Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Adams, Christopher J.' 'Connelly, N.' 'Harding, David J.' 'Hayward, Owen D.' 'Orpen, A.' 'Patron, Elena' 'Rieger, Philip' _publ_contact_author_name 'Prof N Connelly' _publ_contact_author_address ; Prof N Connelly School of Chemistry University of Bristol Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email 'NEIL.CONNELLY@BRISTOL.AC.UK' _publ_section_title ; The d2/d3 alkyne redox pair [WF2(PhC=CPh)Tp']z (z = +1 or 0): missing links in a 'redox family tree' ; #--------------------------------------------------------- data_1 _database_code_CSD 172824 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 B F2 N6 W' _chemical_formula_weight 697.27 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' 'F' 'F' 0.0171 0.0103 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6427(17) _cell_length_b 32.628(7) _cell_length_c 9.8228(17) _cell_angle_alpha 90.00 _cell_angle_beta 113.989(11) _cell_angle_gamma 90.00 _cell_volume 2823.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 123 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Magenta _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 4.134 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 29564 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6494 _reflns_number_gt 4725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6494 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.002 _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 W1 W -0.405028(19) 0.124971(6) -0.380787(19) 0.01907(6) Uani 1 1 d . . . F1 F -0.2191(3) 0.09313(8) -0.3082(3) 0.0265(6) Uani 1 1 d . . . F2 F -0.3252(3) 0.15846(8) -0.1967(3) 0.0267(6) Uani 1 1 d . . . N1 N -0.5127(4) 0.07342(11) -0.5255(4) 0.0204(8) Uani 1 1 d . . . N2 N -0.6544(4) 0.05977(11) -0.5408(4) 0.0222(8) Uani 1 1 d . . . C1 C -0.4728(5) 0.05091(14) -0.6185(5) 0.0241(10) Uani 1 1 d . . . C2 C -0.3253(5) 0.05793(16) -0.6316(5) 0.0303(11) Uani 1 1 d . . . H2A H -0.2677 0.0793 -0.5611 0.045 Uiso 1 1 calc R . . H2B H -0.3451 0.0667 -0.7333 0.045 Uiso 1 1 calc R . . H2C H -0.2664 0.0324 -0.6089 0.045 Uiso 1 1 calc R . . C3 C -0.5872(5) 0.02272(14) -0.6931(5) 0.0258(10) Uani 1 1 d . . . H3A H -0.5875 0.0030 -0.7642 0.031 Uiso 1 1 calc R . . C4 C -0.6997(5) 0.02918(14) -0.6432(5) 0.0249(10) Uani 1 1 d . . . C5 C -0.8500(5) 0.00853(16) -0.6909(6) 0.0340(12) Uani 1 1 d . . . H5A H -0.9047 0.0196 -0.6341 0.051 Uiso 1 1 calc R . . H5B H -0.8349 -0.0210 -0.6726 0.051 Uiso 1 1 calc R . . H5C H -0.9093 0.0134 -0.7974 0.051 Uiso 1 1 calc R . . N3 N -0.4677(4) 0.08488(12) -0.2277(4) 0.0209(8) Uani 1 1 d . . . N4 N -0.6129(4) 0.07038(11) -0.2737(4) 0.0219(8) Uani 1 1 d . . . C6 C -0.3949(5) 0.07478(14) -0.0823(5) 0.0252(10) Uani 1 1 d . . . C7 C -0.2322(5) 0.08557(17) 0.0080(5) 0.0355(13) Uani 1 1 d . . . H7A H -0.1917 0.1003 -0.0547 0.053 Uiso 1 1 calc R . . H7B H -0.1734 0.0604 0.0458 0.053 Uiso 1 1 calc R . . H7C H -0.2250 0.1030 0.0919 0.053 Uiso 1 1 calc R . . C8 C -0.4946(6) 0.05441(14) -0.0362(5) 0.0288(11) Uani 1 1 d . . . H8A H -0.4727 0.0438 0.0605 0.035 Uiso 1 1 calc R . . C9 C -0.6317(5) 0.05253(14) -0.1583(5) 0.0254(10) Uani 1 1 d . . . C10 C -0.7815(6) 0.03599(16) -0.1688(6) 0.0354(12) Uani 1 1 d . . . H10A H -0.8573 0.0385 -0.2716 0.053 Uiso 1 1 calc R . . H10B H -0.8148 0.0516 -0.1023 0.053 Uiso 1 1 calc R . . H10C H -0.7698 0.0071 -0.1392 0.053 Uiso 1 1 calc R . . N5 N -0.6255(4) 0.14923(11) -0.4187(4) 0.0205(8) Uani 1 1 d . . . N6 N -0.7484(4) 0.12360(12) -0.4606(4) 0.0223(8) Uani 1 1 d . . . C11 C -0.6782(5) 0.18801(15) -0.4274(5) 0.0253(10) Uani 1 1 d . . . C12 C -0.5772(6) 0.22452(16) -0.3948(6) 0.0387(13) Uani 1 1 d . . . H12A H -0.4714 0.2155 -0.3603 0.058 Uiso 1 1 calc R . . H12B H -0.5894 0.2411 -0.3171 0.058 Uiso 1 1 calc R . . H12C H -0.6043 0.2410 -0.4854 0.058 Uiso 1 1 calc R . . C13 C -0.8347(5) 0.18687(15) -0.4764(5) 0.0284(11) Uani 1 1 d . . . H13A H -0.9007 0.2097 -0.4940 0.034 Uiso 1 1 calc R . . C14 C -0.8758(5) 0.14624(15) -0.4946(5) 0.0246(10) Uani 1 1 d . . . C15 C -1.0303(5) 0.12756(17) -0.5445(6) 0.0352(12) Uani 1 1 d . . . H15A H -1.0228 0.0978 -0.5536 0.053 Uiso 1 1 calc R . . H15B H -1.0968 0.1390 -0.6413 0.053 Uiso 1 1 calc R . . H15C H -1.0725 0.1336 -0.4712 0.053 Uiso 1 1 calc R . . B1 B -0.7252(6) 0.07703(17) -0.4379(6) 0.0256(12) Uani 1 1 d . . . H1 H -0.8240 0.0632 -0.4579 0.031 Uiso 1 1 calc R . . C16 C -0.4308(5) 0.15219(14) -0.5775(5) 0.0219(10) Uani 1 1 d . . . C17 C -0.3216(5) 0.17061(14) -0.4655(5) 0.0224(10) Uani 1 1 d . . . C18 C -0.2127(5) 0.20459(14) -0.4201(5) 0.0236(10) Uani 1 1 d . . . C19 C -0.0830(5) 0.20214(15) -0.2875(5) 0.0257(10) Uani 1 1 d . . . H19A H -0.0654 0.1783 -0.2271 0.031 Uiso 1 1 calc R . . C20 C 0.0199(5) 0.23388(16) -0.2431(5) 0.0287(12) Uani 1 1 d . . . H20A H 0.1093 0.2315 -0.1540 0.034 Uiso 1 1 calc R . . C21 C -0.0060(6) 0.26917(15) -0.3273(5) 0.0311(12) Uani 1 1 d . . . H21A H 0.0654 0.2910 -0.2960 0.037 Uiso 1 1 calc R . . C22 C -0.1366(6) 0.27283(16) -0.4581(6) 0.0340(12) Uani 1 1 d . . . H22A H -0.1567 0.2975 -0.5144 0.041 Uiso 1 1 calc R . . C23 C -0.2373(5) 0.24014(15) -0.5057(5) 0.0275(11) Uani 1 1 d . . . H23A H -0.3238 0.2420 -0.5976 0.033 Uiso 1 1 calc R . . C24 C -0.5158(5) 0.15332(15) -0.7392(5) 0.0236(10) Uani 1 1 d . . . C25 C -0.4496(6) 0.16724(15) -0.8331(5) 0.0287(11) Uani 1 1 d . . . H25A H -0.3482 0.1772 -0.7914 0.034 Uiso 1 1 calc R . . C26 C -0.5298(6) 0.16677(16) -0.9869(6) 0.0354(13) Uani 1 1 d . . . H26A H -0.4825 0.1754 -1.0500 0.043 Uiso 1 1 calc R . . C27 C -0.6773(6) 0.15378(18) -1.0467(5) 0.0402(14) Uani 1 1 d . . . H27A H -0.7330 0.1539 -1.1517 0.048 Uiso 1 1 calc R . . C28 C -0.7465(6) 0.14039(17) -0.9555(6) 0.0372(13) Uani 1 1 d . . . H28A H -0.8498 0.1320 -0.9981 0.045 Uiso 1 1 calc R . . C29 C -0.6658(5) 0.13925(15) -0.8038(5) 0.0301(11) Uani 1 1 d . . . H29A H -0.7122 0.1288 -0.7421 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01929(9) 0.02087(9) 0.01677(9) -0.00102(9) 0.00703(7) -0.00303(9) F1 0.0233(13) 0.0292(16) 0.0254(15) 0.0027(12) 0.0085(12) 0.0012(11) F2 0.0318(15) 0.0273(15) 0.0206(14) -0.0051(12) 0.0104(12) -0.0082(12) N1 0.0185(18) 0.020(2) 0.022(2) -0.0057(16) 0.0072(16) -0.0041(15) N2 0.0199(19) 0.022(2) 0.024(2) -0.0010(16) 0.0074(17) -0.0017(16) C1 0.027(2) 0.025(3) 0.016(2) 0.0040(19) 0.005(2) 0.006(2) C2 0.030(3) 0.037(3) 0.027(3) -0.006(2) 0.014(2) 0.001(2) C3 0.032(3) 0.024(3) 0.018(2) -0.002(2) 0.007(2) 0.001(2) C4 0.027(2) 0.020(2) 0.022(2) -0.003(2) 0.003(2) -0.004(2) C5 0.031(3) 0.029(3) 0.036(3) -0.008(2) 0.008(2) -0.012(2) N3 0.0217(18) 0.022(2) 0.0176(19) -0.0004(16) 0.0066(16) -0.0044(17) N4 0.025(2) 0.020(2) 0.023(2) -0.0006(16) 0.0115(17) -0.0023(16) C6 0.029(3) 0.022(3) 0.022(2) 0.000(2) 0.008(2) 0.000(2) C7 0.032(3) 0.043(3) 0.024(3) 0.005(2) 0.003(2) -0.006(2) C8 0.042(3) 0.023(3) 0.022(3) 0.007(2) 0.014(2) -0.001(2) C9 0.033(3) 0.024(3) 0.024(3) -0.0006(19) 0.016(2) -0.004(2) C10 0.039(3) 0.034(3) 0.042(3) 0.003(2) 0.026(3) -0.006(2) N5 0.0174(18) 0.021(2) 0.021(2) 0.0006(16) 0.0058(16) -0.0008(15) N6 0.0216(18) 0.025(2) 0.0215(19) 0.0009(18) 0.0100(15) 0.0004(18) C11 0.028(3) 0.024(3) 0.028(3) 0.004(2) 0.015(2) 0.004(2) C12 0.040(3) 0.025(3) 0.056(4) -0.002(3) 0.025(3) 0.000(2) C13 0.029(3) 0.031(3) 0.026(3) 0.005(2) 0.012(2) 0.009(2) C14 0.019(2) 0.031(3) 0.023(2) 0.005(2) 0.009(2) 0.004(2) C15 0.023(2) 0.039(3) 0.042(3) -0.001(3) 0.012(2) 0.002(2) B1 0.023(3) 0.024(3) 0.034(3) -0.005(2) 0.016(2) -0.003(2) C16 0.021(2) 0.023(2) 0.027(3) 0.000(2) 0.014(2) 0.0006(19) C17 0.018(2) 0.028(3) 0.022(2) 0.002(2) 0.0085(19) 0.0023(19) C18 0.023(2) 0.024(3) 0.024(2) 0.000(2) 0.010(2) -0.0028(19) C19 0.025(2) 0.028(3) 0.023(2) 0.002(2) 0.009(2) 0.000(2) C20 0.023(2) 0.033(3) 0.025(3) -0.009(2) 0.004(2) -0.008(2) C21 0.036(3) 0.025(3) 0.034(3) -0.008(2) 0.016(2) -0.011(2) C22 0.043(3) 0.026(3) 0.035(3) 0.010(2) 0.018(3) -0.004(2) C23 0.028(3) 0.030(3) 0.023(3) 0.006(2) 0.009(2) 0.000(2) C24 0.027(2) 0.023(3) 0.019(2) 0.0006(19) 0.007(2) 0.0031(19) C25 0.035(3) 0.027(3) 0.027(3) 0.004(2) 0.016(2) 0.004(2) C26 0.049(3) 0.036(3) 0.027(3) 0.004(2) 0.021(3) 0.007(3) C27 0.051(3) 0.045(4) 0.012(2) 0.004(2) 0.001(2) 0.012(3) C28 0.031(3) 0.040(3) 0.028(3) 0.000(2) -0.001(2) -0.004(2) C29 0.031(3) 0.029(3) 0.029(3) 0.003(2) 0.011(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 F1 1.940(2) . ? W1 F2 1.981(2) . ? W1 C17 2.025(4) . ? W1 C16 2.048(4) . ? W1 N5 2.155(3) . ? W1 N1 2.174(4) . ? W1 N3 2.253(3) . ? N1 C1 1.345(5) . ? N1 N2 1.386(5) . ? N2 C4 1.357(6) . ? N2 B1 1.538(6) . ? C1 C3 1.394(6) . ? C1 C2 1.497(6) . ? C3 C4 1.375(6) . ? C4 C5 1.491(6) . ? N3 C6 1.352(6) . ? N3 N4 1.369(5) . ? N4 C9 1.351(5) . ? N4 B1 1.550(7) . ? C6 C8 1.387(6) . ? C6 C7 1.497(6) . ? C8 C9 1.379(7) . ? C9 C10 1.506(6) . ? N5 C11 1.353(6) . ? N5 N6 1.369(5) . ? N6 C14 1.354(5) . ? N6 B1 1.539(7) . ? C11 C13 1.385(6) . ? C11 C12 1.489(7) . ? C13 C14 1.374(7) . ? C14 C15 1.496(6) . ? C16 C17 1.318(6) . ? C16 C24 1.462(6) . ? C17 C18 1.466(6) . ? C18 C19 1.394(6) . ? C18 C23 1.396(6) . ? C19 C20 1.377(6) . ? C20 C21 1.380(7) . ? C21 C22 1.391(7) . ? C22 C23 1.389(7) . ? C24 C25 1.394(6) . ? C24 C29 1.400(6) . ? C25 C26 1.389(7) . ? C26 C27 1.366(7) . ? C27 C28 1.387(7) . ? C28 C29 1.373(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 F1 W1 F2 90.10(11) . . ? F1 W1 C17 94.76(14) . . ? F2 W1 C17 84.12(15) . . ? F1 W1 C16 108.58(14) . . ? F2 W1 C16 118.37(15) . . ? C17 W1 C16 37.76(17) . . ? F1 W1 N5 163.72(12) . . ? F2 W1 N5 86.85(12) . . ? C17 W1 N5 100.82(16) . . ? C16 W1 N5 86.86(15) . . ? F1 W1 N1 87.15(12) . . ? F2 W1 N1 158.21(12) . . ? C17 W1 N1 117.65(16) . . ? C16 W1 N1 82.88(16) . . ? N5 W1 N1 89.76(13) . . ? F1 W1 N3 84.38(12) . . ? F2 W1 N3 79.70(12) . . ? C17 W1 N3 163.79(16) . . ? C16 W1 N3 156.78(16) . . ? N5 W1 N3 79.33(13) . . ? N1 W1 N3 78.51(13) . . ? C1 N1 N2 107.0(3) . . ? C1 N1 W1 132.4(3) . . ? N2 N1 W1 120.5(3) . . ? C4 N2 N1 108.8(3) . . ? C4 N2 B1 131.4(4) . . ? N1 N2 B1 119.5(4) . . ? N1 C1 C3 109.5(4) . . ? N1 C1 C2 121.3(4) . . ? C3 C1 C2 129.3(4) . . ? C4 C3 C1 106.4(4) . . ? N2 C4 C3 108.3(4) . . ? N2 C4 C5 122.9(4) . . ? C3 C4 C5 128.7(4) . . ? C6 N3 N4 106.6(3) . . ? C6 N3 W1 133.0(3) . . ? N4 N3 W1 119.8(3) . . ? C9 N4 N3 109.9(4) . . ? C9 N4 B1 131.2(4) . . ? N3 N4 B1 118.9(3) . . ? N3 C6 C8 109.3(4) . . ? N3 C6 C7 122.5(4) . . ? C8 C6 C7 128.2(4) . . ? C9 C8 C6 106.5(4) . . ? N4 C9 C8 107.6(4) . . ? N4 C9 C10 123.4(4) . . ? C8 C9 C10 129.0(4) . . ? C11 N5 N6 107.2(4) . . ? C11 N5 W1 132.3(3) . . ? N6 N5 W1 120.0(3) . . ? C14 N6 N5 109.2(4) . . ? C14 N6 B1 129.7(4) . . ? N5 N6 B1 120.2(4) . . ? N5 C11 C13 108.9(4) . . ? N5 C11 C12 122.6(4) . . ? C13 C11 C12 128.4(4) . . ? C14 C13 C11 106.7(4) . . ? N6 C14 C13 108.0(4) . . ? N6 C14 C15 122.8(4) . . ? C13 C14 C15 129.2(4) . . ? N2 B1 N6 110.1(4) . . ? N2 B1 N4 108.9(4) . . ? N6 B1 N4 106.7(4) . . ? C17 C16 C24 143.1(4) . . ? C17 C16 W1 70.2(3) . . ? C24 C16 W1 146.6(3) . . ? C16 C17 C18 146.0(4) . . ? C16 C17 W1 72.1(3) . . ? C18 C17 W1 141.8(3) . . ? C19 C18 C23 118.6(4) . . ? C19 C18 C17 120.0(4) . . ? C23 C18 C17 121.3(4) . . ? C20 C19 C18 120.7(4) . . ? C19 C20 C21 120.4(4) . . ? C20 C21 C22 120.0(4) . . ? C23 C22 C21 119.4(5) . . ? C22 C23 C18 120.7(4) . . ? C25 C24 C29 118.3(4) . . ? C25 C24 C16 121.4(4) . . ? C29 C24 C16 120.3(4) . . ? C26 C25 C24 120.9(5) . . ? C27 C26 C25 119.5(5) . . ? C26 C27 C28 120.7(5) . . ? C29 C28 C27 120.0(5) . . ? C28 C29 C24 120.5(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.673 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.122 data_1+[BF4]- _database_code_CSD 172825 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H31 B2 F6 N6 W' _chemical_formula_weight 783.07 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' 'F' 'F' 0.0171 0.0103 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2631(16) _cell_length_b 12.5168(17) _cell_length_c 20.124(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.574(2) _cell_angle_gamma 90.00 _cell_volume 3045.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 205 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 3.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.362619 _exptl_absorpt_correction_T_max 0.491509 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15983 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5366 _reflns_number_gt 4171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5366 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.008 _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 W1 W 0.763439(14) 0.959127(14) 0.111053(9) 0.01925(6) Uani 1 1 d . . . F1 F 0.6658(2) 1.06493(19) 0.06944(13) 0.0263(6) Uani 1 1 d . . . F2 F 0.89126(19) 1.0409(2) 0.14333(12) 0.0263(6) Uani 1 1 d . . . N1 N 0.6514(3) 0.8497(3) 0.05547(18) 0.0223(9) Uani 1 1 d . . . N2 N 0.6882(3) 0.7691(3) 0.01702(18) 0.0222(9) Uani 1 1 d . . . C1 C 0.5399(4) 0.8382(4) 0.0499(2) 0.0248(11) Uani 1 1 d . . . C2 C 0.4707(4) 0.9130(4) 0.0823(3) 0.0316(12) Uani 1 1 d . . . H2A H 0.4865 0.9866 0.0703 0.047 Uiso 1 1 calc R . . H2B H 0.4875 0.9046 0.1313 0.047 Uiso 1 1 calc R . . H2C H 0.3923 0.8973 0.0666 0.047 Uiso 1 1 calc R . . C3 C 0.5068(4) 0.7517(4) 0.0094(2) 0.0291(11) Uani 1 1 d . . . H3A H 0.4333 0.7258 -0.0027 0.035 Uiso 1 1 calc R . . C4 C 0.6007(4) 0.7095(4) -0.0102(2) 0.0256(11) Uani 1 1 d . . . C5 C 0.6111(4) 0.6134(4) -0.0529(2) 0.0316(12) Uani 1 1 d . . . H5A H 0.6574 0.6308 -0.0867 0.047 Uiso 1 1 calc R . . H5B H 0.5376 0.5914 -0.0756 0.047 Uiso 1 1 calc R . . H5C H 0.6452 0.5549 -0.0243 0.047 Uiso 1 1 calc R . . N3 N 0.8273(3) 0.9680(3) 0.01551(18) 0.0216(8) Uani 1 1 d . . . N4 N 0.8363(3) 0.8770(3) -0.02176(19) 0.0242(9) Uani 1 1 d . . . C6 C 0.8553(3) 1.0509(4) -0.0205(2) 0.0230(10) Uani 1 1 d . . . C7 C 0.8543(4) 1.1634(3) 0.0039(3) 0.0293(12) Uani 1 1 d . . . H7A H 0.8896 1.1666 0.0513 0.044 Uiso 1 1 calc R . . H7B H 0.7777 1.1884 -0.0003 0.044 Uiso 1 1 calc R . . H7C H 0.8950 1.2089 -0.0231 0.044 Uiso 1 1 calc R . . C8 C 0.8823(4) 1.0132(4) -0.0799(2) 0.0287(12) Uani 1 1 d . . . H8A H 0.9057 1.0548 -0.1144 0.034 Uiso 1 1 calc R . . C9 C 0.8691(4) 0.9037(4) -0.0799(2) 0.0241(11) Uani 1 1 d . . . C10 C 0.8848(4) 0.8231(4) -0.1322(2) 0.0342(13) Uani 1 1 d . . . H10A H 0.9332 0.7657 -0.1114 0.051 Uiso 1 1 calc R . . H10B H 0.9187 0.8575 -0.1675 0.051 Uiso 1 1 calc R . . H10C H 0.8129 0.7931 -0.1521 0.051 Uiso 1 1 calc R . . N5 N 0.8727(3) 0.8272(3) 0.12775(19) 0.0216(9) Uani 1 1 d . . . N6 N 0.8835(3) 0.7550(3) 0.07719(19) 0.0223(9) Uani 1 1 d . . . C11 C 0.9446(4) 0.7967(4) 0.1834(2) 0.0247(11) Uani 1 1 d . . . C12 C 0.9611(4) 0.8592(4) 0.2479(2) 0.0330(12) Uani 1 1 d . . . H12A H 0.8930 0.8573 0.2674 0.050 Uiso 1 1 calc R . . H12B H 0.9792 0.9334 0.2387 0.050 Uiso 1 1 calc R . . H12C H 1.0218 0.8277 0.2797 0.050 Uiso 1 1 calc R . . C13 C 0.9990(4) 0.7071(4) 0.1680(3) 0.0309(12) Uani 1 1 d . . . H13A H 1.0538 0.6690 0.1977 0.037 Uiso 1 1 calc R . . C14 C 0.9595(4) 0.6819(4) 0.1013(3) 0.0282(12) Uani 1 1 d . . . C15 C 0.9923(4) 0.5926(4) 0.0598(3) 0.0372(13) Uani 1 1 d . . . H15A H 0.9265 0.5641 0.0309 0.056 Uiso 1 1 calc R . . H15B H 1.0273 0.5358 0.0895 0.056 Uiso 1 1 calc R . . H15C H 1.0447 0.6190 0.0318 0.056 Uiso 1 1 calc R . . B1 B 0.8097(4) 0.7655(4) 0.0070(3) 0.0246(13) Uani 1 1 d . . . C16 C 0.6983(3) 0.8967(4) 0.1908(2) 0.0199(11) Uani 1 1 d . . . C17 C 0.7155(4) 1.0018(4) 0.1995(2) 0.0231(11) Uani 1 1 d . . . C18 C 0.7159(3) 1.0961(4) 0.2419(2) 0.0225(11) Uani 1 1 d . . . C19 C 0.7302(4) 1.1964(4) 0.2156(3) 0.0291(12) Uani 1 1 d . . . H19A H 0.7405 1.2037 0.1700 0.035 Uiso 1 1 calc R . . C20 C 0.7293(4) 1.2864(4) 0.2558(3) 0.0356(13) Uani 1 1 d . . . H20A H 0.7368 1.3556 0.2377 0.043 Uiso 1 1 calc R . . C21 C 0.7177(4) 1.2746(4) 0.3222(3) 0.0406(14) Uani 1 1 d . . . H21A H 0.7186 1.3361 0.3499 0.049 Uiso 1 1 calc R . . C22 C 0.7046(4) 1.1750(4) 0.3491(3) 0.0408(14) Uani 1 1 d . . . H22A H 0.6962 1.1681 0.3950 0.049 Uiso 1 1 calc R . . C23 C 0.7037(4) 1.0858(4) 0.3092(2) 0.0315(12) Uani 1 1 d . . . H23A H 0.6948 1.0171 0.3276 0.038 Uiso 1 1 calc R . . C24 C 0.6598(4) 0.8025(4) 0.2165(2) 0.0265(11) Uani 1 1 d . . . C25 C 0.5989(4) 0.8065(4) 0.2701(2) 0.0285(12) Uani 1 1 d . . . H25A H 0.5837 0.8738 0.2883 0.034 Uiso 1 1 calc R . . C26 C 0.5609(4) 0.7148(4) 0.2966(3) 0.0389(13) Uani 1 1 d . . . H26A H 0.5207 0.7192 0.3330 0.047 Uiso 1 1 calc R . . C27 C 0.5815(4) 0.6164(5) 0.2700(3) 0.0412(14) Uani 1 1 d . . . H27A H 0.5569 0.5530 0.2889 0.049 Uiso 1 1 calc R . . C28 C 0.6385(4) 0.6101(4) 0.2155(3) 0.0381(13) Uani 1 1 d . . . H28A H 0.6510 0.5427 0.1963 0.046 Uiso 1 1 calc R . . C29 C 0.6761(4) 0.7016(4) 0.1901(2) 0.0278(11) Uani 1 1 d . . . H29A H 0.7148 0.6965 0.1531 0.033 Uiso 1 1 calc R . . B2 B 0.7607(6) 0.4165(5) 0.0825(3) 0.0406(16) Uani 1 1 d . . . F3 F 0.7524(3) 0.4002(3) 0.01411(16) 0.0638(10) Uani 1 1 d . . . F4 F 0.8545(3) 0.3670(3) 0.11553(18) 0.0646(10) Uani 1 1 d . . . F5 F 0.6680(3) 0.3749(3) 0.10483(18) 0.0641(10) Uani 1 1 d . . . F6 F 0.7642(3) 0.5254(2) 0.09504(18) 0.0613(10) 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 W1 0.02253(10) 0.01993(10) 0.01596(10) -0.00087(9) 0.00513(7) -0.00028(9) F1 0.0314(14) 0.0275(16) 0.0208(14) 0.0026(11) 0.0068(12) 0.0051(11) F2 0.0274(13) 0.0278(14) 0.0248(14) -0.0027(13) 0.0080(11) -0.0020(13) N1 0.025(2) 0.022(2) 0.020(2) -0.0001(17) 0.0062(17) 0.0015(17) N2 0.031(2) 0.019(2) 0.018(2) -0.0034(16) 0.0068(18) 0.0003(17) C1 0.023(2) 0.034(3) 0.018(3) 0.004(2) 0.005(2) 0.001(2) C2 0.026(3) 0.037(3) 0.033(3) -0.002(2) 0.007(2) 0.003(2) C3 0.026(3) 0.034(3) 0.028(3) 0.001(2) 0.003(2) -0.005(2) C4 0.032(3) 0.028(3) 0.015(2) -0.001(2) -0.003(2) -0.004(2) C5 0.037(3) 0.024(3) 0.031(3) -0.006(2) -0.001(2) 0.002(2) N3 0.0239(19) 0.023(2) 0.018(2) -0.0014(18) 0.0058(16) -0.0008(18) N4 0.027(2) 0.025(2) 0.022(2) -0.0008(19) 0.0058(18) 0.0033(18) C6 0.020(2) 0.027(3) 0.023(3) 0.004(2) 0.003(2) 0.000(2) C7 0.031(3) 0.025(3) 0.033(3) 0.006(2) 0.008(2) -0.003(2) C8 0.033(3) 0.029(3) 0.027(3) 0.006(2) 0.012(2) 0.002(2) C9 0.020(2) 0.038(3) 0.014(2) -0.002(2) 0.003(2) 0.002(2) C10 0.037(3) 0.043(3) 0.025(3) -0.006(2) 0.012(2) -0.003(2) N5 0.023(2) 0.023(2) 0.019(2) -0.0013(17) 0.0054(18) -0.0017(16) N6 0.021(2) 0.021(2) 0.025(2) -0.0041(17) 0.0074(18) -0.0007(17) C11 0.022(2) 0.025(3) 0.028(3) 0.006(2) 0.007(2) -0.003(2) C12 0.037(3) 0.043(3) 0.018(3) 0.003(2) 0.000(2) 0.001(2) C13 0.034(3) 0.026(3) 0.031(3) 0.007(2) 0.000(2) 0.005(2) C14 0.024(3) 0.023(3) 0.039(3) 0.003(2) 0.008(2) 0.003(2) C15 0.039(3) 0.023(3) 0.050(4) -0.003(3) 0.009(3) 0.013(2) B1 0.024(3) 0.029(3) 0.021(3) -0.002(2) 0.004(2) -0.001(2) C16 0.009(2) 0.041(3) 0.009(2) -0.003(2) 0.0005(18) 0.005(2) C17 0.016(2) 0.030(3) 0.024(3) 0.007(2) 0.004(2) 0.0008(19) C18 0.019(2) 0.031(3) 0.018(3) -0.009(2) 0.005(2) -0.001(2) C19 0.034(3) 0.028(3) 0.025(3) -0.004(2) 0.005(2) 0.003(2) C20 0.036(3) 0.027(3) 0.043(4) -0.003(3) 0.003(3) 0.003(2) C21 0.036(3) 0.044(4) 0.043(4) -0.026(3) 0.008(3) -0.001(3) C22 0.046(3) 0.050(4) 0.030(3) -0.019(3) 0.016(3) -0.013(3) C23 0.034(3) 0.036(3) 0.027(3) -0.004(2) 0.013(2) -0.009(2) C24 0.024(3) 0.029(3) 0.023(3) -0.004(2) -0.006(2) 0.004(2) C25 0.029(3) 0.032(3) 0.024(3) -0.002(2) 0.005(2) -0.008(2) C26 0.034(3) 0.052(4) 0.032(3) 0.005(3) 0.011(3) -0.012(3) C27 0.045(3) 0.038(3) 0.040(3) 0.012(3) 0.005(3) -0.015(3) C28 0.049(3) 0.024(3) 0.042(3) 0.004(3) 0.009(3) -0.001(3) C29 0.029(3) 0.032(3) 0.023(3) 0.001(2) 0.004(2) -0.003(2) B2 0.052(4) 0.033(4) 0.033(4) 0.002(3) -0.003(3) -0.007(3) F3 0.101(3) 0.053(2) 0.033(2) -0.0045(17) 0.001(2) 0.034(2) F4 0.057(2) 0.073(2) 0.054(2) 0.007(2) -0.0172(18) 0.005(2) F5 0.056(2) 0.060(2) 0.072(3) 0.017(2) -0.0037(19) -0.0240(19) F6 0.078(2) 0.036(2) 0.074(3) -0.0217(18) 0.027(2) -0.0152(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 F1 1.886(2) . ? W1 F2 1.894(2) . ? W1 C17 2.037(5) . ? W1 C16 2.062(4) . ? W1 N5 2.118(4) . ? W1 N1 2.122(4) . ? W1 N3 2.196(4) . ? N1 C1 1.362(5) . ? N1 N2 1.391(5) . ? N2 C4 1.347(5) . ? N2 B1 1.536(6) . ? C1 C3 1.374(6) . ? C1 C2 1.486(6) . ? C3 C4 1.383(6) . ? C4 C5 1.497(6) . ? N3 C6 1.343(6) . ? N3 N4 1.378(5) . ? N4 C9 1.341(6) . ? N4 B1 1.567(7) . ? C6 C8 1.375(6) . ? C6 C7 1.492(6) . ? C8 C9 1.380(6) . ? C9 C10 1.494(6) . ? N5 C11 1.360(6) . ? N5 N6 1.384(5) . ? N6 C14 1.338(6) . ? N6 B1 1.551(7) . ? C11 C13 1.366(6) . ? C11 C12 1.500(6) . ? C13 C14 1.386(7) . ? C14 C15 1.490(6) . ? C16 C17 1.340(6) . ? C16 C24 1.401(6) . ? C17 C18 1.456(6) . ? C18 C19 1.385(7) . ? C18 C23 1.394(6) . ? C19 C20 1.389(7) . ? C20 C21 1.373(7) . ? C21 C22 1.380(7) . ? C22 C23 1.373(7) . ? C24 C29 1.397(6) . ? C24 C25 1.411(6) . ? C25 C26 1.379(7) . ? C26 C27 1.383(7) . ? C27 C28 1.398(7) . ? C28 C29 1.366(6) . ? B2 F4 1.376(7) . ? B2 F3 1.378(7) . ? B2 F6 1.386(7) . ? B2 F5 1.391(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 F1 W1 F2 101.60(11) . . ? F1 W1 C17 87.11(15) . . ? F2 W1 C17 84.34(15) . . ? F1 W1 C16 108.19(14) . . ? F2 W1 C16 110.11(14) . . ? C17 W1 C16 38.16(18) . . ? F1 W1 N5 163.01(12) . . ? F2 W1 N5 84.34(13) . . ? C17 W1 N5 109.44(16) . . ? C16 W1 N5 84.12(15) . . ? F1 W1 N1 84.93(12) . . ? F2 W1 N1 162.89(12) . . ? C17 W1 N1 111.98(16) . . ? C16 W1 N1 82.23(16) . . ? N5 W1 N1 85.24(14) . . ? F1 W1 N3 82.44(12) . . ? F2 W1 N3 82.98(12) . . ? C17 W1 N3 161.59(17) . . ? C16 W1 N3 160.25(17) . . ? N5 W1 N3 82.53(14) . . ? N1 W1 N3 82.23(13) . . ? C1 N1 N2 107.0(4) . . ? C1 N1 W1 131.7(3) . . ? N2 N1 W1 121.3(3) . . ? C4 N2 N1 108.5(4) . . ? C4 N2 B1 130.9(4) . . ? N1 N2 B1 120.4(4) . . ? N1 C1 C3 109.0(4) . . ? N1 C1 C2 122.4(4) . . ? C3 C1 C2 128.5(4) . . ? C1 C3 C4 107.0(4) . . ? N2 C4 C3 108.5(4) . . ? N2 C4 C5 122.7(4) . . ? C3 C4 C5 128.7(4) . . ? C6 N3 N4 107.1(4) . . ? C6 N3 W1 132.2(3) . . ? N4 N3 W1 120.5(3) . . ? C9 N4 N3 109.4(4) . . ? C9 N4 B1 131.0(4) . . ? N3 N4 B1 119.6(4) . . ? N3 C6 C8 108.9(4) . . ? N3 C6 C7 122.3(4) . . ? C8 C6 C7 128.8(4) . . ? C6 C8 C9 107.2(4) . . ? N4 C9 C8 107.4(4) . . ? N4 C9 C10 122.6(4) . . ? C8 C9 C10 129.9(4) . . ? C11 N5 N6 107.1(4) . . ? C11 N5 W1 131.0(3) . . ? N6 N5 W1 121.9(3) . . ? C14 N6 N5 109.1(4) . . ? C14 N6 B1 130.8(4) . . ? N5 N6 B1 120.1(4) . . ? N5 C11 C13 108.6(4) . . ? N5 C11 C12 122.8(4) . . ? C13 C11 C12 128.5(5) . . ? C11 C13 C14 107.5(4) . . ? N6 C14 C13 107.8(4) . . ? N6 C14 C15 123.1(5) . . ? C13 C14 C15 129.1(4) . . ? N2 B1 N6 108.4(4) . . ? N2 B1 N4 106.7(4) . . ? N6 B1 N4 106.6(4) . . ? C17 C16 C24 146.4(4) . . ? C17 C16 W1 69.9(3) . . ? C24 C16 W1 143.6(3) . . ? C16 C17 C18 149.2(5) . . ? C16 C17 W1 71.9(3) . . ? C18 C17 W1 138.7(3) . . ? C19 C18 C23 119.8(4) . . ? C19 C18 C17 120.0(4) . . ? C23 C18 C17 120.3(4) . . ? C18 C19 C20 119.9(5) . . ? C21 C20 C19 119.5(5) . . ? C20 C21 C22 121.1(5) . . ? C23 C22 C21 119.7(5) . . ? C22 C23 C18 120.1(5) . . ? C29 C24 C16 122.8(4) . . ? C29 C24 C25 116.8(5) . . ? C16 C24 C25 120.4(4) . . ? C26 C25 C24 121.5(5) . . ? C25 C26 C27 119.7(5) . . ? C26 C27 C28 120.1(5) . . ? C29 C28 C27 119.3(5) . . ? C28 C29 C24 122.5(5) . . ? F4 B2 F3 109.5(5) . . ? F4 B2 F6 110.9(5) . . ? F3 B2 F6 108.8(5) . . ? F4 B2 F5 109.7(5) . . ? F3 B2 F5 109.8(5) . . ? F6 B2 F5 108.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.836 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.106