Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Liu, Hongke' 'Sun, Wei-Yin' 'Tang, Wen-Xia' 'Tong, Ye-Xiang' 'Yu, Xiao-Lan' 'Zhang, Hua-Xin' _publ_contact_author_name 'Dr Hong-Ke Liu' _publ_contact_author_address ; Chemistry The University of Toledo 2804 Kenwood #103 Toledo Ohio 43606 UNITED STATES OF AMERICA ; _publ_contact_author_email 'HONGKE_LIU@HOTMAIL.COM' _publ_section_title ; Assembly of Supermolecular Complexes with Tripodal Ligand titmb and tib: A 2D Rhombic Grid Network Assembled from 2-Connected tib ; data_cu _database_code_CSD 157077 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H116 Cu2 N24 O24' _chemical_formula_weight 1925.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.565(2) _cell_length_b 12.130(2) _cell_length_c 17.726(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.72(3) _cell_angle_gamma 90.00 _cell_volume 2206.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.896607 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12735 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 29.99 _reflns_number_total 5465 _reflns_number_gt 2708 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1579P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.007(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5465 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1509 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2686 _refine_ls_wR_factor_gt 0.2218 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Cu1 Cu 0.0000 0.0000 0.0000 0.0380(3) Uani 1 2 d S . . N6 N -0.1733(3) 0.0665(3) 0.0016(2) 0.0399(9) Uani 1 1 d . . . N5 N -0.3470(3) 0.1724(3) -0.0218(2) 0.0415(9) Uani 1 1 d . . . N3 N -0.9017(4) 0.3585(4) -0.2798(2) 0.0462(10) Uani 1 1 d . . . N4 N -0.9377(4) 0.4598(3) -0.3850(2) 0.0422(9) Uani 1 1 d . . . N2 N -0.6103(8) -0.1334(5) -0.2314(4) 0.092(2) Uani 1 1 d . . . N1 N -0.5941(12) -0.2856(5) -0.1632(5) 0.128(3) Uani 1 1 d . . . O1 O -0.8829(7) -0.0823(7) -0.3981(4) 0.143(3) Uani 1 1 d . . . O2W O -1.1166(7) -0.1538(6) -0.4605(5) 0.137(2) Uani 1 1 d . . . O2 O -1.0663(9) 0.1149(7) -0.3999(5) 0.171(3) Uani 1 1 d . . . O1W O -1.0613(4) -0.3174(4) -0.4581(3) 0.0704(12) Uani 1 1 d . . . O3 O -1.2816(13) 0.0123(8) -0.5005(9) 0.250(7) Uani 1 1 d . . . O4 O -1.4561(12) 0.0204(7) -0.4253(7) 0.208(5) Uani 1 1 d . . . C16 C -0.5445(4) 0.2032(4) -0.1265(3) 0.0407(11) Uani 1 1 d . . . C15 C -0.2288(4) 0.1554(4) -0.0347(3) 0.0397(10) Uani 1 1 d . . . H15A H -0.1904 0.2006 -0.0653 0.048 Uiso 1 1 calc R . . C14 C -0.5179(5) 0.1106(4) -0.1661(3) 0.0469(12) Uani 1 1 d . . . H14A H -0.4361 0.0777 -0.1520 0.056 Uiso 1 1 calc R . . C13 C -0.2596(5) 0.0264(4) 0.0417(3) 0.0466(12) Uani 1 1 d . . . H13A H -0.2459 -0.0350 0.0740 0.056 Uiso 1 1 calc R . . C12 C -0.4409(4) 0.2534(4) -0.0603(3) 0.0484(12) Uani 1 1 d . . . H12A H -0.3959 0.3117 -0.0808 0.058 Uiso 1 1 calc R . . H12B H -0.4831 0.2860 -0.0226 0.058 Uiso 1 1 calc R . . C11 C -0.6679(4) 0.2509(4) -0.1473(3) 0.0442(11) Uani 1 1 d . . . H11A H -0.6866 0.3118 -0.1200 0.053 Uiso 1 1 calc R . . C10 C -0.3676(4) 0.0899(4) 0.0269(3) 0.0463(11) Uani 1 1 d . . . H10A H -0.4415 0.0798 0.0460 0.056 Uiso 1 1 calc R . . C9 C -0.6140(5) 0.0663(4) -0.2275(3) 0.0508(12) Uani 1 1 d . . . C8 C -0.5842(7) -0.0335(5) -0.2694(4) 0.0718(18) Uani 1 1 d . . . H8A H -0.6368 -0.0325 -0.3223 0.086 Uiso 1 1 calc R . . H8B H -0.4933 -0.0320 -0.2714 0.086 Uiso 1 1 calc R . . C5 C -0.7632(5) 0.2089(4) -0.2084(3) 0.0466(12) Uani 1 1 d . . . C4 C -0.7337(5) 0.1174(5) -0.2479(3) 0.0537(13) Uani 1 1 d . . . H4B H -0.7967 0.0896 -0.2894 0.064 Uiso 1 1 calc R . . C3 C -0.8974(5) 0.2614(5) -0.2291(3) 0.0578(15) Uani 1 1 d . . . H3A H -0.9605 0.2074 -0.2552 0.069 Uiso 1 1 calc R . . H3B H -0.9215 0.2835 -0.1818 0.069 Uiso 1 1 calc R . . C2 C -0.8583(7) 0.4593(6) -0.2582(3) 0.076(2) Uani 1 1 d . . . H2A H -0.8190 0.4820 -0.2080 0.091 Uiso 1 1 calc R . . C7 C -0.8821(7) 0.5227(5) -0.3233(3) 0.0662(17) Uani 1 1 d . . . H7A H -0.8631 0.5974 -0.3250 0.079 Uiso 1 1 calc R . . C6 C -0.9503(5) 0.3617(4) -0.3569(3) 0.0483(12) Uani 1 1 d . . . H6A H -0.9882 0.3019 -0.3866 0.058 Uiso 1 1 calc R . . C2W C -1.1193(9) -0.2474(5) -0.4790(4) 0.081(2) Uani 1 1 d . . . C1W C -1.2579(8) -0.2672(9) -0.5463(6) 0.123(3) Uani 1 1 d . . . H1WA H -1.2629 -0.3426 -0.5632 0.184 Uiso 1 1 calc R . . H1WB H -1.2596 -0.2196 -0.5899 0.184 Uiso 1 1 calc R . . H1WC H -1.3307 -0.2507 -0.5246 0.184 Uiso 1 1 calc R . . C18 C -0.7371(12) -0.1717(9) -0.2303(6) 0.127(4) Uani 1 1 d . . . H18A H -0.8152 -0.1389 -0.2556 0.152 Uiso 1 1 calc R . . C17 C -0.7258(14) -0.2565(11) -0.1897(8) 0.153(5) Uani 1 1 d . . . H17A H -0.7950 -0.2953 -0.1785 0.184 Uiso 1 1 calc R . . C1 C -0.5203(15) -0.2011(9) -0.1904(6) 0.149(5) Uani 1 1 d . . . H1B H -0.4302 -0.1950 -0.1815 0.179 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 Cu1 0.0292(4) 0.0451(5) 0.0346(4) -0.0034(3) -0.0026(3) 0.0046(3) N6 0.0339(18) 0.043(2) 0.040(2) -0.0001(16) 0.0030(16) 0.0003(16) N5 0.0333(19) 0.043(2) 0.044(2) -0.0039(16) 0.0023(17) 0.0014(15) N3 0.042(2) 0.060(3) 0.034(2) 0.0094(18) 0.0030(17) 0.0066(18) N4 0.042(2) 0.049(2) 0.0311(19) 0.0017(16) -0.0014(17) -0.0018(17) N2 0.142(6) 0.056(4) 0.081(4) -0.024(3) 0.032(4) -0.011(4) N1 0.255(11) 0.051(4) 0.100(5) 0.001(3) 0.083(7) 0.029(5) O1 0.120(5) 0.196(8) 0.096(4) -0.028(5) -0.011(3) -0.035(5) O2W 0.131(5) 0.092(5) 0.176(7) 0.003(4) 0.009(5) -0.008(4) O2 0.216(9) 0.161(7) 0.137(7) -0.009(5) 0.045(6) -0.054(6) O1W 0.057(2) 0.089(3) 0.064(3) -0.009(2) 0.013(2) -0.001(2) O3 0.240(13) 0.169(10) 0.327(18) 0.060(9) 0.039(12) 0.088(8) O4 0.243(13) 0.117(7) 0.241(12) 0.033(6) 0.014(9) -0.022(6) C16 0.035(2) 0.042(2) 0.042(3) 0.0023(19) 0.003(2) -0.0021(18) C15 0.032(2) 0.045(3) 0.040(2) 0.0031(19) 0.0048(19) -0.0005(18) C14 0.042(3) 0.051(3) 0.046(3) 0.001(2) 0.006(2) 0.003(2) C13 0.044(3) 0.049(3) 0.047(3) 0.009(2) 0.011(2) 0.004(2) C12 0.037(2) 0.043(3) 0.060(3) -0.008(2) 0.001(2) 0.0072(19) C11 0.042(2) 0.045(3) 0.044(3) 0.006(2) 0.007(2) 0.003(2) C10 0.036(2) 0.053(3) 0.051(3) 0.002(2) 0.013(2) -0.003(2) C9 0.060(3) 0.050(3) 0.043(3) -0.002(2) 0.013(2) -0.004(2) C8 0.088(5) 0.072(4) 0.052(3) -0.017(3) 0.010(3) -0.009(3) C5 0.042(2) 0.056(3) 0.041(3) 0.018(2) 0.009(2) -0.004(2) C4 0.050(3) 0.063(3) 0.041(3) 0.005(2) -0.004(2) -0.013(2) C3 0.045(3) 0.074(4) 0.049(3) 0.024(3) 0.002(2) -0.004(2) C2 0.111(5) 0.067(4) 0.035(3) -0.003(3) -0.010(3) 0.001(4) C7 0.091(5) 0.049(3) 0.048(3) -0.006(2) -0.003(3) -0.001(3) C6 0.042(3) 0.061(3) 0.036(3) 0.006(2) -0.004(2) -0.005(2) C2W 0.145(7) 0.038(3) 0.085(5) 0.010(3) 0.078(5) 0.025(4) C1W 0.093(6) 0.154(9) 0.106(7) -0.003(6) -0.004(5) 0.004(6) C18 0.155(10) 0.076(6) 0.134(9) -0.002(6) 0.004(7) -0.043(6) C17 0.172(12) 0.099(8) 0.164(11) -0.042(8) -0.011(9) 0.050(8) C1 0.268(15) 0.103(8) 0.102(8) -0.010(6) 0.096(9) 0.069(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 Cu1 N6 2.007(4) 3 ? Cu1 N6 2.007(4) . ? Cu1 N4 2.047(4) 2_444 ? Cu1 N4 2.047(4) 4_666 ? N6 C15 1.319(6) . ? N6 C13 1.372(6) . ? N5 C15 1.338(6) . ? N5 C10 1.373(6) . ? N5 C12 1.447(6) . ? N3 C2 1.330(8) . ? N3 C6 1.341(6) . ? N3 C3 1.476(6) . ? N4 C6 1.309(6) . ? N4 C7 1.349(7) . ? N4 Cu1 2.047(4) 2_454 ? N2 C1 1.333(12) . ? N2 C18 1.422(12) . ? N2 C8 1.445(9) . ? N1 C17 1.404(14) . ? N1 C1 1.439(14) . ? O2W C2W 1.181(8) . ? O1W C2W 1.061(7) . ? C16 C14 1.388(7) . ? C16 C11 1.393(6) . ? C16 C12 1.529(6) . ? C14 C9 1.407(7) . ? C13 C10 1.350(7) . ? C11 C5 1.389(7) . ? C9 C4 1.377(7) . ? C9 C8 1.493(8) . ? C5 C4 1.386(8) . ? C5 C3 1.518(7) . ? C2 C7 1.361(9) . ? C2W C1W 1.672(12) . ? C18 C17 1.245(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N6 180.0(3) 3 . ? N6 Cu1 N4 88.24(15) 3 2_444 ? N6 Cu1 N4 91.76(15) . 2_444 ? N6 Cu1 N4 91.76(15) 3 4_666 ? N6 Cu1 N4 88.24(15) . 4_666 ? N4 Cu1 N4 180.00(8) 2_444 4_666 ? C15 N6 C13 105.6(4) . . ? C15 N6 Cu1 128.5(3) . . ? C13 N6 Cu1 125.9(3) . . ? C15 N5 C10 106.7(4) . . ? C15 N5 C12 126.1(4) . . ? C10 N5 C12 126.7(4) . . ? C2 N3 C6 106.8(4) . . ? C2 N3 C3 126.8(4) . . ? C6 N3 C3 126.4(4) . . ? C6 N4 C7 105.7(4) . . ? C6 N4 Cu1 123.9(3) . 2_454 ? C7 N4 Cu1 130.4(4) . 2_454 ? C1 N2 C18 110.1(9) . . ? C1 N2 C8 125.5(9) . . ? C18 N2 C8 124.3(8) . . ? C17 N1 C1 106.3(10) . . ? C14 C16 C11 119.4(4) . . ? C14 C16 C12 121.1(4) . . ? C11 C16 C12 119.5(4) . . ? N6 C15 N5 111.6(4) . . ? C16 C14 C9 120.3(4) . . ? C10 C13 N6 109.4(4) . . ? N5 C12 C16 112.2(4) . . ? C5 C11 C16 120.9(5) . . ? C13 C10 N5 106.5(4) . . ? C4 C9 C14 118.7(5) . . ? C4 C9 C8 121.5(5) . . ? C14 C9 C8 119.7(5) . . ? N2 C8 C9 111.2(5) . . ? C4 C5 C11 118.6(5) . . ? C4 C5 C3 121.5(5) . . ? C11 C5 C3 119.8(5) . . ? C9 C4 C5 122.0(5) . . ? N3 C3 C5 112.0(4) . . ? N3 C2 C7 107.1(5) . . ? N4 C7 C2 109.0(5) . . ? N4 C6 N3 111.4(4) . . ? O1W C2W O2W 134.3(10) . . ? O1W C2W C1W 118.0(7) . . ? O2W C2W C1W 107.2(7) . . ? C17 C18 N2 108.4(13) . . ? C18 C17 N1 110.7(15) . . ? N2 C1 N1 104.4(12) . . ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.850 _refine_diff_density_max 1.049 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.100 data_ll2 _database_code_CSD 162985 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 N6 O2' _chemical_formula_weight 354.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 18.590(4) _cell_length_b 16.384(3) _cell_length_c 11.721(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.20(3) _cell_angle_gamma 90.00 _cell_volume 3489.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.800699 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12786 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7487 _reflns_number_gt 3724 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0692P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7487 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 N9 N 0.07674(9) 0.42519(9) 0.51614(12) 0.0472(4) Uani 1 1 d . . . C26 C 0.17919(11) 0.36707(11) 0.33770(15) 0.0481(5) Uani 1 1 d . . . H26A H 0.1336 0.3546 0.2909 0.058 Uiso 1 1 calc R . . N8 N 0.40245(9) 0.38376(10) 0.66781(12) 0.0506(4) Uani 1 1 d . . . C25 C 0.18370(11) 0.42671(11) 0.42271(15) 0.0450(5) Uani 1 1 d . . . C27 C 0.24091(11) 0.32558(11) 0.32069(14) 0.0452(5) Uani 1 1 d . . . C23 C 0.31476(11) 0.40311(12) 0.47800(15) 0.0474(5) Uani 1 1 d . . . N11 N 0.22197(10) 0.30215(9) 0.10910(12) 0.0513(4) Uani 1 1 d . . . N7 N 0.44045(10) 0.29322(11) 0.80612(14) 0.0622(5) Uani 1 1 d . . . C30 C 0.01195(12) 0.38719(13) 0.48240(18) 0.0592(6) Uani 1 1 d . . . H30A H -0.0149 0.3869 0.4059 0.071 Uiso 1 1 calc R . . C28 C 0.30841(11) 0.34393(11) 0.39192(14) 0.0474(5) Uani 1 1 d . . . H28A H 0.3502 0.3161 0.3818 0.057 Uiso 1 1 calc R . . C22 C 0.38938(11) 0.42362(13) 0.55289(15) 0.0584(6) Uani 1 1 d . . . H22A H 0.4274 0.4069 0.5124 0.070 Uiso 1 1 calc R . . H22B H 0.3930 0.4823 0.5638 0.070 Uiso 1 1 calc R . . C33 C 0.23472(12) 0.26338(11) 0.22375(15) 0.0555(6) Uani 1 1 d . . . H33A H 0.2797 0.2316 0.2353 0.067 Uiso 1 1 calc R . . H33B H 0.1945 0.2264 0.2268 0.067 Uiso 1 1 calc R . . C24 C 0.25225(12) 0.44442(11) 0.49157(15) 0.0500(5) Uani 1 1 d . . . H24A H 0.2562 0.4850 0.5481 0.060 Uiso 1 1 calc R . . C32 C 0.04537(14) 0.36621(13) 0.66355(18) 0.0634(6) Uani 1 1 d . . . H32A H 0.0462 0.3478 0.7389 0.076 Uiso 1 1 calc R . . N10 N -0.00953(10) 0.35040(11) 0.56865(16) 0.0679(5) Uani 1 1 d . . . C35 C 0.15964(13) 0.30123(14) 0.02781(18) 0.0670(6) Uani 1 1 d . . . H35A H 0.1179 0.2721 0.0352 0.080 Uiso 1 1 calc R . . C29 C 0.11582(11) 0.47063(12) 0.44040(17) 0.0551(5) Uani 1 1 d . . . H29A H 0.1297 0.5237 0.4746 0.066 Uiso 1 1 calc R . . H29B H 0.0831 0.4792 0.3652 0.066 Uiso 1 1 calc R . . C20 C 0.41121(12) 0.35911(13) 0.85125(17) 0.0633(6) Uani 1 1 d . . . H20A H 0.4080 0.3646 0.9290 0.076 Uiso 1 1 calc R . . C21 C 0.43407(12) 0.31114(13) 0.69506(17) 0.0587(6) Uani 1 1 d . . . H21A H 0.4498 0.2771 0.6416 0.070 Uiso 1 1 calc R . . N12 N 0.16361(14) 0.34584(13) -0.06374(16) 0.0827(7) Uani 1 1 d . . . C19 C 0.38776(12) 0.41487(13) 0.76801(16) 0.0601(6) Uani 1 1 d . . . H19A H 0.3658 0.4648 0.7770 0.072 Uiso 1 1 calc R . . C31 C 0.09809(13) 0.41212(13) 0.63273(16) 0.0615(6) Uani 1 1 d . . . H31A H 0.1408 0.4312 0.6817 0.074 Uiso 1 1 calc R . . C34 C 0.26947(15) 0.35103(14) 0.06748(19) 0.0711(7) Uani 1 1 d . . . H34A H 0.3174 0.3641 0.1043 0.085 Uiso 1 1 calc R . . C36 C 0.23281(19) 0.37682(15) -0.0384(2) 0.0823(8) Uani 1 1 d . . . H36A H 0.2524 0.4111 -0.0873 0.099 Uiso 1 1 calc R . . N5 N 0.07802(9) 0.56948(9) 0.00188(13) 0.0510(4) Uani 1 1 d . . . C7 C 0.22453(13) 0.67852(11) 0.33658(15) 0.0484(5) Uani 1 1 d . . . N3 N 0.23455(11) 0.68456(10) 0.55054(14) 0.0544(5) Uani 1 1 d . . . C5 C 0.29809(11) 0.63085(11) 0.20349(16) 0.0465(5) Uani 1 1 d . . . C9 C 0.17295(12) 0.58467(11) 0.18236(15) 0.0450(5) Uani 1 1 d . . . C10 C 0.23864(13) 0.58431(11) 0.14661(16) 0.0498(5) Uani 1 1 d . . . H10B H 0.2435 0.5523 0.0831 0.060 Uiso 1 1 calc R . . C8 C 0.16617(11) 0.63245(11) 0.27743(15) 0.0490(5) Uani 1 1 d . . . H8A H 0.1217 0.6334 0.3017 0.059 Uiso 1 1 calc R . . N2 N 0.40823(9) 0.55222(10) 0.18574(15) 0.0552(5) Uani 1 1 d . . . C6 C 0.28982(13) 0.67698(11) 0.29850(16) 0.0523(6) Uani 1 1 d . . . H6A H 0.3293 0.7078 0.3379 0.063 Uiso 1 1 calc R . . N4 N 0.29695(13) 0.61968(10) 0.70454(15) 0.0643(5) Uani 1 1 d . . . N6 N 0.04778(11) 0.58225(12) -0.18966(15) 0.0754(6) Uani 1 1 d . . . C13 C 0.30104(12) 0.65897(12) 0.60822(17) 0.0555(5) Uani 1 1 d . . . H13A H 0.3446 0.6679 0.5831 0.067 Uiso 1 1 calc R . . C11 C 0.21794(14) 0.73003(13) 0.44050(16) 0.0715(7) Uani 1 1 d . . . H11A H 0.2514 0.7760 0.4458 0.086 Uiso 1 1 calc R . . H11B H 0.1683 0.7515 0.4288 0.086 Uiso 1 1 calc R . . C17 C 0.04667(13) 0.64419(13) -0.0215(2) 0.0696(7) Uani 1 1 d . . . H17A H 0.0389 0.6830 0.0325 0.084 Uiso 1 1 calc R . . N1 N 0.46349(10) 0.43805(11) 0.15427(17) 0.0709(5) Uani 1 1 d . . . C15 C 0.10892(12) 0.53495(14) 0.11732(16) 0.0633(6) Uani 1 1 d . . . H15A H 0.1252 0.4795 0.1082 0.076 Uiso 1 1 calc R . . H15B H 0.0709 0.5329 0.1626 0.076 Uiso 1 1 calc R . . C16 C 0.07704(12) 0.53472(13) -0.10223(17) 0.0613(6) Uani 1 1 d . . . H16A H 0.0951 0.4827 -0.1112 0.074 Uiso 1 1 calc R . . C3 C 0.43059(13) 0.50455(14) 0.1080(2) 0.0657(6) Uani 1 1 d . . . H3A H 0.4236 0.5172 0.0291 0.079 Uiso 1 1 calc R . . C4 C 0.37043(13) 0.63051(12) 0.1640(2) 0.0659(6) Uani 1 1 d . . . H4B H 0.3614 0.6425 0.0812 0.079 Uiso 1 1 calc R . . H4C H 0.4019 0.6731 0.2049 0.079 Uiso 1 1 calc R . . C18 C 0.02921(12) 0.65068(14) -0.1377(2) 0.0729(7) Uani 1 1 d . . . H18A H 0.0072 0.6963 -0.1778 0.088 Uiso 1 1 calc R . . C12 C 0.18506(14) 0.65996(15) 0.6136(2) 0.0684(7) Uani 1 1 d . . . H12B H 0.1345 0.6686 0.5956 0.082 Uiso 1 1 calc R . . C2 C 0.46206(13) 0.44486(15) 0.2703(2) 0.0728(7) Uani 1 1 d . . . H2A H 0.4815 0.4066 0.3271 0.087 Uiso 1 1 calc R . . C14 C 0.22395(17) 0.62049(14) 0.7076(2) 0.0706(7) Uani 1 1 d . . . H14A H 0.2039 0.5971 0.7662 0.085 Uiso 1 1 calc R . . C1 C 0.42885(13) 0.51417(15) 0.2908(2) 0.0733(7) Uani 1 1 d . . . H1B H 0.4214 0.5326 0.3624 0.088 Uiso 1 1 calc R . . O1W O 0.53946(8) 0.20391(9) 0.98045(12) 0.0721(4) Uani 1 1 d . . . O2W O 0.58169(9) 0.34602(10) 0.11064(13) 0.0866(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N9 0.0445(11) 0.0479(9) 0.0479(8) -0.0013(7) 0.0072(8) 0.0032(8) C26 0.0441(13) 0.0493(11) 0.0460(10) 0.0022(8) -0.0018(9) -0.0044(9) N8 0.0465(11) 0.0613(10) 0.0419(8) -0.0022(7) 0.0042(7) -0.0065(8) C25 0.0439(13) 0.0452(10) 0.0464(10) 0.0026(8) 0.0103(9) -0.0013(9) C27 0.0486(14) 0.0431(10) 0.0418(9) 0.0028(7) 0.0047(9) 0.0023(9) C23 0.0427(14) 0.0583(12) 0.0399(9) 0.0031(8) 0.0057(9) -0.0047(10) N11 0.0568(12) 0.0524(9) 0.0426(8) -0.0065(7) 0.0055(8) 0.0038(8) N7 0.0585(13) 0.0707(12) 0.0542(10) 0.0008(9) 0.0047(9) -0.0007(9) C30 0.0513(15) 0.0703(13) 0.0518(11) 0.0019(10) 0.0020(11) -0.0014(11) C28 0.0447(13) 0.0539(11) 0.0425(10) 0.0033(8) 0.0064(9) 0.0040(9) C22 0.0492(14) 0.0795(14) 0.0438(10) 0.0052(10) 0.0034(9) -0.0126(11) C33 0.0684(16) 0.0477(11) 0.0465(10) -0.0043(8) 0.0036(10) -0.0003(10) C24 0.0558(15) 0.0501(11) 0.0430(10) -0.0050(8) 0.0078(10) -0.0070(10) C32 0.0710(18) 0.0685(14) 0.0515(12) 0.0052(10) 0.0147(12) 0.0091(12) N10 0.0570(13) 0.0785(12) 0.0675(11) 0.0104(10) 0.0113(10) -0.0033(10) C35 0.0669(17) 0.0721(14) 0.0547(12) -0.0107(11) -0.0039(11) 0.0059(11) C29 0.0557(15) 0.0489(11) 0.0618(12) 0.0048(9) 0.0149(11) 0.0022(10) C20 0.0696(17) 0.0759(15) 0.0441(11) -0.0056(10) 0.0114(11) -0.0076(12) C21 0.0526(15) 0.0710(14) 0.0508(11) -0.0061(10) 0.0072(10) 0.0045(11) N12 0.1026(19) 0.0856(14) 0.0526(11) -0.0017(10) -0.0003(12) 0.0217(13) C19 0.0696(17) 0.0606(13) 0.0493(11) -0.0098(10) 0.0108(11) -0.0020(11) C31 0.0642(16) 0.0692(14) 0.0455(11) -0.0044(10) -0.0010(11) -0.0022(12) C34 0.0744(19) 0.0773(16) 0.0642(14) -0.0013(12) 0.0200(13) -0.0084(13) C36 0.123(3) 0.0706(16) 0.0603(14) 0.0053(12) 0.0347(16) 0.0116(16) N5 0.0474(11) 0.0522(9) 0.0483(9) -0.0040(7) -0.0014(7) -0.0092(8) C7 0.0498(15) 0.0462(11) 0.0444(10) -0.0017(8) -0.0006(10) 0.0070(9) N3 0.0512(12) 0.0614(10) 0.0480(9) -0.0159(8) 0.0045(9) 0.0024(9) C5 0.0381(14) 0.0440(10) 0.0576(11) 0.0100(9) 0.0106(10) -0.0001(9) C9 0.0407(14) 0.0526(11) 0.0407(9) 0.0018(8) 0.0066(9) -0.0113(9) C10 0.0576(16) 0.0477(11) 0.0436(10) -0.0028(8) 0.0096(10) -0.0021(10) C8 0.0462(14) 0.0568(11) 0.0433(10) 0.0056(8) 0.0081(9) 0.0006(9) N2 0.0448(12) 0.0580(10) 0.0651(10) 0.0158(9) 0.0167(9) 0.0044(8) C6 0.0499(15) 0.0433(10) 0.0541(11) 0.0010(8) -0.0104(10) -0.0048(9) N4 0.0708(16) 0.0650(11) 0.0529(10) -0.0061(8) 0.0034(10) -0.0054(10) N6 0.0822(15) 0.0813(13) 0.0542(10) 0.0011(10) -0.0046(10) 0.0027(11) C13 0.0481(15) 0.0616(12) 0.0550(12) -0.0092(10) 0.0069(11) -0.0016(10) C11 0.094(2) 0.0600(13) 0.0525(12) -0.0092(10) -0.0015(11) 0.0178(12) C17 0.0692(17) 0.0606(14) 0.0729(15) -0.0155(11) 0.0009(12) 0.0056(12) N1 0.0684(14) 0.0615(11) 0.0806(13) 0.0052(10) 0.0107(11) 0.0071(10) C15 0.0642(16) 0.0711(13) 0.0493(11) 0.0039(10) -0.0003(10) -0.0245(11) C16 0.0614(15) 0.0618(13) 0.0556(12) -0.0081(10) 0.0009(11) 0.0031(11) C3 0.0641(17) 0.0671(14) 0.0642(13) 0.0078(11) 0.0095(12) 0.0033(12) C4 0.0542(16) 0.0548(12) 0.0890(15) 0.0188(11) 0.0159(13) 0.0026(10) C18 0.0674(17) 0.0609(14) 0.0781(15) 0.0057(12) -0.0128(13) 0.0018(12) C12 0.0485(16) 0.0822(16) 0.0743(15) -0.0285(13) 0.0127(14) -0.0127(13) C2 0.0664(18) 0.0704(16) 0.0819(17) 0.0294(12) 0.0167(13) 0.0114(12) C14 0.080(2) 0.0718(15) 0.0653(14) -0.0174(12) 0.0264(15) -0.0223(13) C1 0.0766(19) 0.0816(17) 0.0660(14) 0.0235(12) 0.0249(13) 0.0175(14) O1W 0.0699(12) 0.0707(10) 0.0742(9) 0.0049(8) 0.0118(8) 0.0069(8) O2W 0.0891(13) 0.0935(12) 0.0667(9) -0.0192(8) -0.0074(8) 0.0238(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 N9 C30 1.339(2) . ? N9 C31 1.357(2) . ? N9 C29 1.464(2) . ? C26 C27 1.384(3) . ? C26 C25 1.385(2) . ? N8 C21 1.336(2) . ? N8 C19 1.360(2) . ? N8 C22 1.470(2) . ? C25 C24 1.387(3) . ? C25 C29 1.504(3) . ? C27 C28 1.385(3) . ? C27 C33 1.512(2) . ? C23 C24 1.383(3) . ? C23 C28 1.386(2) . ? C23 C22 1.514(3) . ? N11 C35 1.336(3) . ? N11 C34 1.357(3) . ? N11 C33 1.460(2) . ? N7 C21 1.315(2) . ? N7 C20 1.365(3) . ? C30 N10 1.310(3) . ? C32 C31 1.344(3) . ? C32 N10 1.366(3) . ? C35 N12 1.313(3) . ? C20 C19 1.340(3) . ? N12 C36 1.356(3) . ? C34 C36 1.351(3) . ? N5 C16 1.343(2) . ? N5 C17 1.358(2) . ? N5 C15 1.467(2) . ? C7 C6 1.379(3) . ? C7 C8 1.382(3) . ? C7 C11 1.508(3) . ? N3 C13 1.344(2) . ? N3 C12 1.358(3) . ? N3 C11 1.465(3) . ? C5 C6 1.381(3) . ? C5 C10 1.391(3) . ? C5 C4 1.512(3) . ? C9 C10 1.372(3) . ? C9 C8 1.389(3) . ? C9 C15 1.509(3) . ? N2 C3 1.331(3) . ? N2 C1 1.361(2) . ? N2 C4 1.459(2) . ? N4 C13 1.316(3) . ? N4 C14 1.365(3) . ? N6 C16 1.310(2) . ? N6 C18 1.355(3) . ? C17 C18 1.336(3) . ? N1 C3 1.309(3) . ? N1 C2 1.371(3) . ? C12 C14 1.348(3) . ? C2 C1 1.338(3) . ? 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 C30 N9 C31 106.11(18) . . ? C30 N9 C29 126.01(16) . . ? C31 N9 C29 127.87(18) . . ? C27 C26 C25 121.60(17) . . ? C21 N8 C19 106.62(16) . . ? C21 N8 C22 126.44(18) . . ? C19 N8 C22 126.89(17) . . ? C26 C25 C24 118.32(18) . . ? C26 C25 C29 120.75(17) . . ? C24 C25 C29 120.92(17) . . ? C26 C27 C28 118.66(17) . . ? C26 C27 C33 120.36(17) . . ? C28 C27 C33 120.96(18) . . ? C24 C23 C28 118.79(17) . . ? C24 C23 C22 120.93(18) . . ? C28 C23 C22 120.25(19) . . ? C35 N11 C34 106.41(19) . . ? C35 N11 C33 126.8(2) . . ? C34 N11 C33 126.62(17) . . ? C21 N7 C20 104.30(18) . . ? N10 C30 N9 112.82(18) . . ? C27 C28 C23 121.16(19) . . ? N8 C22 C23 112.73(16) . . ? N11 C33 C27 111.72(15) . . ? C23 C24 C25 121.45(17) . . ? C31 C32 N10 110.42(19) . . ? C30 N10 C32 104.13(19) . . ? N12 C35 N11 112.7(2) . . ? N9 C29 C25 112.25(16) . . ? C19 C20 N7 110.60(18) . . ? N7 C21 N8 112.25(19) . . ? C35 N12 C36 104.1(2) . . ? C20 C19 N8 106.23(19) . . ? C32 C31 N9 106.51(19) . . ? C36 C34 N11 105.9(2) . . ? C34 C36 N12 110.8(2) . . ? C16 N5 C17 106.01(17) . . ? C16 N5 C15 127.01(17) . . ? C17 N5 C15 126.95(18) . . ? C6 C7 C8 118.62(18) . . ? C6 C7 C11 119.93(19) . . ? C8 C7 C11 121.5(2) . . ? C13 N3 C12 106.9(2) . . ? C13 N3 C11 127.0(2) . . ? C12 N3 C11 126.1(2) . . ? C6 C5 C10 118.3(2) . . ? C6 C5 C4 120.44(19) . . ? C10 C5 C4 121.28(19) . . ? C10 C9 C8 118.99(17) . . ? C10 C9 C15 120.08(18) . . ? C8 C9 C15 120.9(2) . . ? C9 C10 C5 121.29(18) . . ? C7 C8 C9 121.0(2) . . ? C3 N2 C1 106.35(17) . . ? C3 N2 C4 127.22(18) . . ? C1 N2 C4 126.4(2) . . ? C7 C6 C5 121.78(18) . . ? C13 N4 C14 104.82(19) . . ? C16 N6 C18 104.09(17) . . ? N4 C13 N3 111.7(2) . . ? N3 C11 C7 112.87(16) . . ? C18 C17 N5 106.2(2) . . ? C3 N1 C2 103.8(2) . . ? N5 C15 C9 111.78(16) . . ? N6 C16 N5 112.47(19) . . ? N1 C3 N2 113.0(2) . . ? N2 C4 C5 112.13(17) . . ? C17 C18 N6 111.2(2) . . ? C14 C12 N3 106.2(2) . . ? C1 C2 N1 110.7(2) . . ? C12 C14 N4 110.3(2) . . ? C2 C1 N2 106.2(2) . . ? _diffrn_measured_fraction_theta_max 0.731 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.731 _refine_diff_density_max 0.345 _refine_diff_density_min -0.125 _refine_diff_density_rms 0.031