# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2150 data_complex7b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 B2 N6 O2 W' _chemical_formula_weight 606.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 14.425(7) _cell_length_b 10.168(6) _cell_length_c 16.623(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.35(4) _cell_angle_gamma 90.00 _cell_volume 2436(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 17.2 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 4.771 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 8 _diffrn_reflns_number 6418 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1058 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 29.00 _reflns_number_total 6418 _reflns_number_gt 4136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (C.K.Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0427P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6418 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.20458(2) 0.18203(3) -0.008879(18) 0.02360(8) Uani 1 d . . . O1 O 0.1676(5) 0.4411(6) -0.1051(4) 0.0484(16) Uani 1 d . . . O2 O 0.3085(4) 0.3377(6) 0.1290(3) 0.0428(15) Uani 1 d . . . N1 N 0.1624(4) 0.0506(7) -0.1130(4) 0.0285(14) Uani 1 d . . . N2 N 0.2138(5) -0.0631(7) -0.1266(4) 0.0304(15) Uani 1 d . . . N3 N 0.2375(4) -0.0065(6) 0.0572(3) 0.0231(13) Uani 1 d . . . N4 N 0.2702(4) -0.1110(6) 0.0139(4) 0.0233(13) Uani 1 d . . . N5 N 0.3415(4) 0.1544(6) -0.0583(4) 0.0263(14) Uani 1 d . . . N6 N 0.3675(4) 0.0263(6) -0.0765(3) 0.0240(13) Uani 1 d . . . B1 B 0.1208(7) 0.2997(10) 0.0586(6) 0.034(2) Uani 1 d . . . B2 B 0.2990(7) -0.0915(9) -0.0726(6) 0.0310(19) Uani 1 d . . . C1 C 0.0478(6) 0.1805(10) 0.0462(5) 0.0351(17) Uani 1 d . . . C2 C -0.0466(6) 0.2325(10) 0.0139(5) 0.043(2) Uani 1 d . . . H2A H -0.0882 0.1592 0.0029 0.076(16) Uiso 1 calc R . . H2B H -0.0383 0.2815 -0.0354 0.076(16) Uiso 1 calc R . . H2C H -0.0729 0.2898 0.0537 0.076(16) Uiso 1 calc R . . C3 C 0.0960(7) 0.4286(10) 0.1040(6) 0.049(2) Uani 1 d . . . H3A H 0.1514 0.4845 0.1077 0.07(2) Uiso 1 calc R . . H3B H 0.0485 0.4759 0.0716 0.07(2) Uiso 1 calc R . . C4 C 0.0610(9) 0.4100(14) 0.1877(6) 0.076(4) Uani 1 d . . . H4A H 0.0053 0.3564 0.1850 0.076(16) Uiso 1 calc R . . H4B H 0.0470 0.4950 0.2107 0.076(16) Uiso 1 calc R . . H4C H 0.1083 0.3665 0.2213 0.076(16) Uiso 1 calc R . . C5 C 0.1817(6) 0.3446(8) -0.0697(5) 0.0325(19) Uani 1 d . . . C6 C 0.2668(6) 0.2792(8) 0.0770(5) 0.0349(19) Uani 1 d . . . C7 C 0.0937(5) 0.0525(9) -0.1719(5) 0.0333(18) Uani 1 d . . . C8 C 0.1009(6) -0.0581(10) -0.2207(5) 0.038(2) Uani 1 d . . . C9 C 0.1781(6) -0.1278(9) -0.1921(5) 0.0347(19) Uani 1 d . . . C10 C 0.0246(6) 0.1614(9) -0.1795(5) 0.045(2) Uani 1 d . . . H10A H -0.0256 0.1450 -0.1436 0.076(8) Uiso 1 calc R . . H10B H -0.0001 0.1660 -0.2345 0.076(8) Uiso 1 calc R . . H10C H 0.0545 0.2440 -0.1651 0.076(8) Uiso 1 calc R . . C11 C 0.2180(7) -0.2537(9) -0.2219(5) 0.046(2) Uani 1 d . . . H11A H 0.1797 -0.2863 -0.2669 0.076(8) Uiso 1 calc R . . H11B H 0.2196 -0.3183 -0.1789 0.076(8) Uiso 1 calc R . . H11C H 0.2804 -0.2382 -0.2392 0.076(8) Uiso 1 calc R . . C12 C 0.2253(5) -0.0494(8) 0.1317(4) 0.0285(16) Uani 1 d . . . C13 C 0.2476(5) -0.1820(9) 0.1373(5) 0.0314(16) Uani 1 d . . . C14 C 0.2765(6) -0.2196(7) 0.0623(5) 0.0297(17) Uani 1 d . . . C15 C 0.1976(7) 0.0393(9) 0.1986(4) 0.039(2) Uani 1 d . . . H15A H 0.2415 0.0298 0.2440 0.076(8) Uiso 1 calc R . . H15B H 0.1360 0.0156 0.2149 0.076(8) Uiso 1 calc R . . H15C H 0.1974 0.1298 0.1801 0.076(8) Uiso 1 calc R . . C16 C 0.3089(6) -0.3480(8) 0.0323(6) 0.042(2) Uani 1 d . . . H16A H 0.3201 -0.4074 0.0773 0.076(8) Uiso 1 calc R . . H16B H 0.3660 -0.3357 0.0043 0.076(8) Uiso 1 calc R . . H16C H 0.2619 -0.3851 -0.0044 0.076(8) Uiso 1 calc R . . C17 C 0.4134(5) 0.2318(8) -0.0733(5) 0.0279(16) Uani 1 d . . . C18 C 0.4857(5) 0.1566(9) -0.1019(5) 0.034(2) Uani 1 d . . . C19 C 0.4556(5) 0.0291(8) -0.1023(4) 0.0287(16) Uani 1 d . . . C20 C 0.4113(7) 0.3756(8) -0.0590(5) 0.037(2) Uani 1 d . . . H20A H 0.4646 0.4162 -0.0826 0.076(8) Uiso 1 calc R . . H20B H 0.4132 0.3925 -0.0015 0.076(8) Uiso 1 calc R . . H20C H 0.3548 0.4122 -0.0834 0.076(8) Uiso 1 calc R . . C21 C 0.5062(6) -0.0936(9) -0.1249(5) 0.039(2) Uani 1 d . . . H21A H 0.5021 -0.1581 -0.0821 0.076(8) Uiso 1 calc R . . H21B H 0.5709 -0.0729 -0.1327 0.076(8) Uiso 1 calc R . . H21C H 0.4784 -0.1292 -0.1743 0.076(8) Uiso 1 calc R . . H1B H 0.037(5) 0.141(7) 0.100(4) 0.017(19) Uiso 1 d . . . H2 H 0.333(5) -0.170(8) -0.093(4) 0.03(2) Uiso 1 d . . . H8 H 0.068(5) -0.062(8) -0.268(4) 0.03(2) Uiso 1 d . . . H13 H 0.239(6) -0.228(9) 0.184(5) 0.05(3) Uiso 1 d . . . H18 H 0.542(5) 0.195(7) -0.118(4) 0.012(16) Uiso 1 d . . . H1A H 0.061(5) 0.121(8) 0.016(4) 0.02(2) Uiso 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 W1 0.02415(13) 0.02087(13) 0.02588(13) 0.00029(16) 0.00223(9) -0.00002(17) O1 0.057(4) 0.036(4) 0.052(4) 0.016(3) -0.003(3) 0.004(3) O2 0.051(4) 0.038(4) 0.039(3) -0.007(3) -0.005(3) 0.003(3) N1 0.028(3) 0.028(3) 0.029(3) -0.004(3) 0.000(3) -0.002(3) N2 0.032(4) 0.032(4) 0.027(3) -0.004(3) -0.001(3) -0.005(3) N3 0.028(3) 0.020(3) 0.021(3) 0.002(2) -0.001(2) 0.002(3) N4 0.025(3) 0.016(3) 0.029(3) 0.000(2) 0.004(3) 0.002(2) N5 0.025(3) 0.025(4) 0.030(3) 0.001(3) 0.007(2) 0.000(3) N6 0.026(3) 0.020(3) 0.026(3) 0.004(2) 0.006(2) 0.002(3) B1 0.036(5) 0.032(5) 0.034(4) -0.001(4) 0.006(4) 0.005(4) B2 0.028(5) 0.024(4) 0.041(5) 0.000(4) -0.002(4) 0.008(4) C1 0.032(4) 0.030(4) 0.044(5) 0.003(5) 0.005(3) 0.002(4) C2 0.031(5) 0.049(5) 0.047(5) -0.001(4) 0.003(4) 0.001(4) C3 0.041(5) 0.052(6) 0.054(6) -0.005(5) -0.003(4) 0.002(5) C4 0.072(8) 0.109(11) 0.048(6) -0.029(7) 0.004(6) 0.020(8) C5 0.037(4) 0.035(5) 0.026(4) 0.002(3) 0.002(3) 0.002(4) C6 0.037(5) 0.034(5) 0.033(4) 0.002(3) 0.006(4) 0.005(4) C7 0.022(4) 0.040(5) 0.037(4) 0.002(4) 0.005(3) -0.002(4) C8 0.044(5) 0.047(5) 0.021(4) -0.001(4) -0.003(3) -0.002(4) C9 0.043(5) 0.034(4) 0.027(4) -0.005(3) 0.005(3) -0.009(4) C10 0.036(5) 0.049(6) 0.048(5) -0.002(4) -0.007(4) 0.003(4) C11 0.057(6) 0.050(6) 0.032(5) -0.018(4) 0.000(4) 0.003(5) C12 0.033(4) 0.030(4) 0.023(3) -0.001(3) 0.006(3) -0.002(3) C13 0.033(4) 0.029(4) 0.032(4) 0.014(4) 0.000(3) -0.003(4) C14 0.035(4) 0.019(4) 0.035(4) 0.004(3) -0.002(3) 0.003(3) C15 0.060(6) 0.032(5) 0.025(4) 0.001(3) -0.002(4) -0.001(4) C16 0.042(5) 0.023(4) 0.062(6) 0.004(4) 0.007(4) 0.001(4) C17 0.027(4) 0.029(4) 0.028(4) -0.003(3) 0.000(3) -0.009(3) C18 0.023(4) 0.043(6) 0.035(4) -0.003(4) 0.004(3) -0.007(3) C19 0.027(4) 0.035(4) 0.025(4) 0.001(3) 0.005(3) -0.003(3) C20 0.044(5) 0.027(4) 0.040(5) -0.006(4) 0.005(4) -0.008(4) C21 0.036(5) 0.040(5) 0.041(5) 0.000(4) 0.007(4) 0.017(4) _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 W1 C6 1.928(9) . ? W1 C5 1.959(8) . ? W1 B1 2.064(9) . ? W1 N5 2.188(6) . ? W1 N1 2.250(6) . ? W1 N3 2.250(6) . ? W1 C1 2.475(8) . ? O1 C5 1.158(9) . ? O2 C6 1.191(10) . ? N1 C7 1.366(10) . ? N1 N2 1.397(9) . ? N2 C9 1.355(10) . ? N2 B2 1.519(11) . ? N3 C12 1.332(9) . ? N3 N4 1.377(8) . ? N4 C14 1.368(9) . ? N4 B2 1.525(11) . ? N5 C17 1.334(9) . ? N5 N6 1.393(8) . ? N6 C19 1.358(9) . ? N6 B2 1.556(11) . ? B1 C3 1.561(13) . ? B1 C1 1.613(14) . ? B2 H2 1.01(8) . ? C1 C2 1.537(12) . ? C1 H1B 1.00(7) . ? C1 H1A 0.82(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.513(13) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C7 C8 1.393(12) . ? C7 C10 1.492(12) . ? C8 C9 1.388(12) . ? C8 H8 0.90(7) . ? C9 C11 1.496(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.389(12) . ? C12 C15 1.498(11) . ? C13 C14 1.384(11) . ? C13 H13 0.91(9) . ? C14 C16 1.480(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.392(11) . ? C17 C20 1.482(11) . ? C18 C19 1.367(11) . ? C18 H18 0.95(7) . ? C19 C21 1.502(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 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 C6 W1 C5 90.7(3) . . ? C6 W1 B1 64.2(4) . . ? C5 W1 B1 72.6(4) . . ? C6 W1 N5 86.8(3) . . ? C5 W1 N5 92.9(3) . . ? B1 W1 N5 146.7(3) . . ? C6 W1 N1 167.7(3) . . ? C5 W1 N1 94.0(3) . . ? B1 W1 N1 128.1(3) . . ? N5 W1 N1 81.6(2) . . ? C6 W1 N3 89.6(3) . . ? C5 W1 N3 177.0(3) . . ? B1 W1 N3 110.2(3) . . ? N5 W1 N3 84.1(2) . . ? N1 W1 N3 85.1(2) . . ? C6 W1 C1 97.7(3) . . ? C5 W1 C1 93.4(3) . . ? B1 W1 C1 40.4(4) . . ? N5 W1 C1 172.3(3) . . ? N1 W1 C1 93.4(3) . . ? N3 W1 C1 89.5(3) . . ? C7 N1 N2 105.7(6) . . ? C7 N1 W1 135.1(6) . . ? N2 N1 W1 119.2(5) . . ? C9 N2 N1 110.2(7) . . ? C9 N2 B2 130.9(7) . . ? N1 N2 B2 118.8(6) . . ? C12 N3 N4 107.1(6) . . ? C12 N3 W1 134.4(5) . . ? N4 N3 W1 118.2(4) . . ? C14 N4 N3 109.4(6) . . ? C14 N4 B2 130.2(6) . . ? N3 N4 B2 120.3(6) . . ? C17 N5 N6 107.0(6) . . ? C17 N5 W1 135.7(5) . . ? N6 N5 W1 117.2(4) . . ? C19 N6 N5 108.2(6) . . ? C19 N6 B2 129.4(7) . . ? N5 N6 B2 122.3(6) . . ? C3 B1 C1 122.1(8) . . ? C3 B1 W1 154.2(7) . . ? C1 B1 W1 83.6(5) . . ? N2 B2 N4 109.7(7) . . ? N2 B2 N6 109.1(7) . . ? N4 B2 N6 109.7(7) . . ? N2 B2 H2 110(4) . . ? N4 B2 H2 112(4) . . ? N6 B2 H2 106(4) . . ? C2 C1 B1 110.5(8) . . ? C2 C1 W1 132.7(6) . . ? B1 C1 W1 56.0(4) . . ? C2 C1 H1B 107(4) . . ? B1 C1 H1B 108(4) . . ? W1 C1 H1B 121(4) . . ? C2 C1 H1A 105(6) . . ? B1 C1 H1A 118(6) . . ? W1 C1 H1A 63(5) . . ? H1B C1 H1A 107(7) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 B1 115.6(9) . . ? C4 C3 H3A 108.4 . . ? B1 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? B1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 W1 179.4(7) . . ? O2 C6 W1 177.4(7) . . ? N1 C7 C8 109.7(7) . . ? N1 C7 C10 122.3(8) . . ? C8 C7 C10 128.0(8) . . ? C9 C8 C7 106.9(7) . . ? C9 C8 H8 131(5) . . ? C7 C8 H8 119(5) . . ? N2 C9 C8 107.5(8) . . ? N2 C9 C11 122.9(8) . . ? C8 C9 C11 129.6(8) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 110.0(7) . . ? N3 C12 C15 122.9(7) . . ? C13 C12 C15 127.0(7) . . ? C14 C13 C12 106.6(7) . . ? C14 C13 H13 133(6) . . ? C12 C13 H13 121(6) . . ? N4 C14 C13 107.0(7) . . ? N4 C14 C16 121.9(7) . . ? C13 C14 C16 131.2(8) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 109.8(7) . . ? N5 C17 C20 122.1(8) . . ? C18 C17 C20 128.1(8) . . ? C19 C18 C17 106.3(7) . . ? C19 C18 H18 132(4) . . ? C17 C18 H18 122(4) . . ? N6 C19 C18 108.7(7) . . ? N6 C19 C21 122.2(7) . . ? C18 C19 C21 129.1(7) . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.076 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.194 #===END data_complex14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H47 B O4 W' _chemical_formula_weight 678.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.829(14) _cell_length_b 12.33(2) _cell_length_c 14.24(2) _cell_angle_alpha 103.00(13) _cell_angle_beta 97.29(13) _cell_angle_gamma 97.15(13) _cell_volume 1480(4) _cell_formula_units_Z 2 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.6 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 3.936 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1563 _exptl_absorpt_correction_T_max 0.3162 _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2 _diffrn_reflns_number 6129 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6129 _reflns_number_gt 5762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (C.K.Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.2283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6129 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.396528(15) 0.264287(11) 0.721406(9) 0.02412(6) Uani 1 d . . . O1 O 0.6772(4) 0.1745(3) 0.6354(3) 0.0525(9) Uani 1 d . . . O2 O 0.4024(4) 0.2629(3) 0.9369(2) 0.0399(7) Uani 1 d . . . O3 O 0.9027(4) 0.7745(3) 0.7489(3) 0.0435(7) Uani 1 d . . . O4 O 0.9289(3) 0.5834(2) 0.7501(2) 0.0350(6) Uani 1 d . . . B1 B 0.9678(5) 0.6803(4) 0.7219(3) 0.0354(10) Uani 1 d . . . C1 C 0.5769(5) 0.2091(3) 0.6718(3) 0.0350(8) Uani 1 d . . . C2 C 0.4660(4) 0.2317(3) 0.8668(3) 0.0295(8) Uani 1 d . . . C3 C 0.6034(5) 0.1682(4) 0.8825(3) 0.0423(10) Uani 1 d . . . H3A H 0.5816 0.0947 0.8353 0.048(5) Uiso 1 calc R . . H3B H 0.6957 0.2106 0.8685 0.048(5) Uiso 1 calc R . . C4 C 0.6394(8) 0.1493(6) 0.9848(4) 0.0714(18) Uani 1 d . . . H4A H 0.7308 0.1133 0.9895 0.066(4) Uiso 1 calc R . . H4B H 0.5524 0.1013 0.9974 0.066(4) Uiso 1 calc R . . H4C H 0.6578 0.2212 1.0326 0.066(4) Uiso 1 calc R . . C5 C 0.5865(4) 0.4122(3) 0.8116(3) 0.0290(7) Uani 1 d . . . H5 H 0.6100 0.3652 0.8532 0.114(16) Uiso 1 calc R . . C6 C 0.4371(4) 0.4471(3) 0.8046(3) 0.0292(8) Uani 1 d . . . C7 C 0.3722(4) 0.4389(3) 0.7066(3) 0.0326(8) Uani 1 d . . . H7 H 0.2742 0.4584 0.6907 0.114(16) Uiso 1 calc R . . C8 C 0.4615(5) 0.3998(3) 0.6331(3) 0.0340(8) Uani 1 d . . . H8 H 0.4121 0.3502 0.5739 0.114(16) Uiso 1 calc R . . C9 C 0.6308(5) 0.4359(3) 0.6483(3) 0.0319(8) Uani 1 d . . . C10 C 0.7079(4) 0.4497(3) 0.7533(3) 0.0287(7) Uani 1 d . . . H10 H 0.7820 0.3955 0.7508 0.030(11) Uiso 1 calc R . . C11 C 0.8030(4) 0.5680(3) 0.8052(3) 0.0312(8) Uani 1 d . . . C12 C 0.7043(5) 0.6609(3) 0.8046(3) 0.0341(8) Uani 1 d . . . H12A H 0.6431 0.6631 0.8576 0.048(5) Uiso 1 calc R . . H12B H 0.6315 0.6400 0.7431 0.048(5) Uiso 1 calc R . . C13 C 0.7901(5) 0.7800(4) 0.8156(3) 0.0385(9) Uani 1 d . . . C14 C 0.3601(5) 0.4963(4) 0.8897(3) 0.0404(10) Uani 1 d . . . H14A H 0.4079 0.5740 0.9181 0.052(8) Uiso 1 calc R . . H14B H 0.3721 0.4531 0.9385 0.052(8) Uiso 1 calc R . . H14C H 0.2510 0.4935 0.8672 0.052(8) Uiso 1 calc R . . C15 C 0.7047(6) 0.4468(4) 0.5738(3) 0.0423(10) Uani 1 d . . . C16 C 0.8787(5) 0.5655(4) 0.9078(3) 0.0411(10) Uani 1 d . . . H16A H 0.9117 0.4930 0.9057 0.066(4) Uiso 1 calc R . . H16B H 0.8046 0.5772 0.9524 0.066(4) Uiso 1 calc R . . H16C H 0.9677 0.6248 0.9300 0.066(4) Uiso 1 calc R . . C17 C 0.6786(6) 0.8536(4) 0.7834(4) 0.0529(12) Uani 1 d . . . H17A H 0.6009 0.8610 0.8259 0.066(4) Uiso 1 calc R . . H17B H 0.6286 0.8193 0.7167 0.066(4) Uiso 1 calc R . . H17C H 0.7348 0.9275 0.7868 0.066(4) Uiso 1 calc R . . C18 C 0.8761(8) 0.8370(5) 0.9175(4) 0.0636(15) Uani 1 d . . . H18A H 0.8061 0.8345 0.9646 0.066(4) Uiso 1 calc R . . H18B H 0.9158 0.9148 0.9204 0.066(4) Uiso 1 calc R . . H18C H 0.9614 0.7980 0.9327 0.066(4) Uiso 1 calc R . . C19 C 1.1017(5) 0.6829(5) 0.6583(3) 0.0456(11) Uani 1 d . . . H19A H 1.0932 0.6088 0.6132 0.048(5) Uiso 1 calc R . . H19B H 1.0890 0.7382 0.6193 0.048(5) Uiso 1 calc R . . C20 C 1.2618(6) 0.7130(4) 0.7204(4) 0.0509(12) Uani 1 d . . . H20A H 1.3399 0.7135 0.6782 0.066(4) Uiso 1 calc R . . H20B H 1.2759 0.6575 0.7581 0.066(4) Uiso 1 calc R . . H20C H 1.2716 0.7869 0.7643 0.066(4) Uiso 1 calc R . . C21 C 0.2308(5) 0.1510(3) 0.5869(3) 0.0315(8) Uani 1 d . . . C22 C 0.2786(4) 0.0766(3) 0.6451(3) 0.0291(8) Uani 1 d . . . C23 C 0.2198(4) 0.1047(3) 0.7350(3) 0.0288(7) Uani 1 d . . . C24 C 0.1378(4) 0.1978(3) 0.7340(3) 0.0317(8) Uani 1 d . . . C25 C 0.1415(4) 0.2244(3) 0.6416(3) 0.0301(8) Uani 1 d . . . C26 C 0.2475(5) 0.1389(4) 0.4811(3) 0.0358(9) Uani 1 d . . . H26A H 0.3482 0.1168 0.4709 0.048(5) Uiso 1 calc R . . H26B H 0.2442 0.2117 0.4648 0.048(5) Uiso 1 calc R . . C27 C 0.1195(6) 0.0509(4) 0.4135(3) 0.0446(11) Uani 1 d . . . H27A H 0.1315 0.0471 0.3461 0.066(4) Uiso 1 calc R . . H27B H 0.0196 0.0718 0.4243 0.066(4) Uiso 1 calc R . . H27C H 0.1260 -0.0221 0.4272 0.066(4) Uiso 1 calc R . . C28 C 0.3571(5) -0.0225(3) 0.6135(3) 0.0397(9) Uani 1 d . . . H28A H 0.2808 -0.0904 0.5925 0.053(4) Uiso 1 calc R . . H28B H 0.4313 -0.0288 0.6676 0.053(4) Uiso 1 calc R . . H28C H 0.4104 -0.0128 0.5597 0.053(4) Uiso 1 calc R . . C29 C 0.2171(6) 0.0348(4) 0.8082(3) 0.0408(10) Uani 1 d . . . H29A H 0.1293 -0.0255 0.7874 0.053(4) Uiso 1 calc R . . H29B H 0.2083 0.0817 0.8712 0.053(4) Uiso 1 calc R . . H29C H 0.3119 0.0029 0.8135 0.053(4) Uiso 1 calc R . . C30 C 0.0454(5) 0.2448(4) 0.8102(3) 0.0449(11) Uani 1 d . . . H30A H 0.1045 0.2541 0.8745 0.053(4) Uiso 1 calc R . . H30B H -0.0503 0.1935 0.8031 0.053(4) Uiso 1 calc R . . H30C H 0.0222 0.3174 0.8022 0.053(4) Uiso 1 calc R . . C31 C 0.0439(5) 0.3012(4) 0.6015(3) 0.0399(9) Uani 1 d . . . H31A H -0.0535 0.2576 0.5654 0.053(4) Uiso 1 calc R . . H31B H 0.0986 0.3363 0.5583 0.053(4) Uiso 1 calc R . . H31C H 0.0240 0.3591 0.6550 0.053(4) Uiso 1 calc R . . H15A H 0.814(6) 0.468(4) 0.580(3) 0.034(11) Uiso 1 d . . . H15B H 0.640(5) 0.435(4) 0.514(3) 0.028(11) Uiso 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 W1 0.02425(9) 0.02411(9) 0.02380(9) 0.00562(6) 0.00362(5) 0.00371(6) O1 0.0406(18) 0.0476(19) 0.070(2) 0.0041(17) 0.0233(16) 0.0130(15) O2 0.0447(17) 0.0423(17) 0.0311(14) 0.0086(12) 0.0057(12) 0.0017(13) O3 0.0456(18) 0.0407(17) 0.0513(17) 0.0205(13) 0.0199(14) 0.0039(14) O4 0.0300(14) 0.0364(15) 0.0414(15) 0.0131(12) 0.0122(12) 0.0024(11) B1 0.029(2) 0.043(3) 0.033(2) 0.0110(19) 0.0054(17) -0.0017(19) C1 0.032(2) 0.032(2) 0.039(2) 0.0051(16) 0.0065(16) 0.0027(16) C2 0.0272(18) 0.0259(18) 0.0343(19) 0.0052(14) 0.0062(15) 0.0033(14) C3 0.043(2) 0.042(2) 0.045(2) 0.0164(19) -0.0001(19) 0.0116(19) C4 0.091(5) 0.075(4) 0.053(3) 0.024(3) -0.008(3) 0.034(4) C5 0.0301(18) 0.0279(18) 0.0280(18) 0.0077(14) 0.0043(14) -0.0002(15) C6 0.0328(19) 0.0230(17) 0.0306(18) 0.0045(14) 0.0076(15) 0.0008(14) C7 0.0291(19) 0.0258(18) 0.042(2) 0.0110(16) 0.0003(16) 0.0017(15) C8 0.044(2) 0.0292(19) 0.0272(18) 0.0097(15) -0.0005(16) 0.0000(16) C9 0.038(2) 0.0282(19) 0.0295(18) 0.0084(15) 0.0070(15) 0.0037(16) C10 0.0257(17) 0.0305(19) 0.0308(18) 0.0092(15) 0.0050(14) 0.0045(14) C11 0.0270(18) 0.032(2) 0.0338(19) 0.0097(15) 0.0068(15) -0.0014(15) C12 0.034(2) 0.031(2) 0.037(2) 0.0081(16) 0.0094(16) 0.0003(16) C13 0.042(2) 0.034(2) 0.041(2) 0.0105(17) 0.0135(18) 0.0020(18) C14 0.039(2) 0.038(2) 0.043(2) -0.0004(18) 0.0144(18) 0.0078(18) C15 0.045(3) 0.051(3) 0.033(2) 0.0136(19) 0.0116(18) 0.002(2) C16 0.038(2) 0.045(2) 0.036(2) 0.0131(18) -0.0016(17) -0.0075(19) C17 0.057(3) 0.040(3) 0.070(3) 0.020(2) 0.026(3) 0.011(2) C18 0.086(4) 0.044(3) 0.050(3) 0.002(2) 0.006(3) -0.012(3) C19 0.040(2) 0.058(3) 0.042(2) 0.019(2) 0.0140(19) 0.003(2) C20 0.042(3) 0.046(3) 0.068(3) 0.019(2) 0.011(2) 0.010(2) C21 0.036(2) 0.0282(19) 0.0239(17) 0.0022(14) -0.0039(15) -0.0032(15) C22 0.0255(17) 0.0295(19) 0.0305(18) 0.0046(15) 0.0047(14) 0.0029(14) C23 0.0246(17) 0.0291(18) 0.0310(18) 0.0056(15) 0.0051(14) 0.0002(14) C24 0.0276(18) 0.035(2) 0.0289(18) 0.0046(15) 0.0036(15) 0.0000(15) C25 0.0231(17) 0.034(2) 0.0312(18) 0.0063(15) 0.0018(14) 0.0028(15) C26 0.036(2) 0.042(2) 0.0281(19) 0.0078(16) 0.0065(15) 0.0002(17) C27 0.051(3) 0.048(3) 0.028(2) 0.0058(18) 0.0019(18) -0.004(2) C28 0.046(2) 0.027(2) 0.045(2) 0.0031(17) 0.0118(19) 0.0057(17) C29 0.049(2) 0.035(2) 0.037(2) 0.0119(17) 0.0078(18) -0.0049(18) C30 0.036(2) 0.054(3) 0.043(2) 0.005(2) 0.0124(19) 0.006(2) C31 0.035(2) 0.042(2) 0.040(2) 0.0130(18) -0.0048(17) 0.0052(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 W1 C1 1.959(5) . ? W1 C2 2.222(5) . ? W1 C7 2.244(5) . ? W1 C6 2.260(6) . ? W1 C21 2.311(6) . ? W1 C25 2.329(6) . ? W1 C5 2.330(6) . ? W1 C8 2.365(5) . ? W1 C22 2.367(6) . ? W1 C24 2.372(5) . ? W1 C23 2.415(6) . ? O1 C1 1.160(5) . ? O2 C2 1.218(5) . ? O3 B1 1.359(6) . ? O3 C13 1.457(6) . ? O4 B1 1.363(6) . ? O4 C11 1.457(5) . ? B1 C19 1.579(7) . ? C2 C3 1.543(6) . ? C3 C4 1.527(7) . ? C5 C6 1.436(6) . ? C5 C10 1.526(6) . ? C6 C7 1.417(6) . ? C6 C14 1.509(6) . ? C7 C8 1.424(6) . ? C8 C9 1.479(6) . ? C9 C15 1.336(6) . ? C9 C10 1.525(6) . ? C10 C11 1.560(6) . ? C11 C12 1.525(6) . ? C11 C16 1.536(6) . ? C12 C13 1.531(6) . ? C13 C17 1.516(7) . ? C13 C18 1.518(7) . ? C19 C20 1.524(7) . ? C21 C22 1.434(6) . ? C21 C25 1.437(6) . ? C21 C26 1.508(6) . ? C22 C23 1.429(6) . ? C22 C28 1.490(6) . ? C23 C24 1.433(6) . ? C23 C29 1.494(6) . ? C24 C25 1.429(6) . ? C24 C30 1.495(7) . ? C25 C31 1.514(6) . ? C26 C27 1.526(7) . ? 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 C1 W1 C2 92.5(2) . . ? C1 W1 C7 113.7(2) . . ? C2 W1 C7 120.86(18) . . ? C1 W1 C6 115.2(2) . . ? C2 W1 C6 84.5(2) . . ? C7 W1 C6 36.66(16) . . ? C1 W1 C21 91.7(2) . . ? C2 W1 C21 129.40(18) . . ? C7 W1 C21 103.0(2) . . ? C6 W1 C21 137.03(17) . . ? C1 W1 C25 127.30(19) . . ? C2 W1 C25 122.81(17) . . ? C7 W1 C25 82.4(2) . . ? C6 W1 C25 106.7(2) . . ? C21 W1 C25 36.08(16) . . ? C1 W1 C5 81.5(2) . . ? C2 W1 C5 71.69(19) . . ? C7 W1 C5 62.17(18) . . ? C6 W1 C5 36.42(16) . . ? C21 W1 C5 158.36(15) . . ? C25 W1 C5 142.43(17) . . ? C1 W1 C8 80.5(2) . . ? C2 W1 C8 139.00(17) . . ? C7 W1 C8 35.87(16) . . ? C6 W1 C8 63.19(18) . . ? C21 W1 C8 91.36(19) . . ? C25 W1 C8 91.79(19) . . ? C5 W1 C8 67.33(18) . . ? C1 W1 C22 82.0(2) . . ? C2 W1 C22 95.4(2) . . ? C7 W1 C22 138.12(17) . . ? C6 W1 C22 162.80(15) . . ? C21 W1 C22 35.69(16) . . ? C25 W1 C22 59.08(19) . . ? C5 W1 C22 158.45(15) . . ? C8 W1 C22 123.02(18) . . ? C1 W1 C24 140.41(18) . . ? C2 W1 C24 87.46(19) . . ? C7 W1 C24 99.79(19) . . ? C6 W1 C24 104.2(2) . . ? C21 W1 C24 59.54(19) . . ? C25 W1 C24 35.38(15) . . ? C5 W1 C24 135.01(17) . . ? C8 W1 C24 122.96(18) . . ? C22 W1 C24 58.66(18) . . ? C1 W1 C23 108.3(2) . . ? C2 W1 C23 72.25(19) . . ? C7 W1 C23 134.57(17) . . ? C6 W1 C23 131.14(17) . . ? C21 W1 C23 58.67(18) . . ? C25 W1 C23 58.21(18) . . ? C5 W1 C23 142.96(15) . . ? C8 W1 C23 148.26(15) . . ? C22 W1 C23 34.76(15) . . ? C24 W1 C23 34.83(15) . . ? B1 O3 C13 121.3(4) . . ? B1 O4 C11 122.6(3) . . ? O3 B1 O4 123.7(4) . . ? O3 B1 C19 119.3(4) . . ? O4 B1 C19 117.0(4) . . ? O1 C1 W1 174.9(4) . . ? O2 C2 C3 117.0(4) . . ? O2 C2 W1 123.4(3) . . ? C3 C2 W1 119.6(3) . . ? C4 C3 C2 115.0(4) . . ? C6 C5 C10 121.6(3) . . ? C6 C5 W1 69.1(2) . . ? C10 C5 W1 113.9(3) . . ? C7 C6 C5 111.9(4) . . ? C7 C6 C14 122.3(4) . . ? C5 C6 C14 125.6(4) . . ? C7 C6 W1 71.1(3) . . ? C5 C6 W1 74.5(3) . . ? C14 C6 W1 125.8(3) . . ? C6 C7 C8 117.2(4) . . ? C6 C7 W1 72.3(3) . . ? C8 C7 W1 76.7(3) . . ? C7 C8 C9 121.1(4) . . ? C7 C8 W1 67.4(2) . . ? C9 C8 W1 111.0(3) . . ? C15 C9 C8 121.3(4) . . ? C15 C9 C10 125.4(4) . . ? C8 C9 C10 113.2(3) . . ? C9 C10 C5 108.8(3) . . ? C9 C10 C11 116.0(3) . . ? C5 C10 C11 112.3(3) . . ? O4 C11 C12 110.1(3) . . ? O4 C11 C16 106.3(3) . . ? C12 C11 C16 113.8(4) . . ? O4 C11 C10 105.7(3) . . ? C12 C11 C10 111.4(3) . . ? C16 C11 C10 109.2(4) . . ? C11 C12 C13 116.8(4) . . ? O3 C13 C17 105.7(4) . . ? O3 C13 C18 107.6(4) . . ? C17 C13 C18 109.7(4) . . ? O3 C13 C12 108.7(4) . . ? C17 C13 C12 110.0(4) . . ? C18 C13 C12 114.7(4) . . ? C20 C19 B1 112.5(4) . . ? C22 C21 C25 107.5(4) . . ? C22 C21 C26 125.1(4) . . ? C25 C21 C26 126.6(4) . . ? C22 C21 W1 74.3(2) . . ? C25 C21 W1 72.7(2) . . ? C26 C21 W1 127.0(3) . . ? C23 C22 C21 108.0(4) . . ? C23 C22 C28 125.1(4) . . ? C21 C22 C28 126.4(4) . . ? C23 C22 W1 74.5(2) . . ? C21 C22 W1 70.0(2) . . ? C28 C22 W1 127.4(3) . . ? C22 C23 C24 108.4(4) . . ? C22 C23 C29 125.3(4) . . ? C24 C23 C29 125.3(4) . . ? C22 C23 W1 70.8(3) . . ? C24 C23 W1 71.0(2) . . ? C29 C23 W1 133.2(3) . . ? C25 C24 C23 107.5(4) . . ? C25 C24 C30 126.8(4) . . ? C23 C24 C30 125.0(4) . . ? C25 C24 W1 70.7(2) . . ? C23 C24 W1 74.2(3) . . ? C30 C24 W1 127.8(3) . . ? C24 C25 C21 108.5(4) . . ? C24 C25 C31 125.2(4) . . ? C21 C25 C31 125.4(4) . . ? C24 C25 W1 73.9(2) . . ? C21 C25 W1 71.2(2) . . ? C31 C25 W1 129.2(3) . . ? C21 C26 C27 111.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.056 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.114 #===END data_complex16a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H46 B2 N6 O2 W' _chemical_formula_weight 860.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y-1/2, -z' _cell_length_a 19.664(11) _cell_length_b 8.005(5) _cell_length_c 26.158(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.63(5) _cell_angle_gamma 90.00 _cell_volume 4098(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.3 _exptl_crystal_description plate _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.860 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3289 _exptl_absorpt_correction_T_max 0.8702 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 9 _diffrn_reflns_number 7228 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.1297 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7224 _reflns_number_gt 4645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (C.K.Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0565P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7224 _refine_ls_number_parameters 486 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1228 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.694873(18) 0.39743(5) 0.246065(16) 0.02699(13) Uani 1 d . . . O1 O 0.7944(3) 0.6828(10) 0.2874(3) 0.046(2) Uani 1 d . . . O2 O 0.8069(3) 0.2174(11) 0.1899(3) 0.046(2) Uani 1 d . . . N1 N 0.6189(4) 0.2146(11) 0.2128(3) 0.0290(19) Uani 1 d . . . N2 N 0.5559(4) 0.2672(12) 0.1880(3) 0.033(2) Uani 1 d . . . N3 N 0.6039(4) 0.5407(10) 0.2684(3) 0.032(2) Uani 1 d . . . N4 N 0.5451(4) 0.5389(11) 0.2340(3) 0.033(2) Uani 1 d . . . N5 N 0.6705(3) 0.5288(11) 0.1739(3) 0.0281(19) Uani 1 d . . . N6 N 0.6025(4) 0.5319(11) 0.1526(3) 0.033(2) Uani 1 d . . . B1 B 0.7715(6) 0.2938(17) 0.2952(5) 0.038(3) Uani 1 d . . . B2 B 0.5437(6) 0.4546(18) 0.1819(5) 0.040(3) Uani 1 d . . . C2 C 0.7084(6) 0.2264(14) 0.3269(5) 0.038(3) Uani 1 d . . . C3 C 0.7565(5) 0.5776(15) 0.2720(4) 0.035(3) Uani 1 d . . . C4 C 0.7662(5) 0.2824(15) 0.2124(4) 0.035(3) Uani 1 d . . . C5 C 0.8491(5) 0.2600(15) 0.3115(4) 0.037(3) Uani 1 d . . . C6 C 0.8680(6) 0.1300(18) 0.3455(5) 0.058(4) Uani 1 d . . . H6 H 0.8340 0.0668 0.3594 0.069(14) Uiso 1 calc R . . C7 C 0.9368(6) 0.093(2) 0.3593(5) 0.065(4) Uani 1 d . . . H7 H 0.9488 0.0076 0.3834 0.069(14) Uiso 1 calc R . . C8 C 0.9866(6) 0.179(2) 0.3379(5) 0.061(4) Uani 1 d . . . H8 H 1.0327 0.1495 0.3457 0.069(14) Uiso 1 calc R . . C9 C 0.9698(6) 0.3118(19) 0.3044(5) 0.056(4) Uani 1 d . . . H9 H 1.0040 0.3745 0.2906 0.069(14) Uiso 1 calc R . . C10 C 0.9014(5) 0.3487(15) 0.2921(4) 0.041(3) Uani 1 d . . . H10 H 0.8899 0.4380 0.2695 0.069(14) Uiso 1 calc R . . C11 C 0.7068(5) 0.2761(13) 0.3817(4) 0.033(2) Uani 1 d . . . C12 C 0.7553(5) 0.3793(17) 0.4087(4) 0.047(3) Uani 1 d . . . H12 H 0.7910 0.4243 0.3917 0.069(14) Uiso 1 calc R . . C13 C 0.7515(6) 0.416(2) 0.4595(5) 0.066(4) Uani 1 d . . . H13 H 0.7857 0.4829 0.4765 0.069(14) Uiso 1 calc R . . C14 C 0.6994(6) 0.3577(15) 0.4871(5) 0.048(3) Uani 1 d . . . C15 C 0.6499(6) 0.2571(18) 0.4600(4) 0.053(3) Uani 1 d . . . H15 H 0.6126 0.2176 0.4764 0.069(14) Uiso 1 calc R . . C16 C 0.6557(5) 0.2164(15) 0.4099(4) 0.042(3) Uani 1 d . . . H16 H 0.6230 0.1434 0.3935 0.069(14) Uiso 1 calc R . . C17 C 0.6952(8) 0.398(2) 0.5428(5) 0.087(5) Uani 1 d . . . H17A H 0.7267 0.3275 0.5639 0.16(5) Uiso 1 calc R . . H17B H 0.6490 0.3790 0.5514 0.16(5) Uiso 1 calc R . . H17C H 0.7073 0.5145 0.5489 0.16(5) Uiso 1 calc R . . C18 C 0.5185(5) 0.1362(15) 0.1692(4) 0.041(3) Uani 1 d . . . C19 C 0.5568(6) -0.0050(13) 0.1813(5) 0.043(3) Uani 1 d . . . H19 H 0.5442 -0.1154 0.1727 0.012(12) Uiso 1 calc R . . C20 C 0.6167(5) 0.0451(14) 0.2083(4) 0.037(3) Uani 1 d . . . C21 C 0.4493(5) 0.1502(18) 0.1402(5) 0.062(4) Uani 1 d . . . H21A H 0.4189 0.2092 0.1609 0.100(13) Uiso 1 calc R . . H21B H 0.4314 0.0393 0.1323 0.100(13) Uiso 1 calc R . . H21C H 0.4529 0.2110 0.1085 0.100(13) Uiso 1 calc R . . C22 C 0.6754(6) -0.0635(15) 0.2261(5) 0.056(4) Uani 1 d . . . H22A H 0.6915 -0.0353 0.2613 0.100(13) Uiso 1 calc R . . H22B H 0.7120 -0.0467 0.2043 0.100(13) Uiso 1 calc R . . H22C H 0.6611 -0.1795 0.2244 0.100(13) Uiso 1 calc R . . C23 C 0.4987(5) 0.6417(13) 0.2533(5) 0.042(3) Uani 1 d . . . C24 C 0.5263(6) 0.7122(14) 0.2990(5) 0.047(3) Uani 1 d . . . H24 H 0.5055 0.7881 0.3200 0.012(12) Uiso 1 calc R . . C25 C 0.5928(5) 0.6445(13) 0.3070(4) 0.038(3) Uani 1 d . . . C26 C 0.4261(5) 0.6665(17) 0.2256(5) 0.063(4) Uani 1 d . . . H26A H 0.4291 0.7301 0.1944 0.100(13) Uiso 1 calc R . . H26B H 0.3981 0.7265 0.2480 0.100(13) Uiso 1 calc R . . H26C H 0.4058 0.5584 0.2172 0.100(13) Uiso 1 calc R . . C27 C 0.6439(6) 0.6801(16) 0.3528(4) 0.047(3) Uani 1 d . . . H27A H 0.6369 0.6021 0.3802 0.100(13) Uiso 1 calc R . . H27B H 0.6375 0.7933 0.3647 0.100(13) Uiso 1 calc R . . H27C H 0.6899 0.6678 0.3429 0.100(13) Uiso 1 calc R . . C28 C 0.5983(5) 0.6117(15) 0.1069(4) 0.035(2) Uani 1 d . . . C29 C 0.6636(5) 0.6611(15) 0.0978(4) 0.041(3) Uani 1 d . . . H29 H 0.6762 0.7201 0.0692 0.012(12) Uiso 1 calc R . . C30 C 0.7061(5) 0.6062(16) 0.1394(4) 0.038(2) Uani 1 d . . . C31 C 0.5321(6) 0.6401(16) 0.0739(5) 0.057(4) Uani 1 d . . . H31A H 0.5143 0.5338 0.0607 0.100(13) Uiso 1 calc R . . H31B H 0.5401 0.7128 0.0454 0.100(13) Uiso 1 calc R . . H31C H 0.4992 0.6917 0.0943 0.100(13) Uiso 1 calc R . . C32 C 0.7828(5) 0.6332(14) 0.1492(5) 0.046(3) Uani 1 d . . . H32A H 0.7927 0.6984 0.1803 0.100(13) Uiso 1 calc R . . H32B H 0.7990 0.6924 0.1204 0.100(13) Uiso 1 calc R . . H32C H 0.8056 0.5259 0.1533 0.100(13) Uiso 1 calc R . . C33 C 0.2502(10) 0.466(2) 0.0398(7) 0.083(5) Uani 1 d . . . C34 C 0.2141(12) 0.383(2) 0.0768(5) 0.091(6) Uani 1 d . . . H34 H 0.2380 0.3449 0.1075 0.23(6) Uiso 1 calc R . . C35 C 0.1461(13) 0.356(3) 0.0684(13) 0.144(12) Uani 1 d . . . H35 H 0.1258 0.2947 0.0935 0.23(6) Uiso 1 calc R . . C36 C 0.1073(16) 0.406(5) 0.0307(14) 0.20(2) Uani 1 d . . . H36 H 0.0595 0.3964 0.0291 0.23(6) Uiso 1 calc R . . C37 C 0.141(2) 0.478(4) -0.0094(9) 0.156(15) Uani 1 d . . . H37 H 0.1149 0.5010 -0.0408 0.23(6) Uiso 1 calc R . . C38 C 0.2103(14) 0.516(3) -0.0041(8) 0.105(7) Uani 1 d . . . H38 H 0.2299 0.5742 -0.0301 0.23(6) Uiso 1 calc R . . C39 C 0.3216(13) 0.504(3) 0.0442(10) 0.167(12) Uani 1 d . . . H39A H 0.3285 0.6145 0.0307 0.31(11) Uiso 1 calc R . . H39B H 0.3451 0.4223 0.0248 0.31(11) Uiso 1 calc R . . H39C H 0.3396 0.4992 0.0800 0.31(11) Uiso 1 calc R . . H2B H 0.494(4) 0.493(12) 0.154(4) 0.030 Uiso 1 d . . . H2 H 0.715(5) 0.148(13) 0.320(4) 0.030 Uiso 1 d . . . C40 C 0.9607(15) 0.467(4) 0.4524(9) 0.065(8) Uiso 0.50 d PD . . C41 C 0.9942(16) 0.623(4) 0.4418(10) 0.092(10) Uiso 0.50 d PD . . C42 C 1.0393(16) 0.706(4) 0.4808(13) 0.099(11) Uiso 0.50 d PD . . C43 C 1.0470(17) 0.630(4) 0.5311(11) 0.105(12) Uiso 0.50 d PD . . C44 C 1.015(2) 0.474(4) 0.5419(10) 0.112(15) Uiso 0.50 d PD . . C45 C 0.9712(14) 0.391(3) 0.5024(10) 0.073(8) Uiso 0.50 d PD . . 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 W1 0.02678(19) 0.0272(2) 0.0270(2) 0.0001(3) 0.00272(13) -0.0008(2) O1 0.037(4) 0.042(5) 0.060(5) -0.003(4) 0.002(4) -0.010(4) O2 0.039(4) 0.062(6) 0.038(4) -0.010(4) 0.007(3) 0.018(4) N1 0.032(4) 0.026(5) 0.028(5) 0.000(4) 0.001(4) 0.000(4) N2 0.024(4) 0.038(6) 0.035(5) -0.002(5) 0.002(4) -0.002(4) N3 0.036(4) 0.024(4) 0.037(5) -0.008(4) 0.004(4) 0.001(4) N4 0.031(4) 0.031(5) 0.037(5) 0.001(4) 0.007(4) 0.003(4) N5 0.020(4) 0.029(5) 0.035(5) -0.008(4) 0.003(3) 0.002(3) N6 0.033(4) 0.030(5) 0.035(5) 0.002(4) 0.002(4) -0.001(4) B1 0.057(8) 0.033(8) 0.025(7) 0.001(6) 0.003(5) -0.004(6) B2 0.027(6) 0.052(9) 0.041(8) -0.017(6) 0.004(5) -0.009(6) C2 0.053(6) 0.024(6) 0.037(7) -0.007(5) 0.008(5) 0.003(5) C3 0.024(5) 0.042(8) 0.039(6) 0.004(6) -0.002(4) 0.003(5) C4 0.034(5) 0.037(7) 0.032(6) -0.004(5) -0.005(4) -0.005(5) C5 0.040(6) 0.035(7) 0.036(6) -0.018(6) 0.001(5) 0.006(5) C6 0.049(7) 0.072(11) 0.054(8) 0.002(8) 0.012(6) 0.025(7) C7 0.068(8) 0.082(11) 0.042(7) 0.013(9) -0.008(6) 0.035(9) C8 0.038(6) 0.074(10) 0.069(9) -0.017(8) 0.000(6) 0.023(7) C9 0.037(6) 0.072(10) 0.059(9) -0.024(8) 0.001(6) 0.003(7) C10 0.050(6) 0.053(8) 0.018(5) 0.004(5) -0.001(4) 0.002(5) C11 0.040(5) 0.029(6) 0.029(6) 0.003(5) 0.004(4) 0.006(5) C12 0.043(6) 0.064(9) 0.032(6) 0.001(7) 0.000(4) -0.006(6) C13 0.049(7) 0.092(12) 0.056(8) -0.014(9) -0.004(6) -0.013(8) C14 0.051(6) 0.044(8) 0.049(7) -0.019(6) 0.006(5) -0.002(6) C15 0.051(7) 0.075(10) 0.036(7) -0.002(7) 0.017(5) 0.000(7) C16 0.041(6) 0.042(7) 0.045(7) -0.003(6) 0.014(5) 0.000(5) C17 0.116(12) 0.097(13) 0.050(9) -0.011(11) 0.020(8) -0.021(12) C18 0.030(5) 0.049(9) 0.047(7) -0.009(6) 0.013(5) -0.015(5) C19 0.061(7) 0.012(6) 0.057(8) -0.013(5) 0.011(6) -0.013(5) C20 0.039(6) 0.037(7) 0.036(6) 0.007(5) 0.003(5) -0.004(5) C21 0.040(6) 0.069(11) 0.076(10) -0.012(8) -0.010(6) -0.005(6) C22 0.063(8) 0.036(8) 0.068(9) -0.015(6) 0.001(6) 0.005(6) C23 0.032(5) 0.034(7) 0.064(8) 0.005(6) 0.021(5) 0.018(5) C24 0.063(7) 0.021(6) 0.062(8) -0.009(6) 0.031(6) 0.013(6) C25 0.051(6) 0.028(7) 0.037(6) 0.006(5) 0.017(5) 0.009(5) C26 0.037(6) 0.059(9) 0.092(11) 0.011(8) 0.013(6) 0.029(6) C27 0.074(8) 0.044(7) 0.025(6) -0.016(6) 0.009(5) 0.004(6) C28 0.040(5) 0.029(6) 0.034(6) 0.005(6) -0.002(4) 0.004(5) C29 0.046(6) 0.046(7) 0.029(6) 0.014(5) 0.001(5) 0.002(5) C30 0.038(5) 0.046(6) 0.030(5) 0.009(6) 0.007(4) 0.003(6) C31 0.058(7) 0.056(10) 0.051(8) 0.021(7) -0.020(6) -0.003(6) C32 0.037(5) 0.041(8) 0.058(8) 0.023(6) 0.006(5) -0.001(5) C33 0.115(14) 0.070(11) 0.063(11) -0.020(9) -0.002(10) 0.032(10) C34 0.183(18) 0.058(11) 0.031(7) 0.012(8) 0.004(9) 0.045(13) C35 0.117(18) 0.088(19) 0.24(4) -0.08(2) 0.08(2) -0.013(15) C36 0.14(2) 0.24(4) 0.20(4) -0.14(4) -0.05(2) 0.07(3) C37 0.28(4) 0.12(2) 0.056(13) -0.036(15) -0.02(2) 0.08(3) C38 0.19(2) 0.069(13) 0.057(12) -0.005(10) 0.039(15) 0.018(15) C39 0.15(2) 0.12(2) 0.23(3) -0.11(2) 0.04(2) -0.035(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C4 1.958(11) . ? W1 C3 1.961(11) . ? W1 B1 2.058(13) . ? W1 N5 2.173(8) . ? W1 N1 2.209(8) . ? W1 N3 2.249(8) . ? W1 C2 2.510(13) . ? O1 C3 1.170(12) . ? O2 C4 1.161(12) . ? N1 C20 1.363(14) . ? N1 N2 1.405(11) . ? N2 C18 1.346(13) . ? N2 B2 1.525(18) . ? N3 C25 1.341(13) . ? N3 N4 1.394(11) . ? N4 C23 1.362(12) . ? N4 B2 1.520(15) . ? N5 C30 1.345(12) . ? N5 N6 1.398(10) . ? N6 C28 1.351(13) . ? N6 B2 1.574(14) . ? B1 C5 1.567(16) . ? B1 C2 1.648(17) . ? B2 H2B 1.19(9) . ? C2 C11 1.493(15) . ? C2 H2 0.67(10) . ? C5 C10 1.385(15) . ? C5 C6 1.397(17) . ? C6 C7 1.397(15) . ? C6 H6 0.9400 . ? C7 C8 1.366(19) . ? C7 H7 0.9400 . ? C8 C9 1.393(19) . ? C8 H8 0.9400 . ? C9 C10 1.384(14) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C16 1.389(13) . ? C11 C12 1.399(15) . ? C12 C13 1.370(16) . ? C12 H12 0.9400 . ? C13 C14 1.388(17) . ? C13 H13 0.9400 . ? C14 C15 1.401(16) . ? C14 C17 1.503(17) . ? C15 C16 1.365(15) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.378(15) . ? C18 C21 1.495(15) . ? C19 C20 1.372(15) . ? C19 H19 0.9400 . ? C20 C22 1.483(15) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.384(16) . ? C23 C26 1.547(15) . ? C24 C25 1.412(14) . ? C24 H24 0.9400 . ? C25 C27 1.513(15) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.385(14) . ? C28 C31 1.508(13) . ? C29 C30 1.377(14) . ? C29 H29 0.9400 . ? C30 C32 1.521(13) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C38 1.38(2) . ? C33 C34 1.42(2) . ? C33 C39 1.43(3) . ? C34 C35 1.35(3) . ? C34 H34 0.9400 . ? C35 C36 1.25(4) . ? C35 H35 0.9400 . ? C36 C37 1.41(5) . ? C36 H36 0.9400 . ? C37 C38 1.40(4) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 C44 0.68(4) 3_766 ? C40 C43 0.91(3) 3_766 ? C40 C45 1.440(17) . ? C40 C41 1.449(18) . ? C41 C44 0.91(3) 3_766 ? C41 C42 1.444(17) . ? C41 C45 1.55(4) 3_766 ? C42 C45 0.92(3) 3_766 ? C42 C43 1.443(18) . ? C42 C44 1.85(4) 3_766 ? C43 C40 0.91(3) 3_766 ? C43 C45 0.93(4) 3_766 ? C43 C44 1.442(17) . ? C44 C40 0.68(4) 3_766 ? C44 C41 0.91(3) 3_766 ? C44 C45 1.440(17) . ? C44 C45 1.63(4) 3_766 ? C44 C42 1.85(4) 3_766 ? C45 C42 0.92(3) 3_766 ? C45 C43 0.93(4) 3_766 ? C45 C41 1.55(4) 3_766 ? C45 C44 1.63(4) 3_766 ? 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 C4 W1 C3 93.2(4) . . ? C4 W1 B1 65.1(5) . . ? C3 W1 B1 72.0(5) . . ? C4 W1 N5 86.7(4) . . ? C3 W1 N5 91.2(4) . . ? B1 W1 N5 145.5(4) . . ? C4 W1 N1 89.9(4) . . ? C3 W1 N1 174.1(4) . . ? B1 W1 N1 113.9(5) . . ? N5 W1 N1 84.0(3) . . ? C4 W1 N3 168.3(4) . . ? C3 W1 N3 90.9(4) . . ? B1 W1 N3 126.5(4) . . ? N5 W1 N3 82.3(3) . . ? N1 W1 N3 85.2(3) . . ? C4 W1 C2 95.8(4) . . ? C3 W1 C2 95.7(4) . . ? B1 W1 C2 40.8(4) . . ? N5 W1 C2 172.5(3) . . ? N1 W1 C2 89.0(4) . . ? N3 W1 C2 94.6(3) . . ? C20 N1 N2 103.9(8) . . ? C20 N1 W1 135.1(7) . . ? N2 N1 W1 121.0(6) . . ? C18 N2 N1 111.1(9) . . ? C18 N2 B2 130.8(9) . . ? N1 N2 B2 117.8(8) . . ? C25 N3 N4 107.8(8) . . ? C25 N3 W1 134.7(7) . . ? N4 N3 W1 117.3(6) . . ? C23 N4 N3 107.4(9) . . ? C23 N4 B2 130.3(9) . . ? N3 N4 B2 121.6(8) . . ? C30 N5 N6 105.4(8) . . ? C30 N5 W1 136.1(6) . . ? N6 N5 W1 118.4(6) . . ? C28 N6 N5 109.4(7) . . ? C28 N6 B2 129.3(8) . . ? N5 N6 B2 121.3(8) . . ? C5 B1 C2 124.7(10) . . ? C5 B1 W1 150.8(9) . . ? C2 B1 W1 84.5(7) . . ? N4 B2 N2 110.6(11) . . ? N4 B2 N6 108.2(9) . . ? N2 B2 N6 108.8(9) . . ? N4 B2 H2B 112(5) . . ? N2 B2 H2B 115(5) . . ? N6 B2 H2B 102(4) . . ? C11 C2 B1 118.9(10) . . ? C11 C2 W1 130.8(8) . . ? B1 C2 W1 54.7(6) . . ? C11 C2 H2 123(10) . . ? B1 C2 H2 90(9) . . ? W1 C2 H2 106(10) . . ? O1 C3 W1 178.6(9) . . ? O2 C4 W1 176.4(9) . . ? C10 C5 C6 117.1(10) . . ? C10 C5 B1 123.4(11) . . ? C6 C5 B1 119.5(11) . . ? C5 C6 C7 121.0(13) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 119.9(13) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.6(11) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 118.4(12) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C9 C10 C5 122.9(12) . . ? C9 C10 H10 118.5 . . ? C5 C10 H10 118.5 . . ? C16 C11 C12 115.4(10) . . ? C16 C11 C2 120.3(10) . . ? C12 C11 C2 124.4(9) . . ? C13 C12 C11 121.0(11) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 123.1(12) . . ? C12 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 116.1(11) . . ? C13 C14 C17 123.0(11) . . ? C15 C14 C17 120.9(11) . . ? C16 C15 C14 120.2(11) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 124.1(11) . . ? C15 C16 H16 118.0 . . ? C11 C16 H16 118.0 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 106.7(9) . . ? N2 C18 C21 124.4(11) . . ? C19 C18 C21 128.9(11) . . ? C20 C19 C18 107.5(10) . . ? C20 C19 H19 126.2 . . ? C18 C19 H19 126.2 . . ? N1 C20 C19 110.7(10) . . ? N1 C20 C22 122.6(10) . . ? C19 C20 C22 126.4(11) . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 110.1(9) . . ? N4 C23 C26 121.7(11) . . ? C24 C23 C26 128.2(10) . . ? C23 C24 C25 104.6(9) . . ? C23 C24 H24 127.7 . . ? C25 C24 H24 127.7 . . ? N3 C25 C24 110.0(10) . . ? N3 C25 C27 124.7(9) . . ? C24 C25 C27 125.3(10) . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 C29 108.1(8) . . ? N6 C28 C31 123.5(9) . . ? C29 C28 C31 128.4(10) . . ? C30 C29 C28 105.9(9) . . ? C30 C29 H29 127.0 . . ? C28 C29 H29 127.0 . . ? N5 C30 C29 111.2(8) . . ? N5 C30 C32 121.6(9) . . ? C29 C30 C32 127.1(9) . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 114.7(18) . . ? C38 C33 C39 119(2) . . ? C34 C33 C39 127(2) . . ? C35 C34 C33 121.0(19) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 127(3) . . ? C36 C35 H35 116.7 . . ? C34 C35 H35 116.7 . . ? C35 C36 C37 115(3) . . ? C35 C36 H36 122.4 . . ? C37 C36 H36 122.4 . . ? C38 C37 C36 122(3) . . ? C38 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? C33 C38 C37 120(2) . . ? C33 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C44 C40 C43 130(5) 3_766 3_766 ? C44 C40 C45 93(3) 3_766 . ? C43 C40 C45 39(2) 3_766 . ? C44 C40 C41 28(3) 3_766 . ? C43 C40 C41 158(3) 3_766 . ? C45 C40 C41 120.7(12) . . ? C44 C41 C42 101(3) 3_766 . ? C44 C41 C40 21(3) 3_766 . ? C42 C41 C40 121.4(13) . . ? C44 C41 C45 66(2) 3_766 3_766 ? C42 C41 C45 35.6(14) . 3_766 ? C40 C41 C45 85.8(14) . 3_766 ? C45 C42 C43 39(2) 3_766 . ? C45 C42 C41 78(2) 3_766 . ? C43 C42 C41 116.9(13) . . ? C45 C42 C44 49.7(19) 3_766 3_766 ? C43 C42 C44 88.4(13) . 3_766 ? C41 C42 C44 28.8(13) . 3_766 ? C40 C43 C45 103(4) 3_766 3_766 ? C40 C43 C44 21(3) 3_766 . ? C45 C43 C44 84(2) 3_766 . ? C40 C43 C42 142(3) 3_766 . ? C45 C43 C42 39(2) 3_766 . ? C44 C43 C42 122.2(13) . . ? C40 C44 C41 131(6) 3_766 3_766 ? C40 C44 C45 147(4) 3_766 . ? C41 C44 C45 79(3) 3_766 . ? C40 C44 C43 29(3) 3_766 . ? C41 C44 C43 160(3) 3_766 . ? C45 C44 C43 120.2(13) . . ? C40 C44 C45 62(3) 3_766 3_766 ? C41 C44 C45 163(4) 3_766 3_766 ? C45 C44 C45 85.8(17) . 3_766 ? C43 C44 C45 34.6(14) . 3_766 ? C40 C44 C42 169(7) 3_766 3_766 ? C41 C44 C42 50(2) 3_766 3_766 ? C45 C44 C42 29.3(12) . 3_766 ? C43 C44 C42 149.4(15) . 3_766 ? C45 C44 C42 115(2) 3_766 3_766 ? C42 C45 C43 102(4) 3_766 3_766 ? C42 C45 C44 101(2) 3_766 . ? C43 C45 C44 155(3) 3_766 . ? C42 C45 C40 140(3) 3_766 . ? C43 C45 C40 38(2) 3_766 . ? C44 C45 C40 118.5(12) . . ? C42 C45 C41 66(2) 3_766 3_766 ? C43 C45 C41 165(4) 3_766 3_766 ? C44 C45 C41 35.1(14) . 3_766 ? C40 C45 C41 153.4(16) . 3_766 ? C42 C45 C44 163(4) 3_766 3_766 ? C43 C45 C44 61.7(19) 3_766 3_766 ? C44 C45 C44 94.2(17) . 3_766 ? C40 C45 C44 24.6(14) . 3_766 ? C41 C45 C44 129(2) 3_766 3_766 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.944 _refine_diff_density_min -1.120 _refine_diff_density_rms 0.170 #===END data_complex16b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H41 B2 N6 O2 W' _chemical_formula_weight 771.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.308(8) _cell_length_b 12.342(9) _cell_length_c 13.508(10) _cell_angle_alpha 84.29(6) _cell_angle_beta 81.00(6) _cell_angle_gamma 81.62(6) _cell_volume 1674(2) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 15.1 _cell_measurement_theta_max 16.0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 774 _exptl_absorpt_coefficient_mu 3.490 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9760 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9760 _reflns_number_gt 8813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (C.K.Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.4952P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9760 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.245362(11) 0.823903(9) 0.863371(8) 0.02617(4) Uani 1 d . . . O1 O 0.2226(3) 0.6354(2) 0.7333(2) 0.0519(7) Uani 1 d . . . O2 O 0.3754(3) 0.9525(2) 0.67133(19) 0.0504(7) Uani 1 d . . . N1 N 0.4332(3) 0.7268(2) 0.88972(19) 0.0304(5) Uani 1 d . . . N2 N 0.4527(2) 0.6960(2) 0.98862(19) 0.0290(5) Uani 1 d . . . N3 N 0.3026(3) 0.9249(2) 0.97597(18) 0.0287(5) Uani 1 d . . . N4 N 0.3406(3) 0.8714(2) 1.06423(18) 0.0293(5) Uani 1 d . . . N5 N 0.1579(3) 0.7232(2) 0.99952(19) 0.0306(5) Uani 1 d . . . N6 N 0.2204(3) 0.7068(2) 1.08491(19) 0.0299(5) Uani 1 d . . . B1 B 0.0982(4) 0.8622(3) 0.7727(3) 0.0328(7) Uani 1 d . . . B2 B 0.3564(4) 0.7448(3) 1.0792(3) 0.0308(7) Uani 1 d . . . C1 C 0.0279(3) 0.9392(3) 0.8615(2) 0.0333(6) Uani 1 d . . . C2 C -0.0053(4) 1.0583(3) 0.8174(3) 0.0423(8) Uani 1 d . . . C3 C 0.0364(3) 0.8605(3) 0.6749(2) 0.0348(6) Uani 1 d . . . C4 C 0.1162(4) 0.8512(3) 0.5812(3) 0.0430(8) Uani 1 d . . . C5 C 0.0614(5) 0.8542(4) 0.4934(3) 0.0512(10) Uani 1 d . . . C6 C -0.0744(5) 0.8665(4) 0.4968(3) 0.0529(10) Uani 1 d . . . C7 C -0.1563(5) 0.8756(4) 0.5877(3) 0.0512(10) Uani 1 d . . . C8 C -0.1011(4) 0.8736(3) 0.6761(3) 0.0424(8) Uani 1 d . . . C9 C 0.2281(3) 0.7086(3) 0.7804(3) 0.0352(6) Uani 1 d . . . C10 C 0.3270(4) 0.9063(3) 0.7450(2) 0.0361(7) Uani 1 d . . . C11 C 0.5691(3) 0.6288(3) 0.9896(2) 0.0321(6) Uani 1 d . . . C12 C 0.6273(3) 0.6173(3) 0.8910(3) 0.0359(7) Uani 1 d . . . C13 C 0.5400(3) 0.6787(3) 0.8311(2) 0.0329(6) Uani 1 d . . . C14 C 0.6194(4) 0.5769(3) 1.0835(3) 0.0400(7) Uani 1 d . . . C15 C 0.5562(4) 0.6914(4) 0.7188(3) 0.0472(9) Uani 1 d . . . C16 C 0.3639(3) 0.9462(3) 1.1240(2) 0.0334(6) Uani 1 d . . . C17 C 0.3441(3) 1.0481(3) 1.0734(3) 0.0358(7) Uani 1 d . . . C18 C 0.3062(3) 1.0325(3) 0.9818(2) 0.0308(6) Uani 1 d . . . C19 C 0.3968(4) 0.9156(4) 1.2277(3) 0.0443(8) Uani 1 d . . . C20 C 0.2742(4) 1.1185(3) 0.9000(3) 0.0406(7) Uani 1 d . . . C21 C 0.1467(4) 0.6517(3) 1.1592(3) 0.0366(7) Uani 1 d . . . C22 C 0.0366(4) 0.6296(3) 1.1221(3) 0.0400(7) Uani 1 d . . . C23 C 0.0470(3) 0.6742(3) 1.0218(3) 0.0351(6) Uani 1 d . . . C24 C 0.1848(5) 0.6260(4) 1.2625(3) 0.0506(9) Uani 1 d . . . C25 C -0.0441(4) 0.6675(4) 0.9480(3) 0.0433(8) Uani 1 d . . . C26 C -0.1154(5) 0.5728(4) 0.5112(3) 0.0556(10) Uani 1 d . . . C27 C -0.0119(5) 0.5840(4) 0.5618(3) 0.0548(11) Uani 1 d . . . C28 C 0.1027(5) 0.5122(4) 0.5508(3) 0.0544(10) Uani 1 d . . . C29 C 0.6059(7) 0.7848(5) 0.4036(5) 0.0738(16) Uani 1 d . . . C30 C 0.6600(7) 0.6949(9) 0.3435(5) 0.098(3) Uani 1 d . . . C31 C 0.5908(9) 0.6062(6) 0.3488(4) 0.086(2) Uani 1 d . . . C32 C 0.4735(7) 0.6051(5) 0.4087(5) 0.0805(17) Uani 1 d . . . H32 H 0.4271 0.5444 0.4116 0.097 Uiso 1 calc R . . C33 C 0.4224(7) 0.6890(5) 0.4641(5) 0.0781(16) Uani 1 d . . . C34 C 0.4859(6) 0.7778(5) 0.4631(4) 0.0659(13) Uani 1 d . . . H2 H 0.392(4) 0.715(4) 1.157(3) 0.051(12) Uiso 1 d . . . H1A H -0.052(4) 0.901(3) 0.889(3) 0.032(9) Uiso 1 d . . . H1B H 0.074(4) 0.942(3) 0.921(3) 0.043(11) Uiso 1 d . . . H2A H -0.029(5) 1.105(4) 0.869(4) 0.056(13) Uiso 1 d . . . H2B H -0.073(6) 1.065(5) 0.788(4) 0.066(16) Uiso 1 d . . . H2C H 0.078(5) 1.089(4) 0.775(3) 0.057(13) Uiso 1 d . . . H4 H 0.208(4) 0.842(3) 0.576(3) 0.029(9) Uiso 1 d . . . H5 H 0.117(5) 0.853(4) 0.429(4) 0.060(14) Uiso 1 d . . . H6 H -0.113(4) 0.872(4) 0.435(3) 0.051(12) Uiso 1 d . . . H7 H -0.245(6) 0.885(5) 0.589(4) 0.071(16) Uiso 1 d . . . H8 H -0.155(4) 0.879(4) 0.737(3) 0.043(11) Uiso 1 d . . . H12 H 0.716(4) 0.578(4) 0.866(3) 0.043(11) Uiso 1 d . . . H14A H 0.556(5) 0.540(4) 1.123(3) 0.052(13) Uiso 1 d . . . H14B H 0.652(5) 0.621(4) 1.121(4) 0.064(15) Uiso 1 d . . . H14C H 0.695(5) 0.530(5) 1.070(4) 0.066(15) Uiso 1 d . . . H15A H 0.643(5) 0.664(4) 0.697(3) 0.051(12) Uiso 1 d . . . H15B H 0.481(7) 0.662(6) 0.694(5) 0.10(2) Uiso 1 d . . . H15C H 0.535(7) 0.750(6) 0.694(5) 0.10(3) Uiso 1 d . . . H17 H 0.354(4) 1.109(3) 1.092(3) 0.032(9) Uiso 1 d . . . H19A H 0.429(6) 0.978(5) 1.254(4) 0.075(17) Uiso 1 d . . . H19B H 0.457(6) 0.851(5) 1.236(4) 0.078(17) Uiso 1 d . . . H19C H 0.321(7) 0.912(6) 1.282(5) 0.11(2) Uiso 1 d . . . H20A H 0.323(5) 1.179(4) 0.899(3) 0.055(13) Uiso 1 d . . . H20B H 0.295(4) 1.083(4) 0.827(3) 0.050(12) Uiso 1 d . . . H20C H 0.183(5) 1.142(4) 0.904(3) 0.050(12) Uiso 1 d . . . H22 H -0.036(5) 0.597(4) 1.154(4) 0.071(16) Uiso 1 d . . . H24A H 0.274(7) 0.580(6) 1.262(5) 0.11(2) Uiso 1 d . . . H24B H 0.206(5) 0.681(4) 1.289(4) 0.057(14) Uiso 1 d . . . H24C H 0.120(6) 0.581(5) 1.301(4) 0.074(16) Uiso 1 d . . . H25A H -0.009(6) 0.660(5) 0.878(5) 0.091(19) Uiso 1 d . . . H25B H -0.114(9) 0.730(8) 0.945(6) 0.15(3) Uiso 1 d . . . H25C H -0.093(7) 0.616(6) 0.971(5) 0.10(2) Uiso 1 d . . . H26 H -0.197(5) 0.620(4) 0.519(4) 0.062(14) Uiso 1 d . . . H27 H -0.025(5) 0.644(5) 0.609(4) 0.067(15) Uiso 1 d . . . H28 H 0.186(4) 0.526(3) 0.581(3) 0.042(11) Uiso 1 d . . . H29 H 0.648(6) 0.833(5) 0.398(4) 0.064(17) Uiso 1 d . . . H30 H 0.722(5) 0.710(4) 0.322(3) 0.041(13) Uiso 1 d . . . H31 H 0.642(7) 0.543(6) 0.312(5) 0.10(2) Uiso 1 d . . . H33 H 0.337(8) 0.673(7) 0.509(6) 0.13(3) Uiso 1 d . . . H34 H 0.440(6) 0.833(5) 0.497(4) 0.089(19) Uiso 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 W1 0.02781(6) 0.02394(6) 0.02718(6) -0.00597(4) -0.00504(4) -0.00100(4) O1 0.0605(17) 0.0395(15) 0.0614(17) -0.0241(13) -0.0223(14) 0.0029(13) O2 0.0671(18) 0.0475(16) 0.0372(13) -0.0004(11) 0.0007(12) -0.0201(14) N1 0.0297(12) 0.0315(13) 0.0297(12) -0.0043(10) -0.0048(9) -0.0010(10) N2 0.0275(12) 0.0273(12) 0.0322(12) -0.0040(10) -0.0069(9) 0.0000(9) N3 0.0313(12) 0.0251(12) 0.0303(12) -0.0049(9) -0.0048(9) -0.0030(10) N4 0.0305(12) 0.0309(13) 0.0279(11) -0.0067(10) -0.0063(9) -0.0035(10) N5 0.0309(12) 0.0288(13) 0.0327(12) -0.0042(10) -0.0059(10) -0.0034(10) N6 0.0326(13) 0.0247(12) 0.0318(12) -0.0016(9) -0.0032(10) -0.0038(10) B1 0.0350(17) 0.0295(17) 0.0343(16) -0.0073(13) -0.0051(13) -0.0022(13) B2 0.0326(16) 0.0306(17) 0.0300(15) -0.0038(12) -0.0065(12) -0.0041(13) C1 0.0295(15) 0.0346(16) 0.0348(15) -0.0092(12) -0.0053(12) 0.0043(12) C2 0.047(2) 0.0330(18) 0.0469(19) -0.0088(15) -0.0147(16) 0.0069(15) C3 0.0402(17) 0.0327(16) 0.0323(14) -0.0066(12) -0.0094(12) -0.0007(13) C4 0.050(2) 0.042(2) 0.0379(17) -0.0108(14) -0.0076(15) -0.0034(16) C5 0.072(3) 0.051(2) 0.0330(17) -0.0075(16) -0.0085(17) -0.013(2) C6 0.074(3) 0.049(2) 0.043(2) -0.0010(17) -0.0291(19) -0.012(2) C7 0.055(2) 0.050(2) 0.054(2) -0.0031(18) -0.0272(19) -0.0049(19) C8 0.0430(19) 0.046(2) 0.0412(18) -0.0060(15) -0.0160(15) -0.0019(15) C9 0.0363(16) 0.0314(16) 0.0383(16) -0.0070(12) -0.0094(12) 0.0013(13) C10 0.0421(17) 0.0336(16) 0.0341(15) -0.0099(12) -0.0071(13) -0.0037(13) C11 0.0298(14) 0.0259(14) 0.0426(16) -0.0052(12) -0.0101(12) -0.0028(11) C12 0.0282(15) 0.0361(17) 0.0427(17) -0.0109(13) -0.0032(12) 0.0010(12) C13 0.0289(14) 0.0326(16) 0.0376(15) -0.0099(12) -0.0016(11) -0.0035(12) C14 0.0369(18) 0.0357(18) 0.0487(19) 0.0009(15) -0.0147(15) -0.0022(15) C15 0.041(2) 0.059(3) 0.0381(18) -0.0130(18) 0.0010(15) 0.0044(18) C16 0.0282(14) 0.0394(17) 0.0350(15) -0.0142(13) -0.0048(11) -0.0050(12) C17 0.0334(16) 0.0355(17) 0.0418(17) -0.0161(14) -0.0035(12) -0.0078(13) C18 0.0286(14) 0.0294(15) 0.0351(14) -0.0086(11) -0.0010(11) -0.0054(11) C19 0.0427(19) 0.056(2) 0.0373(17) -0.0172(16) -0.0126(15) -0.0008(17) C20 0.050(2) 0.0272(16) 0.0448(18) -0.0061(13) -0.0043(15) -0.0053(15) C21 0.0404(17) 0.0290(15) 0.0371(16) -0.0011(12) 0.0025(13) -0.0034(13) C22 0.0407(18) 0.0319(17) 0.0465(18) -0.0011(14) 0.0004(14) -0.0105(14) C23 0.0323(15) 0.0284(15) 0.0457(17) -0.0078(13) -0.0039(13) -0.0060(12) C24 0.060(3) 0.054(3) 0.0370(18) 0.0051(17) -0.0064(17) -0.012(2) C25 0.0363(18) 0.045(2) 0.053(2) -0.0069(17) -0.0086(15) -0.0146(16) C26 0.058(3) 0.051(2) 0.056(2) -0.0003(19) -0.0115(19) 0.002(2) C27 0.081(3) 0.037(2) 0.051(2) -0.0043(17) -0.018(2) -0.011(2) C28 0.062(3) 0.048(2) 0.058(2) 0.0018(19) -0.019(2) -0.014(2) C29 0.085(4) 0.062(3) 0.079(4) 0.019(3) -0.040(3) -0.009(3) C30 0.066(4) 0.139(8) 0.061(3) 0.034(4) 0.001(3) 0.038(4) C31 0.132(6) 0.064(4) 0.054(3) -0.019(3) -0.034(3) 0.041(4) C32 0.111(5) 0.059(3) 0.075(4) -0.004(3) -0.039(4) 0.001(3) C33 0.097(5) 0.062(3) 0.071(3) -0.003(3) -0.007(3) -0.004(3) C34 0.088(4) 0.058(3) 0.048(2) -0.013(2) -0.014(2) 0.011(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 W1 C9 1.941(4) . ? W1 C10 1.951(4) . ? W1 B1 2.069(4) . ? W1 N1 2.183(3) . ? W1 N3 2.255(3) . ? W1 N5 2.257(3) . ? W1 C1 2.476(4) . ? O1 C9 1.168(4) . ? O2 C10 1.174(4) . ? N1 C13 1.350(4) . ? N1 N2 1.390(4) . ? N2 C11 1.356(4) . ? N2 B2 1.562(4) . ? N3 C18 1.344(4) . ? N3 N4 1.388(4) . ? N4 C16 1.355(4) . ? N4 B2 1.543(5) . ? N5 C23 1.349(4) . ? N5 N6 1.391(4) . ? N6 C21 1.350(4) . ? N6 B2 1.530(4) . ? B1 C3 1.557(5) . ? B1 C1 1.619(5) . ? B2 H2 1.18(4) . ? C1 C2 1.541(5) . ? C1 H1A 1.01(4) . ? C1 H1B 1.00(4) . ? C2 H2A 0.93(5) . ? C2 H2B 0.85(6) . ? C2 H2C 1.05(5) . ? C3 C4 1.402(5) . ? C3 C8 1.401(5) . ? C4 C5 1.386(5) . ? C4 H4 0.92(4) . ? C5 C6 1.380(7) . ? C5 H5 0.97(5) . ? C6 C7 1.382(7) . ? C6 H6 0.97(4) . ? C7 C8 1.397(5) . ? C7 H7 0.90(5) . ? C8 H8 0.92(4) . ? C11 C12 1.385(5) . ? C11 C14 1.494(5) . ? C12 C13 1.396(5) . ? C12 H12 1.00(4) . ? C13 C15 1.495(5) . ? C14 H14A 0.92(5) . ? C14 H14B 0.91(5) . ? C14 H14C 0.90(6) . ? C15 H15A 0.93(5) . ? C15 H15B 1.01(7) . ? C15 H15C 0.79(8) . ? C16 C17 1.375(5) . ? C16 C19 1.492(5) . ? C17 C18 1.393(4) . ? C17 H17 0.84(4) . ? C18 C20 1.495(5) . ? C19 H19A 1.00(6) . ? C19 H19B 0.94(6) . ? C19 H19C 0.98(7) . ? C20 H20A 0.96(5) . ? C20 H20B 1.10(4) . ? C20 H20C 0.94(5) . ? C21 C22 1.381(5) . ? C21 C24 1.500(5) . ? C22 C23 1.404(5) . ? C22 H22 0.93(5) . ? C23 C25 1.488(5) . ? C24 H24A 1.01(7) . ? C24 H24B 0.86(5) . ? C24 H24C 0.98(6) . ? C25 H25A 0.96(6) . ? C25 H25B 0.98(10) . ? C25 H25C 0.87(8) . ? C26 C27 1.384(7) . ? C26 C28 1.385(7) 2_566 ? C26 H26 0.95(5) . ? C27 C28 1.367(7) . ? C27 H27 1.01(5) . ? C28 C26 1.385(7) 2_566 ? C28 H28 1.05(4) . ? C29 C34 1.375(9) . ? C29 C30 1.435(11) . ? C29 H29 0.77(5) . ? C30 C31 1.381(12) . ? C30 H30 0.70(4) . ? C31 C32 1.347(10) . ? C31 H31 1.00(7) . ? C32 C33 1.336(8) . ? C32 H32 0.9400 . ? C33 C34 1.354(9) . ? C33 H33 1.02(8) . ? C34 H34 0.89(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 W1 C10 89.96(15) . . ? C9 W1 B1 65.05(15) . . ? C10 W1 B1 75.42(16) . . ? C9 W1 N1 85.62(13) . . ? C10 W1 N1 93.09(14) . . ? B1 W1 N1 148.07(12) . . ? C9 W1 N3 165.52(12) . . ? C10 W1 N3 95.48(13) . . ? B1 W1 N3 129.33(13) . . ? N1 W1 N3 80.70(11) . . ? C9 W1 N5 89.03(14) . . ? C10 W1 N5 177.71(12) . . ? B1 W1 N5 105.98(14) . . ? N1 W1 N5 84.78(12) . . ? N3 W1 N5 85.03(11) . . ? C9 W1 C1 101.15(14) . . ? C10 W1 C1 92.70(15) . . ? B1 W1 C1 40.50(13) . . ? N1 W1 C1 171.10(10) . . ? N3 W1 C1 92.02(12) . . ? N5 W1 C1 89.52(12) . . ? C13 N1 N2 106.5(3) . . ? C13 N1 W1 135.3(2) . . ? N2 N1 W1 117.95(19) . . ? C11 N2 N1 109.4(3) . . ? C11 N2 B2 128.6(3) . . ? N1 N2 B2 121.8(2) . . ? C18 N3 N4 106.5(2) . . ? C18 N3 W1 135.1(2) . . ? N4 N3 W1 118.37(19) . . ? C16 N4 N3 109.5(3) . . ? C16 N4 B2 130.3(3) . . ? N3 N4 B2 120.2(2) . . ? C23 N5 N6 106.8(3) . . ? C23 N5 W1 133.7(2) . . ? N6 N5 W1 119.48(19) . . ? C21 N6 N5 109.6(3) . . ? C21 N6 B2 131.6(3) . . ? N5 N6 B2 118.7(2) . . ? C3 B1 C1 121.7(3) . . ? C3 B1 W1 154.7(3) . . ? C1 B1 W1 83.4(2) . . ? N6 B2 N4 108.9(3) . . ? N6 B2 N2 110.0(3) . . ? N4 B2 N2 109.2(3) . . ? N6 B2 H2 106(2) . . ? N4 B2 H2 110(2) . . ? N2 B2 H2 113(2) . . ? C2 C1 B1 109.9(3) . . ? C2 C1 W1 129.8(3) . . ? B1 C1 W1 56.12(17) . . ? C2 C1 H1A 114(2) . . ? B1 C1 H1A 101(2) . . ? W1 C1 H1A 116(2) . . ? C2 C1 H1B 107(2) . . ? B1 C1 H1B 119(2) . . ? W1 C1 H1B 63(2) . . ? H1A C1 H1B 105(3) . . ? C1 C2 H2A 110(3) . . ? C1 C2 H2B 111(4) . . ? H2A C2 H2B 104(5) . . ? C1 C2 H2C 112(3) . . ? H2A C2 H2C 103(4) . . ? H2B C2 H2C 115(4) . . ? C4 C3 C8 117.3(3) . . ? C4 C3 B1 121.2(3) . . ? C8 C3 B1 121.4(3) . . ? C5 C4 C3 121.4(4) . . ? C5 C4 H4 118(2) . . ? C3 C4 H4 121(2) . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 119(3) . . ? C4 C5 H5 120(3) . . ? C5 C6 C7 120.2(4) . . ? C5 C6 H6 120(3) . . ? C7 C6 H6 119(3) . . ? C6 C7 C8 119.7(4) . . ? C6 C7 H7 119(3) . . ? C8 C7 H7 121(3) . . ? C7 C8 C3 121.3(4) . . ? C7 C8 H8 121(3) . . ? C3 C8 H8 118(3) . . ? O1 C9 W1 176.3(3) . . ? O2 C10 W1 177.2(3) . . ? N2 C11 C12 108.1(3) . . ? N2 C11 C14 123.9(3) . . ? C12 C11 C14 128.0(3) . . ? C11 C12 C13 106.2(3) . . ? C11 C12 H12 128(2) . . ? C13 C12 H12 126(2) . . ? N1 C13 C12 109.9(3) . . ? N1 C13 C15 123.0(3) . . ? C12 C13 C15 127.1(3) . . ? C11 C14 H14A 110(3) . . ? C11 C14 H14B 117(3) . . ? H14A C14 H14B 110(4) . . ? C11 C14 H14C 112(3) . . ? H14A C14 H14C 110(4) . . ? H14B C14 H14C 97(4) . . ? C13 C15 H15A 106(3) . . ? C13 C15 H15B 110(4) . . ? H15A C15 H15B 120(5) . . ? C13 C15 H15C 117(5) . . ? H15A C15 H15C 113(6) . . ? H15B C15 H15C 91(6) . . ? N4 C16 C17 107.6(3) . . ? N4 C16 C19 122.6(3) . . ? C17 C16 C19 129.7(3) . . ? C16 C17 C18 106.9(3) . . ? C16 C17 H17 128(3) . . ? C18 C17 H17 125(3) . . ? N3 C18 C17 109.4(3) . . ? N3 C18 C20 123.3(3) . . ? C17 C18 C20 127.3(3) . . ? C16 C19 H19A 110(3) . . ? C16 C19 H19B 116(3) . . ? H19A C19 H19B 110(5) . . ? C16 C19 H19C 116(4) . . ? H19A C19 H19C 94(5) . . ? H19B C19 H19C 107(5) . . ? C18 C20 H20A 111(3) . . ? C18 C20 H20B 110(2) . . ? H20A C20 H20B 110(4) . . ? C18 C20 H20C 112(3) . . ? H20A C20 H20C 111(4) . . ? H20B C20 H20C 101(3) . . ? N6 C21 C22 108.0(3) . . ? N6 C21 C24 122.3(3) . . ? C22 C21 C24 129.7(3) . . ? C21 C22 C23 106.6(3) . . ? C21 C22 H22 131(3) . . ? C23 C22 H22 123(3) . . ? N5 C23 C22 109.0(3) . . ? N5 C23 C25 123.6(3) . . ? C22 C23 C25 127.3(3) . . ? C21 C24 H24A 112(4) . . ? C21 C24 H24B 115(3) . . ? H24A C24 H24B 95(5) . . ? C21 C24 H24C 107(3) . . ? H24A C24 H24C 106(5) . . ? H24B C24 H24C 120(4) . . ? C23 C25 H25A 120(4) . . ? C23 C25 H25B 114(5) . . ? H25A C25 H25B 103(6) . . ? C23 C25 H25C 108(5) . . ? H25A C25 H25C 110(6) . . ? H25B C25 H25C 99(6) . . ? C27 C26 C28 119.6(4) . 2_566 ? C27 C26 H26 123(3) . . ? C28 C26 H26 118(3) 2_566 . ? C28 C27 C26 120.5(4) . . ? C28 C27 H27 121(3) . . ? C26 C27 H27 118(3) . . ? C27 C28 C26 119.8(4) . 2_566 ? C27 C28 H28 121(2) . . ? C26 C28 H28 119(2) 2_566 . ? C34 C29 C30 117.4(7) . . ? C34 C29 H29 127(4) . . ? C30 C29 H29 116(4) . . ? C31 C30 C29 119.1(6) . . ? C31 C30 H30 139(4) . . ? C29 C30 H30 102(5) . . ? C32 C31 C30 120.3(6) . . ? C32 C31 H31 126(4) . . ? C30 C31 H31 113(4) . . ? C33 C32 C31 120.8(7) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 121.8(7) . . ? C32 C33 H33 111(5) . . ? C34 C33 H33 127(5) . . ? C33 C34 C29 120.6(6) . . ? C33 C34 H34 116(4) . . ? C29 C34 H34 123(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.660 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.108