(4) 0.02(4) 0.00(4) C16 0.09(6) 0.07(4) 0.09(5) -0.01(4) 0.01(4) -0.01(4) C17 0.09(6) 0.07(4) 0.09(5) -0.01(4) 0.01(4) -0.01(4) C18 0.09(6) 0.07(5) 0.09(6) -0.01(4) 0.01(5) 0.00(4) C1' 0.09(6) 0.07(6) 0.09(7) -0.01(5) 0.02(5) -0.01(5) C2' 0.1(3) 0.07(18) 0.09(12) 0.00(12) 0.02(18) -0.01(14) C3' 0.09(8) 0.07(6) 0.09(7) -0.01(4) 0.02(6) -0.01(5) C4' 0.09(8) 0.06(5) 0.09(7) -0.01(4) 0.02(6) -0.01(4) C5' 0.09(7) 0.07(5) 0.09(7) -0.01(4) 0.02(6) -0.01(4) C6' 0.09(5) 0.07(4) 0.09(5) -0.01(4) 0.02(4) -0.01(3) C7' 0.09(6) 0.07(5) 0.09(5) -0.01(4) 0.01(4) 0.00(4) C8' 0.09(6) 0.07(5) 0.09(6) -0.01(4) 0.01(5) -0.01(4) C9' 0.09(6) 0.07(4) 0.09(5) -0.01(4) 0.01(4) -0.01(4) C10' 0.09(5) 0.07(4) 0.09(5) -0.02(4) 0.01(4) -0.01(4) C11' 0.09(6) 0.07(5) 0.09(5) -0.01(4) 0.01(4) -0.01(4) C12' 0.09(6) 0.07(4) 0.09(5) -0.01(4) 0.01(4) -0.01(4) C13' 0.09(6) 0.07(4) 0.09(5) 0.00(4) 0.02(5) -0.01(4) C14' 0.09(6) 0.08(5) 0.09(6) -0.02(4) 0.01(5) 0.00(4) C15' 0.09(6) 0.08(4) 0.09(5) -0.01(4) 0.01(4) 0.00(4) C16' 0.09(10) 0.07(6) 0.09(9) -0.02(6) 0.01(6) 0.00(6) C17' 0.09(12) 0.07(7) 0.09(13) -0.01(7) 0.01(8) 0.00(6) C18' 0.09(7) 0.07(6) 0.09(6) -0.01(5) 0.01(5) 0.00(5) C19 0.06(3) 0.055(19) 0.036(19) -0.004(15) 0.005(18) -0.001(17) C20 0.06(3) 0.042(17) 0.03(2) -0.002(14) 0.004(18) -0.002(16) C21 0.07(3) 0.056(19) 0.04(2) -0.007(15) 0.005(17) 0.002(17) C22 0.07(3) 0.07(2) 0.05(2) -0.003(16) 0.012(18) 0.005(17) C23 0.07(2) 0.057(19) 0.05(2) 0.000(15) -0.001(18) -0.011(16) C24 0.07(3) 0.06(2) 0.05(2) -0.005(15) -0.001(19) -0.006(17) C25 0.05(2) 0.06(2) 0.04(2) -0.006(16) 0.004(18) 0.003(16) C26 0.05(3) 0.05(2) 0.04(2) -0.005(17) -0.002(19) 0.004(17) C27 0.06(2) 0.06(2) 0.05(2) -0.009(16) -0.001(17) 0.006(16) C28 0.06(2) 0.07(2) 0.05(2) -0.002(16) 0.008(18) 0.009(17) C29 0.06(2) 0.07(2) 0.06(2) -0.004(17) 0.000(18) 0.005(17) C30 0.05(2) 0.06(2) 0.04(2) -0.006(16) 0.006(17) 0.000(16) C31 0.06(2) 0.044(18) 0.04(2) -0.011(16) -0.001(18) -0.006(16) C32 0.06(2) 0.036(16) 0.04(2) -0.004(14) -0.002(18) -0.004(15) C33 0.04(2) 0.041(17) 0.04(2) -0.008(14) -0.007(17) -0.004(14) C34 0.05(2) 0.049(19) 0.04(2) -0.006(16) -0.004(18) -0.008(16) C35 0.06(3) 0.05(2) 0.04(2) -0.012(17) -0.007(19) -0.002(17) C36 0.05(2) 0.053(18) 0.04(2) -0.008(15) -0.007(17) -0.007(15) C37 0.05(2) 0.031(14) 0.06(2) -0.001(14) 0.018(17) -0.005(13) C38 0.05(3) 0.043(19) 0.06(3) 0.005(17) 0.02(2) -0.003(16) C39 0.06(2) 0.043(17) 0.07(2) -0.005(16) 0.014(19) -0.009(15) C40 0.05(2) 0.036(16) 0.08(3) -0.010(17) 0.01(2) -0.002(15) C41 0.06(3) 0.044(18) 0.08(3) -0.003(17) 0.02(2) -0.004(16) C42 0.05(2) 0.039(16) 0.07(2) -0.010(15) 0.020(16) -0.003(13) C43 0.036(17) 0.040(16) 0.047(19) -0.011(13) 0.008(14) -0.012(13) C44 0.037(18) 0.042(17) 0.048(18) -0.005(13) 0.018(15) -0.005(12) C45 0.042(17) 0.046(16) 0.060(19) -0.009(14) 0.011(15) -0.011(13) C46 0.046(19) 0.050(17) 0.060(19) -0.019(14) 0.010(15) -0.016(14) C47 0.041(18) 0.06(2) 0.06(2) -0.013(16) -0.004(15) -0.007(14) C48 0.042(18) 0.046(16) 0.055(19) -0.015(14) 0.006(15) -0.005(13) C49 0.06(2) 0.058(19) 0.07(2) 0.005(16) 0.022(19) -0.003(15) C50 0.05(2) 0.053(17) 0.07(2) 0.012(15) 0.020(17) -0.002(14) C51 0.06(2) 0.062(19) 0.08(2) 0.011(15) 0.019(17) -0.011(14) C52 0.05(2) 0.049(17) 0.07(3) 0.016(16) 0.011(18) -0.005(14) C53 0.06(2) 0.053(18) 0.08(3) 0.008(17) 0.01(2) -0.008(15) C54 0.05(2) 0.049(17) 0.07(2) 0.004(15) 0.011(16) -0.009(14) C55 0.04(2) 0.051(18) 0.04(2) -0.003(15) -0.003(15) -0.001(14) C56 0.04(2) 0.06(2) 0.05(2) -0.004(17) -0.003(18) 0.001(17) C57 0.045(19) 0.052(19) 0.04(2) -0.004(14) -0.001(15) -0.008(14) C58 0.05(2) 0.06(2) 0.044(19) 0.002(16) 0.007(15) -0.006(16) C59 0.05(2) 0.057(19) 0.06(2) 0.006(17) -0.004(17) -0.008(15) C60 0.05(2) 0.06(2) 0.05(2) -0.001(16) -0.005(17) -0.003(16) C61 0.05(2) 0.050(19) 0.04(2) -0.008(15) 0.001(18) 0.001(15) C62 0.05(3) 0.06(2) 0.04(2) -0.010(17) -0.003(19) 0.001(17) C63 0.05(2) 0.07(2) 0.05(2) -0.015(16) 0.002(18) 0.007(17) C64 0.05(2) 0.07(2) 0.04(2) -0.011(15) 0.013(17) 0.001(15) C65 0.05(2) 0.063(19) 0.06(2) -0.007(15) 0.002(17) 0.005(14) C66 0.06(2) 0.06(2) 0.05(2) -0.007(16) 0.009(18) -0.004(16) C67 0.05(2) 0.07(2) 0.06(3) -0.012(18) -0.004(19) -0.003(17) C68 0.06(3) 0.07(2) 0.05(3) -0.006(18) 0.00(2) -0.004(18) C69 0.05(3) 0.08(2) 0.06(2) -0.017(19) -0.01(2) 0.004(19) C70 0.05(3) 0.07(2) 0.05(2) -0.014(18) 0.006(19) -0.007(18) C71 0.06(3) 0.07(2) 0.05(3) -0.014(19) 0.00(2) -0.006(19) C72 0.05(2) 0.06(2) 0.05(2) -0.016(16) 0.000(17) -0.007(16) _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' 2.3(4) . ? Cd1 N9 2.26(3) . ? Cd1 N3 2.3(4) . ? Cd1 I8 2.680(4) . ? Cd1 I5 2.694(4) . ? Cd2 N12 2.30(3) . ? Cd2 N15 2.31(3) . ? Cd2 I1 2.668(4) . ? Cd2 I3 2.692(4) . ? Cd3 N21 2.25(3) . ? Cd3 N18 2.32(2) . ? Cd3 I4 2.678(4) . ? Cd3 I2 2.703(4) . ? Cd4 N6 2.2(2) . ? Cd4 N24 2.28(3) . ? Cd4 N6' 2.3(2) . ? Cd4 I7 2.666(5) . ? Cd4 I6 2.672(4) . ? N1 C13 1.4(7) . ? N1 N2 1.4(5) . ? N1 C2 1.4(6) . ? N2 N3 1.4(4) . ? N3 C1 1.4(4) . ? N4 C18 1.35(9) . ? N4 C8 1(3) . ? N4 N5 1.39(8) . ? N5 N6 1.4(2) . ? N6 C7 1.4(2) . ? N1' C13' 1.35(8) . ? N1' C2' 1.4(9) . ? N1' N2' 1.39(7) . ? N2' N3' 1.4(4) . ? N3' C1' 1.4(3) . ? N4' C18' 1(2) . ? N4' N5' 1.4(16) . ? N4' C8' 1(2) . ? N5' N6' 1.4(2) . ? N6' C7' 1.39(17) . ? N7 C20 1.32(5) . ? N7 N8 1.37(5) . ? N7 C31 1.53(5) . ? N8 N9 1.31(5) . ? N9 C19 1.35(5) . ? N10 N11 1.32(5) . ? N10 C26 1.35(5) . ? N10 C36 1.47(5) . ? N11 N12 1.36(5) . ? N12 C25 1.38(5) . ? N13 N14 1.29(3) . ? N13 C38 1.33(5) . ? N13 C49 1.47(4) . ? N14 N15 1.32(4) . ? N15 C37 1.36(4) . ? N16 N17 1.32(3) . ? N16 C44 1.32(4) . ? N16 C54 1.46(4) . ? N17 N18 1.34(3) . ? N18 C43 1.36(4) . ? N19 N20 1.27(5) . ? N19 C67 1.42(5) . ? N19 C56 1.44(5) . ? N20 N21 1.34(5) . ? N21 C55 1.42(5) . ? N22 C62 1.32(5) . ? N22 N23 1.37(4) . ? N22 C72 1.48(5) . ? N23 N24 1.25(4) . ? N24 C61 1.36(5) . ? C1 C2 1.39(10) . ? C1 C6 1.58(10) . ? C2 C3 1.39(9) . ? C3 C4 1.38(9) . ? C3 H3 0.9300 . ? C4 C5 1.37(9) . ? C4 C18 1.96(10) 4_454 ? C4 H4 0.9300 . ? C5 C18 1.34(10) 4_454 ? C5 C6 1.37(8) . ? C5 H5 0.9300 . ? C6 C18 1.75(10) 4_454 ? C6 H6 0.9300 . ? C7 C12 1.38(12) . ? C7 C8 1(2) . ? C8 C9 1(3) . ? C9 C10 1.4(3) . ? C9 H9 0.9300 . ? C10 C11 1.4(4) . ? C10 H10 0.9300 . ? C11 C12 1.39(17) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.54(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.53(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.53(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.52(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.53(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C5 1.34(10) 4 ? C18 C6 1.75(10) 4 ? C18 C4 1.96(10) 4 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C1' C2' 1.4(6) . ? C1' C6' 1.58(11) . ? C2' C3' 1.4(9) . ? C3' C4' 1.38(14) . ? C3' H3' 0.9300 . ? C4' C5' 1.38(14) . ? C4' H4' 0.9300 . ? C5' C6' 1.37(10) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? C7' C8' 1.39(9) . ? C7' C12' 1.39(9) . ? C8' C9' 1.39(9) . ? C9' C10' 1.39(9) . ? C9' H9' 0.9300 . ? C10' C11' 1.38(8) . ? C10' H10' 0.9300 . ? C11' C13' 1.35(9) 4_554 ? C11' C12' 1.39(9) . ? C11' C14' 1.85(10) 4_454 ? C11' C15' 1.90(10) 4_454 ? C11' H11' 0.9300 . ? C12' C13' 1.56(9) 4_554 ? C12' H12' 0.9300 . ? C13' C11' 1.35(9) 4_455 ? C13' C14' 1.53(9) 1_455 ? C13' C12' 1.56(9) 4_455 ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' C13' 1.53(9) 1_655 ? C14' C15' 1.53(9) . ? C14' C11' 1.85(10) 4 ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16' 1.52(11) . ? C15' C11' 1.90(10) 4 ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16' C17' 1.5(3) . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C17' C18' 1.5(3) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19 C24 1.39(6) . ? C19 C20 1.39(6) . ? C20 C21 1.39(6) . ? C21 C22 1.39(6) . ? C21 H21 0.9300 . ? C22 C23 1.38(5) . ? C22 H22 0.9300 . ? C23 C24 1.38(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.43(6) . ? C25 C30 1.45(6) . ? C26 C27 1.33(6) . ? C27 C28 1.34(6) . ? C27 H27 0.9300 . ? C28 C29 1.48(6) . ? C28 H28 0.9300 . ? C29 C30 1.28(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.52(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.53(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.55(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.50(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.43(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C42 1.34(4) . ? C37 C38 1.41(5) . ? C38 C39 1.45(4) . ? C39 C40 1.31(5) . ? C39 H39 0.9300 . ? C40 C41 1.50(5) . ? C40 H40 0.9300 . ? C41 C42 1.38(4) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.34(4) . ? C43 C44 1.38(4) . ? C44 C45 1.41(4) . ? C45 C46 1.35(4) . ? C45 H45 0.9300 . ? C46 C47 1.37(4) . ? C46 H46 0.9300 . ? C47 C48 1.40(4) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.48(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.52(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.52(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.64(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.48(5) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.38(6) . ? C55 C60 1.40(6) . ? C56 C57 1.34(6) . ? C57 C58 1.38(5) . ? C57 H57 0.9300 . ? C58 C59 1.38(5) . ? C58 H58 0.9300 . ? C59 C60 1.39(6) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C66 1.36(6) . ? C61 C62 1.39(6) . ? C62 C63 1.49(6) . ? C63 C64 1.34(6) . ? C63 H63 0.9300 . ? C64 C65 1.39(5) . ? C64 H64 0.9300 . ? C65 C66 1.42(6) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.48(6) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.59(6) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.47(3) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.47(6) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.58(6) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? 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 106(10) . . ? N3' Cd1 N3 12(9) . . ? N9 Cd1 N3 105(10) . . ? N3' Cd1 I8 102(6) . . ? N9 Cd1 I8 111.1(10) . . ? N3 Cd1 I8 114(6) . . ? N3' Cd1 I5 110(7) . . ? N9 Cd1 I5 103.4(9) . . ? N3 Cd1 I5 99(8) . . ? I8 Cd1 I5 122.51(17) . . ? N12 Cd2 N15 101.5(12) . . ? N12 Cd2 I1 110.6(9) . . ? N15 Cd2 I1 107.4(8) . . ? N12 Cd2 I3 104.2(8) . . ? N15 Cd2 I3 103.7(8) . . ? I1 Cd2 I3 126.61(16) . . ? N21 Cd3 N18 105.8(11) . . ? N21 Cd3 I4 110.5(8) . . ? N18 Cd3 I4 104.5(7) . . ? N21 Cd3 I2 105.1(8) . . ? N18 Cd3 I2 104.4(7) . . ? I4 Cd3 I2 124.98(17) . . ? N6 Cd4 N24 105(5) . . ? N6 Cd4 N6' 15(4) . . ? N24 Cd4 N6' 106(5) . . ? N6 Cd4 I7 99(4) . . ? N24 Cd4 I7 111.6(9) . . ? N6' Cd4 I7 112(4) . . ? N6 Cd4 I6 114(3) . . ? N24 Cd4 I6 102.4(9) . . ? N6' Cd4 I6 100(4) . . ? I7 Cd4 I6 123.28(18) . . ? C13 N1 N2 130(10) . . ? C13 N1 C2 119(10) . . ? N2 N1 C2 111(10) . . ? N1 N2 N3 104(10) . . ? C1 N3 N2 111(10) . . ? C1 N3 Cd1 135(10) . . ? N2 N3 Cd1 106(10) . . ? C18 N4 C8 130(10) . . ? C18 N4 N5 120(7) . . ? C8 N4 N5 110(10) . . ? N6 N5 N4 105(10) . . ? N5 N6 C7 111(10) . . ? N5 N6 Cd4 113(10) . . ? C7 N6 Cd4 135(10) . . ? C13' N1' C2' 120(10) . . ? C13' N1' N2' 127(7) . . ? C2' N1' N2' 113(10) . . ? N3' N2' N1' 103(10) . . ? N2' N3' C1' 111(10) . . ? N2' N3' Cd1 114(10) . . ? C1' N3' Cd1 134(10) . . ? C18' N4' N5' 121(10) . . ? C18' N4' C8' 128(10) . . ? N5' N4' C8' 111(10) . . ? N6' N5' N4' 104(10) . . ? N5' N6' C7' 111(10) . . ? N5' N6' Cd4 110(8) . . ? C7' N6' Cd4 132(10) . . ? C20 N7 N8 113(3) . . ? C20 N7 C31 132(3) . . ? N8 N7 C31 115(3) . . ? N9 N8 N7 107(3) . . ? N8 N9 C19 107(3) . . ? N8 N9 Cd1 122(3) . . ? C19 N9 Cd1 131(3) . . ? N11 N10 C26 115(3) . . ? N11 N10 C36 120(4) . . ? C26 N10 C36 124(4) . . ? N10 N11 N12 104(3) . . ? N11 N12 C25 111(3) . . ? N11 N12 Cd2 120(2) . . ? C25 N12 Cd2 126(3) . . ? N14 N13 C38 111(3) . . ? N14 N13 C49 120(3) . . ? C38 N13 C49 129(3) . . ? N13 N14 N15 109(2) . . ? N14 N15 C37 109(2) . . ? N14 N15 Cd2 119(2) . . ? C37 N15 Cd2 132(2) . . ? N17 N16 C44 109(3) . . ? N17 N16 C54 120(3) . . ? C44 N16 C54 131(3) . . ? N16 N17 N18 109(3) . . ? N17 N18 C43 108(2) . . ? N17 N18 Cd3 112.8(19) . . ? C43 N18 Cd3 136(2) . . ? N20 N19 C67 127(4) . . ? N20 N19 C56 109(3) . . ? C67 N19 C56 124(4) . . ? N19 N20 N21 112(4) . . ? N20 N21 C55 107(3) . . ? N20 N21 Cd3 124(2) . . ? C55 N21 Cd3 127(2) . . ? C62 N22 N23 110(3) . . ? C62 N22 C72 130(3) . . ? N23 N22 C72 119(3) . . ? N24 N23 N22 108(3) . . ? N23 N24 C61 110(3) . . ? N23 N24 Cd4 121(3) . . ? C61 N24 Cd4 129(3) . . ? N3 C1 C2 107(10) . . ? N3 C1 C6 128(10) . . ? C2 C1 C6 124(8) . . ? C3 C2 C1 118(9) . . ? C3 C2 N1 135(10) . . ? C1 C2 N1 106(10) . . ? C4 C3 C2 119(8) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 124(7) . . ? C5 C4 C18 43(4) . 4_454 ? C3 C4 C18 109(6) . 4_454 ? C5 C4 H4 118.2 . . ? C3 C4 H4 118.1 . . ? C18 C4 H4 115.1 4_454 . ? C18 C5 C4 93(6) 4_454 . ? C18 C5 C6 80(6) 4_454 . ? C4 C5 C6 125(8) . . ? C18 C5 H5 97.4 4_454 . ? C4 C5 H5 117.4 . . ? C6 C5 H5 117.4 . . ? C5 C6 C1 109(6) . . ? C5 C6 C18 49(4) . 4_454 ? C1 C6 C18 101(5) . 4_454 ? C5 C6 H6 125.3 . . ? C1 C6 H6 125.3 . . ? C18 C6 H6 113.6 4_454 . ? C12 C7 N6 133(10) . . ? C12 C7 C8 121(10) . . ? N6 C7 C8 106(10) . . ? C9 C8 N4 133(10) . . ? C9 C8 C7 119(10) . . ? N4 C8 C7 107(10) . . ? C8 C9 C10 120(10) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 121(10) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120(10) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 119(10) . . ? C7 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N1 C13 C14 107(10) . . ? N1 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? N1 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? C15 C14 C13 111(8) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 114(7) . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 112(6) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 113(6) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C5 C18 N4 149(7) 4 . ? C5 C18 C17 113(7) 4 . ? N4 C18 C17 91(6) . . ? C5 C18 C6 50(4) 4 4 ? N4 C18 C6 137(7) . 4 ? C17 C18 C6 113(6) . 4 ? C5 C18 C4 44(4) 4 4 ? N4 C18 C4 105(5) . 4 ? C17 C18 C4 136(6) . 4 ? C6 C18 C4 82(5) 4 4 ? C5 C18 H18A 40.6 4 . ? N4 C18 H18A 113.4 . . ? C17 C18 H18A 113.4 . . ? C6 C18 H18A 89.2 4 . ? C4 C18 H18A 22.9 4 . ? C5 C18 H18B 75.0 4 . ? N4 C18 H18B 113.4 . . ? C17 C18 H18B 113.4 . . ? C6 C18 H18B 25.5 4 . ? C4 C18 H18B 97.0 4 . ? H18A C18 H18B 110.7 . . ? C2' C1' N3' 107(10) . . ? C2' C1' C6' 123(10) . . ? N3' C1' C6' 130(10) . . ? N1' C2' C1' 105(10) . . ? N1' C2' C3' 137(10) . . ? C1' C2' C3' 118(10) . . ? C4' C3' C2' 120(10) . . ? C4' C3' H3' 119.8 . . ? C2' C3' H3' 119.8 . . ? C5' C4' C3' 123(9) . . ? C5' C4' H4' 118.6 . . ? C3' C4' H4' 118.6 . . ? C6' C5' C4' 125(9) . . ? C6' C5' H5' 117.7 . . ? C4' C5' H5' 117.7 . . ? C5' C6' C1' 111(7) . . ? C5' C6' H6' 124.6 . . ? C1' C6' H6' 124.6 . . ? C8' C7' C12' 120(8) . . ? C8' C7' N6' 107(10) . . ? C12' C7' N6' 133(10) . . ? C7' C8' N4' 107(10) . . ? C7' C8' C9' 120(9) . . ? N4' C8' C9' 133(10) . . ? C10' C9' C8' 120(7) . . ? C10' C9' H9' 120.2 . . ? C8' C9' H9' 120.2 . . ? C11' C10' C9' 120(6) . . ? C11' C10' H10' 119.9 . . ? C9' C10' H10' 119.8 . . ? C13' C11' C10' 104(6) 4_554 . ? C13' C11' C12' 70(5) 4_554 . ? C10' C11' C12' 120(7) . . ? C13' C11' C14' 54(4) 4_554 4_454 ? C10' C11' C14' 116(6) . 4_454 ? C12' C11' C14' 107(6) . 4_454 ? C13' C11' C15' 100(6) 4_554 4_454 ? C10' C11' C15' 122(6) . 4_454 ? C12' C11' C15' 118(6) . 4_454 ? C14' C11' C15' 48(3) 4_454 4_454 ? C13' C11' H11' 96.3 4_554 . ? C10' C11' H11' 119.9 . . ? C12' C11' H11' 119.9 . . ? C14' C11' H11' 43.1 4_454 . ? C15' C11' H11' 5.6 4_454 . ? C7' C12' C11' 120(7) . . ? C7' C12' C13' 108(6) . 4_554 ? C11' C12' C13' 54(4) . 4_554 ? C7' C12' H12' 120.2 . . ? C11' C12' H12' 120.2 . . ? C13' C12' H12' 105.7 4_554 . ? N1' C13' C11' 133(7) . 4_455 ? N1' C13' C14' 103(6) . 1_455 ? C11' C13' C14' 80(6) 4_455 1_455 ? N1' C13' C12' 141(7) . 4_455 ? C11' C13' C12' 56(5) 4_455 4_455 ? C14' C13' C12' 116(6) 1_455 4_455 ? N1' C13' H13C 111.2 . . ? C11' C13' H13C 34.0 4_455 . ? C14' C13' H13C 111.1 1_455 . ? C12' C13' H13C 52.6 4_455 . ? N1' C13' H13D 111.1 . . ? C11' C13' H13D 111.0 4_455 . ? C14' C13' H13D 111.1 1_455 . ? C12' C13' H13D 58.5 4_455 . ? H13C C13' H13D 109.1 . . ? C13' C14' C15' 111(6) 1_655 . ? C13' C14' C11' 46(4) 1_655 4 ? C15' C14' C11' 68(5) . 4 ? C13' C14' H14C 109.3 1_655 . ? C15' C14' H14C 109.3 . . ? C11' C14' H14C 139.0 4 . ? C13' C14' H14D 109.3 1_655 . ? C15' C14' H14D 109.4 . . ? C11' C14' H14D 111.3 4 . ? H14C C14' H14D 108.0 . . ? C16' C15' C14' 111(8) . . ? C16' C15' C11' 170(8) . 4 ? C14' C15' C11' 64(4) . 4 ? C16' C15' H15C 109.4 . . ? C14' C15' H15C 109.4 . . ? C11' C15' H15C 80.9 4 . ? C16' C15' H15D 109.3 . . ? C14' C15' H15D 109.3 . . ? C11' C15' H15D 65.7 4 . ? H15C C15' H15D 108.0 . . ? C17' C16' C15' 113(10) . . ? C17' C16' H16C 108.9 . . ? C15' C16' H16C 108.9 . . ? C17' C16' H16D 108.9 . . ? C15' C16' H16D 108.9 . . ? H16C C16' H16D 107.8 . . ? C16' C17' C18' 113(10) . . ? C16' C17' H17C 109.0 . . ? C18' C17' H17C 109.0 . . ? C16' C17' H17D 109.0 . . ? C18' C17' H17D 109.0 . . ? H17C C17' H17D 107.8 . . ? N4' C18' C17' 111(10) . . ? N4' C18' H18C 109.5 . . ? C17' C18' H18C 109.5 . . ? N4' C18' H18D 109.5 . . ? C17' C18' H18D 109.5 . . ? H18C C18' H18D 108.1 . . ? N9 C19 C24 128(4) . . ? N9 C19 C20 111(4) . . ? C24 C19 C20 119(4) . . ? N7 C20 C21 138(4) . . ? N7 C20 C19 102(3) . . ? C21 C20 C19 120(4) . . ? C22 C21 C20 119(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 121(4) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C24 C23 C22 119(4) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C19 120(4) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? N12 C25 C26 105(4) . . ? N12 C25 C30 134(4) . . ? C26 C25 C30 119(4) . . ? C27 C26 N10 132(4) . . ? C27 C26 C25 124(4) . . ? N10 C26 C25 104(3) . . ? C26 C27 C28 117(4) . . ? C26 C27 H27 121.5 . . ? C28 C27 H27 121.5 . . ? C27 C28 C29 120(4) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 125(4) . . ? C30 C29 H29 117.3 . . ? C28 C29 H29 117.3 . . ? C29 C30 C25 114(4) . . ? C29 C30 H30 122.8 . . ? C25 C30 H30 122.8 . . ? C32 C31 N7 110(3) . . ? C32 C31 H31A 109.7 . . ? N7 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? N7 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 C32 C33 110(3) . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C32 C33 C34 113(2) . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 112(3) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 115(3) . . ? C36 C35 H35A 108.6 . . ? C34 C35 H35A 108.6 . . ? C36 C35 H35B 108.6 . . ? C34 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C35 C36 N10 114(3) . . ? C35 C36 H36A 108.8 . . ? N10 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? N10 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C42 C37 N15 131(3) . . ? C42 C37 C38 124(3) . . ? N15 C37 C38 105(3) . . ? N13 C38 C37 106(3) . . ? N13 C38 C39 135(3) . . ? C37 C38 C39 119(3) . . ? C40 C39 C38 118(3) . . ? C40 C39 H39 121.1 . . ? C38 C39 H39 121.1 . . ? C39 C40 C41 122(3) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C42 C41 C40 119(3) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C37 C42 C41 118(3) . . ? C37 C42 H42 121.0 . . ? C41 C42 H42 121.0 . . ? C48 C43 N18 129(3) . . ? C48 C43 C44 125(3) . . ? N18 C43 C44 106(3) . . ? N16 C44 C43 108(3) . . ? N16 C44 C45 132(3) . . ? C43 C44 C45 120(3) . . ? C46 C45 C44 113(3) . . ? C46 C45 H45 123.4 . . ? C44 C45 H45 123.4 . . ? C45 C46 C47 127(3) . . ? C45 C46 H46 116.3 . . ? C47 C46 H46 116.3 . . ? C46 C47 C48 119(3) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C43 C48 C47 116(3) . . ? C43 C48 H48 122.2 . . ? C47 C48 H48 122.2 . . ? N13 C49 C50 113(3) . . ? N13 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? N13 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C49 C50 C51 110(3) . . ? C49 C50 H50A 109.6 . . ? C51 C50 H50A 109.6 . . ? C49 C50 H50B 109.6 . . ? C51 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? C50 C51 C52 109(3) . . ? C50 C51 H51A 109.9 . . ? C52 C51 H51A 109.9 . . ? C50 C51 H51B 109.9 . . ? C52 C51 H51B 109.9 . . ? H51A C51 H51B 108.3 . . ? C51 C52 C53 105(3) . . ? C51 C52 H52A 110.7 . . ? C53 C52 H52A 110.7 . . ? C51 C52 H52B 110.7 . . ? C53 C52 H52B 110.7 . . ? H52A C52 H52B 108.8 . . ? C54 C53 C52 119(3) . . ? C54 C53 H53A 107.7 . . ? C52 C53 H53A 107.7 . . ? C54 C53 H53B 107.7 . . ? C52 C53 H53B 107.7 . . ? H53A C53 H53B 107.1 . . ? N16 C54 C53 113(3) . . ? N16 C54 H54A 109.0 . . ? C53 C54 H54A 109.0 . . ? N16 C54 H54B 109.0 . . ? C53 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C60 120(4) . . ? C56 C55 N21 107(3) . . ? C60 C55 N21 132(3) . . ? C57 C56 C55 127(4) . . ? C57 C56 N19 128(4) . . ? C55 C56 N19 105(3) . . ? C56 C57 C58 115(4) . . ? C56 C57 H57 122.4 . . ? C58 C57 H57 122.4 . . ? C57 C58 C59 118(4) . . ? C57 C58 H58 121.0 . . ? C59 C58 H58 121.0 . . ? C58 C59 C60 128(4) . . ? C58 C59 H59 116.0 . . ? C60 C59 H59 116.0 . . ? C59 C60 C55 111(4) . . ? C59 C60 H60 124.5 . . ? C55 C60 H60 124.5 . . ? N24 C61 C66 129(4) . . ? N24 C61 C62 107(4) . . ? C66 C61 C62 123(4) . . ? N22 C62 C61 105(3) . . ? N22 C62 C63 138(4) . . ? C61 C62 C63 116(4) . . ? C64 C63 C62 120(4) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 121(4) . . ? C63 C64 H64 119.4 . . ? C65 C64 H64 119.4 . . ? C64 C65 C66 120(4) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C61 C66 C65 119(4) . . ? C61 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? N19 C67 C68 111(3) . . ? N19 C67 H67A 109.4 . . ? C68 C67 H67A 109.4 . . ? N19 C67 H67B 109.4 . . ? C68 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? C67 C68 C69 116(3) . . ? C67 C68 H68A 108.3 . . ? C69 C68 H68A 108.3 . . ? C67 C68 H68B 108.3 . . ? C69 C68 H68B 108.3 . . ? H68A C68 H68B 107.4 . . ? C70 C69 C68 114(3) . . ? C70 C69 H69A 108.9 . . ? C68 C69 H69A 108.9 . . ? C70 C69 H69B 108.9 . . ? C68 C69 H69B 108.9 . . ? H69A C69 H69B 107.7 . . ? C69 C70 C71 114(3) . . ? C69 C70 H70A 108.6 . . ? C71 C70 H70A 108.6 . . ? C69 C70 H70B 108.6 . . ? C71 C70 H70B 108.6 . . ? H70A C70 H70B 107.6 . . ? C70 C71 C72 112(3) . . ? C70 C71 H71A 109.3 . . ? C72 C71 H71A 109.3 . . ? C70 C71 H71B 109.3 . . ? C72 C71 H71B 109.3 . . ? H71A C71 H71B 107.9 . . ? N22 C72 C71 109(3) . . ? N22 C72 H72A 110.0 . . ? C71 C72 H72A 110.0 . . ? N22 C72 H72B 110.0 . . ? C71 C72 H72B 110.0 . . ? H72A C72 H72B 108.3 . . ? 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 C13 N1 N2 N3 179(53) . . . . ? C2 N1 N2 N3 -1(47) . . . . ? N1 N2 N3 C1 0(38) . . . . ? N1 N2 N3 Cd1 -153(29) . . . . ? N3' Cd1 N3 C1 -127(100) . . . . ? N9 Cd1 N3 C1 134(24) . . . . ? I8 Cd1 N3 C1 -105(22) . . . . ? I5 Cd1 N3 C1 27(26) . . . . ? N3' Cd1 N3 N2 16(77) . . . . ? N9 Cd1 N3 N2 -83(21) . . . . ? I8 Cd1 N3 N2 39(26) . . . . ? I5 Cd1 N3 N2 171(20) . . . . ? C18 N4 N5 N6 -180(9) . . . . ? C8 N4 N5 N6 0(100) . . . . ? N4 N5 N6 C7 0(14) . . . . ? N4 N5 N6 Cd4 173(7) . . . . ? N24 Cd4 N6 N5 48(10) . . . . ? N6' Cd4 N6 N5 -48(32) . . . . ? I7 Cd4 N6 N5 163(9) . . . . ? I6 Cd4 N6 N5 -64(12) . . . . ? N24 Cd4 N6 C7 -141(15) . . . . ? N6' Cd4 N6 C7 123(49) . . . . ? I7 Cd4 N6 C7 -25(16) . . . . ? I6 Cd4 N6 C7 108(14) . . . . ? C13' N1' N2' N3' 179(16) . . . . ? C2' N1' N2' N3' -1(40) . . . . ? N1' N2' N3' C1' 0(25) . . . . ? N1' N2' N3' Cd1 -179(14) . . . . ? N9 Cd1 N3' N2' 43(21) . . . . ? N3 Cd1 N3' N2' -41(80) . . . . ? I8 Cd1 N3' N2' 160(18) . . . . ? I5 Cd1 N3' N2' -68(23) . . . . ? N9 Cd1 N3' C1' -135(29) . . . . ? N3 Cd1 N3' C1' 141(100) . . . . ? I8 Cd1 N3' C1' -18(32) . . . . ? I5 Cd1 N3' C1' 114(27) . . . . ? C18' N4' N5' N6' -180(100) . . . . ? C8' N4' N5' N6' -1(100) . . . . ? N4' N5' N6' C7' 0(75) . . . . ? N4' N5' N6' Cd4 -154(73) . . . . ? N6 Cd4 N6' N5' 8(28) . . . . ? N24 Cd4 N6' N5' -80(12) . . . . ? I7 Cd4 N6' N5' 42(14) . . . . ? I6 Cd4 N6' N5' 174(11) . . . . ? N6 Cd4 N6' C7' -138(50) . . . . ? N24 Cd4 N6' C7' 133(14) . . . . ? I7 Cd4 N6' C7' -105(13) . . . . ? I6 Cd4 N6' C7' 27(15) . . . . ? C20 N7 N8 N9 0(4) . . . . ? C31 N7 N8 N9 177(3) . . . . ? N7 N8 N9 C19 -3(4) . . . . ? N7 N8 N9 Cd1 173(2) . . . . ? N3' Cd1 N9 N8 123(6) . . . . ? N3 Cd1 N9 N8 136(7) . . . . ? I8 Cd1 N9 N8 13(3) . . . . ? I5 Cd1 N9 N8 -121(3) . . . . ? N3' Cd1 N9 C19 -63(6) . . . . ? N3 Cd1 N9 C19 -50(8) . . . . ? I8 Cd1 N9 C19 -173(3) . . . . ? I5 Cd1 N9 C19 54(3) . . . . ? C26 N10 N11 N12 5(4) . . . . ? C36 N10 N11 N12 -173(3) . . . . ? N10 N11 N12 C25 -7(4) . . . . ? N10 N11 N12 Cd2 -170(2) . . . . ? N15 Cd2 N12 N11 -128(3) . . . . ? I1 Cd2 N12 N11 -14(3) . . . . ? I3 Cd2 N12 N11 124(3) . . . . ? N15 Cd2 N12 C25 72(3) . . . . ? I1 Cd2 N12 C25 -174(3) . . . . ? I3 Cd2 N12 C25 -35(3) . . . . ? C38 N13 N14 N15 0(4) . . . . ? C49 N13 N14 N15 174(3) . . . . ? N13 N14 N15 C37 1(4) . . . . ? N13 N14 N15 Cd2 -176(2) . . . . ? N12 Cd2 N15 N14 -47(3) . . . . ? I1 Cd2 N15 N14 -163(2) . . . . ? I3 Cd2 N15 N14 61(3) . . . . ? N12 Cd2 N15 C37 137(3) . . . . ? I1 Cd2 N15 C37 21(4) . . . . ? I3 Cd2 N15 C37 -115(3) . . . . ? C44 N16 N17 N18 1(4) . . . . ? C54 N16 N17 N18 -175(3) . . . . ? N16 N17 N18 C43 -3(3) . . . . ? N16 N17 N18 Cd3 160(2) . . . . ? N21 Cd3 N18 N17 75(2) . . . . ? I4 Cd3 N18 N17 -42(2) . . . . ? I2 Cd3 N18 N17 -174.3(19) . . . . ? N21 Cd3 N18 C43 -128(3) . . . . ? I4 Cd3 N18 C43 115(3) . . . . ? I2 Cd3 N18 C43 -17(3) . . . . ? C67 N19 N20 N21 -175(3) . . . . ? C56 N19 N20 N21 4(4) . . . . ? N19 N20 N21 C55 -4(4) . . . . ? N19 N20 N21 Cd3 -169(2) . . . . ? N18 Cd3 N21 N20 -135(3) . . . . ? I4 Cd3 N21 N20 -22(3) . . . . ? I2 Cd3 N21 N20 115(3) . . . . ? N18 Cd3 N21 C55 64(3) . . . . ? I4 Cd3 N21 C55 177(2) . . . . ? I2 Cd3 N21 C55 -46(3) . . . . ? C62 N22 N23 N24 6(4) . . . . ? C72 N22 N23 N24 176(3) . . . . ? N22 N23 N24 C61 -5(4) . . . . ? N22 N23 N24 Cd4 173(2) . . . . ? N6 Cd4 N24 N23 121(4) . . . . ? N6' Cd4 N24 N23 137(4) . . . . ? I7 Cd4 N24 N23 14(3) . . . . ? I6 Cd4 N24 N23 -119(3) . . . . ? N6 Cd4 N24 C61 -62(5) . . . . ? N6' Cd4 N24 C61 -46(5) . . . . ? I7 Cd4 N24 C61 -169(3) . . . . ? I6 Cd4 N24 C61 58(3) . . . . ? N2 N3 C1 C2 0(30) . . . . ? Cd1 N3 C1 C2 143(19) . . . . ? N2 N3 C1 C6 -179(13) . . . . ? Cd1 N3 C1 C6 -37(34) . . . . ? N3 C1 C2 C3 -179(18) . . . . ? C6 C1 C2 C3 0(11) . . . . ? N3 C1 C2 N1 -1(33) . . . . ? C6 C1 C2 N1 178(28) . . . . ? C13 N1 C2 C3 -1(73) . . . . ? N2 N1 C2 C3 179(14) . . . . ? C13 N1 C2 C1 -178(38) . . . . ? N2 N1 C2 C1 1(46) . . . . ? C1 C2 C3 C4 0(11) . . . . ? N1 C2 C3 C4 -177(37) . . . . ? C2 C3 C4 C5 -2(12) . . . . ? C2 C3 C4 C18 44(9) . . . 4_454 ? C3 C4 C5 C18 83(9) . . . 4_454 ? C3 C4 C5 C6 2(13) . . . . ? C18 C4 C5 C6 -80(9) 4_454 . . . ? C18 C5 C6 C1 -88(7) 4_454 . . . ? C4 C5 C6 C1 -2(11) . . . . ? C4 C5 C6 C18 87(9) . . . 4_454 ? N3 C1 C6 C5 180(22) . . . . ? C2 C1 C6 C5 0(10) . . . . ? N3 C1 C6 C18 129(22) . . . 4_454 ? C2 C1 C6 C18 -50(9) . . . 4_454 ? N5 N6 C7 C12 180(10) . . . . ? Cd4 N6 C7 C12 8(24) . . . . ? N5 N6 C7 C8 0(100) . . . . ? Cd4 N6 C7 C8 -172(100) . . . . ? C18 N4 C8 C9 1(100) . . . . ? N5 N4 C8 C9 -179(100) . . . . ? C18 N4 C8 C7 180(58) . . . . ? N5 N4 C8 C7 -1(100) . . . . ? C12 C7 C8 C9 -1(100) . . . . ? N6 C7 C8 C9 179(100) . . . . ? C12 C7 C8 N4 -179(82) . . . . ? N6 C7 C8 N4 1(100) . . . . ? N4 C8 C9 C10 179(100) . . . . ? C7 C8 C9 C10 1(100) . . . . ? C8 C9 C10 C11 0(100) . . . . ? C9 C10 C11 C12 -1(23) . . . . ? N6 C7 C12 C11 180(14) . . . . ? C8 C7 C12 C11 0(100) . . . . ? C10 C11 C12 C7 1(18) . . . . ? N2 N1 C13 C14 -82(60) . . . . ? C2 N1 C13 C14 97(42) . . . . ? N1 C13 C14 C15 83(25) . . . . ? C13 C14 C15 C16 -149(8) . . . . ? C14 C15 C16 C17 -135(7) . . . . ? C15 C16 C17 C18 -62(8) . . . . ? C8 N4 C18 C5 156(100) . . . 4 ? N5 N4 C18 C5 -24(19) . . . 4 ? C8 N4 C18 C17 -60(100) . . . . ? N5 N4 C18 C17 120(6) . . . . ? C8 N4 C18 C6 67(100) . . . 4 ? N5 N4 C18 C6 -113(9) . . . 4 ? C8 N4 C18 C4 161(100) . . . 4 ? N5 N4 C18 C4 -19(8) . . . 4 ? C16 C17 C18 C5 31(9) . . . 4 ? C16 C17 C18 N4 -130(6) . . . . ? C16 C17 C18 C6 86(7) . . . 4 ? C16 C17 C18 C4 -16(11) . . . 4 ? N2' N3' C1' C2' 1(45) . . . . ? Cd1 N3' C1' C2' 179(43) . . . . ? N2' N3' C1' C6' 180(12) . . . . ? Cd1 N3' C1' C6' -2(40) . . . . ? C13' N1' C2' C1' -178(26) . . . . ? N2' N1' C2' C1' 1(60) . . . . ? C13' N1' C2' C3' 0(100) . . . . ? N2' N1' C2' C3' 179(71) . . . . ? N3' C1' C2' N1' -1(59) . . . . ? C6' C1' C2' N1' 180(23) . . . . ? N3' C1' C2' C3' -180(49) . . . . ? C6' C1' C2' C3' 1(81) . . . . ? N1' C2' C3' C4' -180(66) . . . . ? C1' C2' C3' C4' -2(79) . . . . ? C2' C3' C4' C5' 2(43) . . . . ? C3' C4' C5' C6' -2(16) . . . . ? C4' C5' C6' C1' 1(13) . . . . ? C2' C1' C6' C5' -1(43) . . . . ? N3' C1' C6' C5' -180(20) . . . . ? N5' N6' C7' C8' 1(17) . . . . ? Cd4 N6' C7' C8' 148(11) . . . . ? N5' N6' C7' C12' 179(10) . . . . ? Cd4 N6' C7' C12' -35(22) . . . . ? C12' C7' C8' N4' -180(75) . . . . ? N6' C7' C8' N4' -2(75) . . . . ? C12' C7' C8' C9' 2(11) . . . . ? N6' C7' C8' C9' -180(11) . . . . ? C18' N4' C8' C7' -179(100) . . . . ? N5' N4' C8' C7' 2(100) . . . . ? C18' N4' C8' C9' -2(100) . . . . ? N5' N4' C8' C9' 179(38) . . . . ? C7' C8' C9' C10' -1(11) . . . . ? N4' C8' C9' C10' -178(97) . . . . ? C8' C9' C10' C11' 0(11) . . . . ? C9' C10' C11' C13' 73(9) . . . 4_554 ? C9' C10' C11' C12' -1(11) . . . . ? C9' C10' C11' C14' 130(7) . . . 4_454 ? C9' C10' C11' C15' -175(6) . . . 4_454 ? C8' C7' C12' C11' -3(11) . . . . ? N6' C7' C12' C11' 179(13) . . . . ? C8' C7' C12' C13' -62(9) . . . 4_554 ? N6' C7' C12' C13' 120(14) . . . 4_554 ? C13' C11' C12' C7' -92(8) 4_554 . . . ? C10' C11' C12' C7' 3(11) . . . . ? C14' C11' C12' C7' -132(7) 4_454 . . . ? C15' C11' C12' C7' 177(6) 4_454 . . . ? C10' C11' C12' C13' 95(8) . . . 4_554 ? C14' C11' C12' C13' -40(5) 4_454 . . 4_554 ? C15' C11' C12' C13' -91(7) 4_454 . . 4_554 ? C2' N1' C13' C11' 177(40) . . . 4_455 ? N2' N1' C13' C11' -2(14) . . . 4_455 ? C2' N1' C13' C14' -95(40) . . . 1_455 ? N2' N1' C13' C14' 86(8) . . . 1_455 ? C2' N1' C13' C12' 90(41) . . . 4_455 ? N2' N1' C13' C12' -89(12) . . . 4_455 ? C13' C14' C15' C16' -175(8) 1_655 . . . ? C11' C14' C15' C16' 170(8) 4 . . . ? C13' C14' C15' C11' 15(5) 1_655 . . 4 ? C14' C15' C16' C17' 140(13) . . . . ? C11' C15' C16' C17' -158(40) 4 . . . ? C15' C16' C17' C18' 76(17) . . . . ? N5' N4' C18' C17' -103(100) . . . . ? C8' N4' C18' C17' 79(100) . . . . ? C16' C17' C18' N4' 56(72) . . . . ? N8 N9 C19 C24 167(4) . . . . ? Cd1 N9 C19 C24 -8(6) . . . . ? N8 N9 C19 C20 4(5) . . . . ? Cd1 N9 C19 C20 -170(3) . . . . ? N8 N7 C20 C21 -175(5) . . . . ? C31 N7 C20 C21 9(8) . . . . ? N8 N7 C20 C19 2(4) . . . . ? C31 N7 C20 C19 -174(3) . . . . ? N9 C19 C20 N7 -4(4) . . . . ? C24 C19 C20 N7 -169(3) . . . . ? N9 C19 C20 C21 174(3) . . . . ? C24 C19 C20 C21 10(6) . . . . ? N7 C20 C21 C22 177(4) . . . . ? C19 C20 C21 C22 -1(6) . . . . ? C20 C21 C22 C23 -4(6) . . . . ? C21 C22 C23 C24 -1(6) . . . . ? C22 C23 C24 C19 10(6) . . . . ? N9 C19 C24 C23 -176(4) . . . . ? C20 C19 C24 C23 -15(6) . . . . ? N11 N12 C25 C26 6(4) . . . . ? Cd2 N12 C25 C26 167(3) . . . . ? N11 N12 C25 C30 172(4) . . . . ? Cd2 N12 C25 C30 -27(6) . . . . ? N11 N10 C26 C27 -179(4) . . . . ? C36 N10 C26 C27 0(7) . . . . ? N11 N10 C26 C25 -1(4) . . . . ? C36 N10 C26 C25 177(3) . . . . ? N12 C25 C26 C27 175(4) . . . . ? C30 C25 C26 C27 6(6) . . . . ? N12 C25 C26 N10 -3(4) . . . . ? C30 C25 C26 N10 -171(3) . . . . ? N10 C26 C27 C28 175(4) . . . . ? C25 C26 C27 C28 -2(6) . . . . ? C26 C27 C28 C29 -1(6) . . . . ? C27 C28 C29 C30 0(6) . . . . ? C28 C29 C30 C25 5(6) . . . . ? N12 C25 C30 C29 -172(4) . . . . ? C26 C25 C30 C29 -7(5) . . . . ? C20 N7 C31 C32 85(5) . . . . ? N8 N7 C31 C32 -90(4) . . . . ? N7 C31 C32 C33 -170(3) . . . . ? C31 C32 C33 C34 82(4) . . . . ? C32 C33 C34 C35 -179(4) . . . . ? C33 C34 C35 C36 -76(4) . . . . ? C34 C35 C36 N10 179(4) . . . . ? N11 N10 C36 C35 84(5) . . . . ? C26 N10 C36 C35 -94(5) . . . . ? N14 N15 C37 C42 -179(4) . . . . ? Cd2 N15 C37 C42 -2(6) . . . . ? N14 N15 C37 C38 -1(4) . . . . ? Cd2 N15 C37 C38 176(3) . . . . ? N14 N13 C38 C37 0(4) . . . . ? C49 N13 C38 C37 -174(3) . . . . ? N14 N13 C38 C39 -178(5) . . . . ? C49 N13 C38 C39 8(8) . . . . ? C42 C37 C38 N13 179(3) . . . . ? N15 C37 C38 N13 1(4) . . . . ? C42 C37 C38 C39 -3(6) . . . . ? N15 C37 C38 C39 179(4) . . . . ? N13 C38 C39 C40 179(5) . . . . ? C37 C38 C39 C40 1(6) . . . . ? C38 C39 C40 C41 2(6) . . . . ? C39 C40 C41 C42 -4(6) . . . . ? N15 C37 C42 C41 179(4) . . . . ? C38 C37 C42 C41 1(6) . . . . ? C40 C41 C42 C37 2(5) . . . . ? N17 N18 C43 C48 -179(3) . . . . ? Cd3 N18 C43 C48 23(5) . . . . ? N17 N18 C43 C44 4(3) . . . . ? Cd3 N18 C43 C44 -154(2) . . . . ? N17 N16 C44 C43 1(4) . . . . ? C54 N16 C44 C43 176(3) . . . . ? N17 N16 C44 C45 179(3) . . . . ? C54 N16 C44 C45 -5(6) . . . . ? C48 C43 C44 N16 180(3) . . . . ? N18 C43 C44 N16 -3(3) . . . . ? C48 C43 C44 C45 1(4) . . . . ? N18 C43 C44 C45 179(3) . . . . ? N16 C44 C45 C46 -178(3) . . . . ? C43 C44 C45 C46 1(4) . . . . ? C44 C45 C46 C47 -1(5) . . . . ? C45 C46 C47 C48 1(5) . . . . ? N18 C43 C48 C47 -179(3) . . . . ? C44 C43 C48 C47 -2(4) . . . . ? C46 C47 C48 C43 1(4) . . . . ? N14 N13 C49 C50 -96(3) . . . . ? C38 N13 C49 C50 77(5) . . . . ? N13 C49 C50 C51 -178(2) . . . . ? C49 C50 C51 C52 -176(3) . . . . ? C50 C51 C52 C53 -174(2) . . . . ? C51 C52 C53 C54 -70(4) . . . . ? N17 N16 C54 C53 109(4) . . . . ? C44 N16 C54 C53 -66(5) . . . . ? C52 C53 C54 N16 -62(4) . . . . ? N20 N21 C55 C56 3(4) . . . . ? Cd3 N21 C55 C56 167(3) . . . . ? N20 N21 C55 C60 171(4) . . . . ? Cd3 N21 C55 C60 -25(6) . . . . ? C60 C55 C56 C57 4(6) . . . . ? N21 C55 C56 C57 173(4) . . . . ? C60 C55 C56 N19 -171(3) . . . . ? N21 C55 C56 N19 -1(4) . . . . ? N20 N19 C56 C57 -176(4) . . . . ? C67 N19 C56 C57 3(6) . . . . ? N20 N19 C56 C55 -1(4) . . . . ? C67 N19 C56 C55 178(3) . . . . ? C55 C56 C57 C58 4(6) . . . . ? N19 C56 C57 C58 177(3) . . . . ? C56 C57 C58 C59 -4(5) . . . . ? C57 C58 C59 C60 -3(6) . . . . ? C58 C59 C60 C55 10(5) . . . . ? C56 C55 C60 C59 -10(5) . . . . ? N21 C55 C60 C59 -177(4) . . . . ? N23 N24 C61 C66 174(4) . . . . ? Cd4 N24 C61 C66 -3(6) . . . . ? N23 N24 C61 C62 2(5) . . . . ? Cd4 N24 C61 C62 -175(3) . . . . ? N23 N22 C62 C61 -4(4) . . . . ? C72 N22 C62 C61 -173(4) . . . . ? N23 N22 C62 C63 -172(5) . . . . ? C72 N22 C62 C63 18(8) . . . . ? N24 C61 C62 N22 1(4) . . . . ? C66 C61 C62 N22 -171(4) . . . . ? N24 C61 C62 C63 173(3) . . . . ? C66 C61 C62 C63 0(6) . . . . ? N22 C62 C63 C64 169(5) . . . . ? C61 C62 C63 C64 1(6) . . . . ? C62 C63 C64 C65 1(6) . . . . ? C63 C64 C65 C66 -3(6) . . . . ? N24 C61 C66 C65 -173(4) . . . . ? C62 C61 C66 C65 -3(6) . . . . ? C64 C65 C66 C61 4(6) . . . . ? N20 N19 C67 C68 78(5) . . . . ? C56 N19 C67 C68 -101(4) . . . . ? N19 C67 C68 C69 178(4) . . . . ? C67 C68 C69 C70 -71(5) . . . . ? C68 C69 C70 C71 176(4) . . . . ? C69 C70 C71 C72 77(4) . . . . ? C62 N22 C72 C71 80(5) . . . . ? N23 N22 C72 C71 -89(4) . . . . ? C70 C71 C72 N22 -171(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.984 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.159