# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1438 data_Complex_2-Me _audit_creation_method SHELXL #======================================================================= _publ_contact_author_name 'Peter Burger' _publ_contact_author_address ; 'Anorg.-Chem Inst., University of Zuerich, Winterthurerstr. 190, 8057 Zuerich' ; _publ_contact_author_email 'chburger@aci.unizh.ch' _publ_contact_author_fax '+41 1 635 6802' _publ_contact_author_phone '+41 1 635 4692' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' loop_ _publ_author_name 'Christian Cremer' 'Peter Burger' _chemical_name_systematic ; ? ; _chemical_formula_structural '(EtMe4C5)*W(Me2-bipy)Cl3 * 2 CH2Cl2' _chemical_formula_sum 'C25 H33 Cl7 N2 W' _chemical_formula_weight 793.53 _chemical_melting_point n/a _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3240(10) _cell_length_b 17.879(3) _cell_length_c 20.464(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.92 _cell_angle_gamma 90.00 _cell_volume 2990.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 10 _cell_measurement_theta_max 18 _exptl_crystal_description 'rectangular parallelepiped' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.763 _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 4.507 _exptl_absorpt_correction_type 'empirical, PSI-scans' _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.99 _exptl_special_details ; n/a ; _diffrn_ambient_temperature 183(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 'Nicolet-Siemens P4' _diffrn_measurement_method 'omega-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 147 _diffrn_standards_decay_% none _diffrn_reflns_number 5749 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5339 _reflns_number_observed 5076 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens-P3' _computing_cell_refinement 'Siemens-P3' _computing_data_reduction 'Siemens-XDISK' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XPMA, Platon (Spek, 1997)' _computing_publication_material 'SHELXL-93, Platon' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0162P)^2^+33.5611P] 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 'riding model with fixed isotropic U' _refine_ls_extinction_method n/a _refine_ls_extinction_coef n/a _refine_ls_number_reflns 5334 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all 0.1463 _refine_ls_wR_factor_obs 0.1069 _refine_ls_goodness_of_fit_all 1.321 _refine_ls_goodness_of_fit_obs 1.336 _refine_ls_restrained_S_all 1.782 _refine_ls_restrained_S_obs 1.336 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.77503(4) 0.85876(2) 0.186448(15) 0.01281(10) Uani 1 d . . Cl1 Cl 1.0630(2) 0.90345(11) 0.20428(10) 0.0223(4) Uani 1 d . . Cl2 Cl 0.7474(3) 0.94075(12) 0.28085(10) 0.0253(5) Uani 1 d . . Cl3 Cl 0.9148(3) 0.78304(11) 0.28573(9) 0.0208(4) Uani 1 d . . Cl4 Cl 0.5695(4) 0.7218(2) 0.43104(15) 0.0498(7) Uani 1 d . . Cl5 Cl 0.7973(4) 0.8441(2) 0.47195(15) 0.0530(8) Uani 1 d . . Cl6 Cl 1.1024(4) 1.0073(2) 0.4231(2) 0.0615(9) Uani 1 d . . Cl7 Cl 1.2706(4) 0.8654(2) 0.4248(2) 0.0552(8) Uani 1 d . . N1 N 0.5897(8) 0.7839(4) 0.2098(3) 0.0167(14) Uani 1 d . . N2 N 0.8374(8) 0.7512(4) 0.1497(3) 0.0128(13) Uani 1 d . . C1 C 0.6619(11) 0.8571(5) 0.0676(4) 0.022(2) Uani 1 d . . C2 C 0.5314(10) 0.8756(4) 0.0992(4) 0.019(2) Uani 1 d . . C3 C 0.5702(11) 0.9422(5) 0.1372(4) 0.024(2) Uani 1 d . . C4 C 0.7301(11) 0.9658(5) 0.1286(4) 0.024(2) Uani 1 d . . C5 C 0.7879(11) 0.9110(5) 0.0845(4) 0.021(2) Uani 1 d . . C6 C 0.6577(13) 0.7961(6) 0.0174(4) 0.031(2) Uani 1 d . . H6A H 0.5971(13) 0.7541(6) 0.0293(4) 0.080 Uiso 1 d R . H6B H 0.7670(13) 0.7797(6) 0.0162(4) 0.080 Uiso 1 d R . C7 C 0.5761(16) 0.8262(7) -0.0512(5) 0.047(3) Uani 1 d . . H7A H 0.5727(16) 0.7874(7) -0.0839(5) 0.080 Uiso 1 d R . H7B H 0.4667(16) 0.8421(7) -0.0497(5) 0.080 Uiso 1 d R . H7C H 0.6378(16) 0.8679(7) -0.0628(5) 0.080 Uiso 1 d R . C8 C 0.3692(12) 0.8371(6) 0.0883(5) 0.031(2) Uani 1 d . . H8A H 0.3004(12) 0.8571(6) 0.0492(5) 0.080 Uiso 1 d R . H8B H 0.3844(12) 0.7845(6) 0.0825(5) 0.080 Uiso 1 d R . H8C H 0.3186(12) 0.8451(6) 0.1261(5) 0.080 Uiso 1 d R . C9 C 0.4529(12) 0.9878(5) 0.1670(5) 0.033(2) Uani 1 d . . H9A H 0.3848(12) 1.0162(5) 0.1327(5) 0.080 Uiso 1 d R . H9B H 0.3859(12) 0.9555(5) 0.1880(5) 0.080 Uiso 1 d R . H9C H 0.5124(12) 1.0213(5) 0.1995(5) 0.080 Uiso 1 d R . C10 C 0.8079(14) 1.0409(5) 0.1472(6) 0.040(3) Uani 1 d . . H10A H 0.7661(14) 1.0767(5) 0.1133(6) 0.080 Uiso 1 d R . H10B H 0.7827(14) 1.0569(5) 0.1889(6) 0.080 Uiso 1 d R . H10C H 0.9244(14) 1.0369(5) 0.1512(6) 0.080 Uiso 1 d R . C11 C 0.9261(13) 0.9223(6) 0.0493(5) 0.038(2) Uani 1 d . . H11A H 0.8870(13) 0.9462(6) 0.0073(5) 0.080 Uiso 1 d R . H11B H 1.0077(13) 0.9532(6) 0.0758(5) 0.080 Uiso 1 d R . H11C H 0.9730(13) 0.8747(6) 0.0419(5) 0.080 Uiso 1 d R . C12 C 0.4677(10) 0.8036(5) 0.2401(4) 0.021(2) Uani 1 d . . H12A H 0.4569(10) 0.8553(5) 0.2511(4) 0.080 Uiso 1 d R . C13 C 0.3561(11) 0.7530(5) 0.2564(4) 0.025(2) Uani 1 d . . H13A H 0.2684(11) 0.7696(5) 0.2773(4) 0.080 Uiso 1 d R . C14 C 0.3728(11) 0.6770(5) 0.2420(4) 0.027(2) Uani 1 d . . C15 C 0.4970(11) 0.6569(4) 0.2098(4) 0.023(2) Uani 1 d . . H15A H 0.5097(11) 0.6054(4) 0.1985(4) 0.080 Uiso 1 d R . C16 C 0.6045(10) 0.7103(4) 0.1932(4) 0.017(2) Uani 1 d . . C17 C 0.2588(12) 0.6198(6) 0.2623(5) 0.035(2) Uani 1 d . . H17A H 0.2873(12) 0.5710(6) 0.2487(5) 0.080 Uiso 1 d R . H17B H 0.2683(12) 0.6207(6) 0.3098(5) 0.080 Uiso 1 d R . H17C H 0.1483(12) 0.6312(6) 0.2415(5) 0.080 Uiso 1 d R . C18 C 0.9674(11) 0.7385(5) 0.1221(4) 0.019(2) Uani 1 d . . H18A H 1.0372(11) 0.7797(5) 0.1162(4) 0.080 Uiso 1 d R . C19 C 1.0056(11) 0.6678(5) 0.1012(4) 0.024(2) Uani 1 d . . H19A H 1.0990(11) 0.6609(5) 0.0806(4) 0.080 Uiso 1 d R . C20 C 0.9081(11) 0.6075(5) 0.1104(4) 0.024(2) Uani 1 d . . C21 C 0.7769(11) 0.6207(4) 0.1406(4) 0.019(2) Uani 1 d . . H21A H 0.7096(11) 0.5795(4) 0.1491(4) 0.080 Uiso 1 d R . C22 C 0.7396(10) 0.6927(4) 0.1592(4) 0.016(2) Uani 1 d . . C23 C 0.9438(14) 0.5291(5) 0.0889(5) 0.034(2) Uani 1 d . . H23A H 0.8630(14) 0.4952(5) 0.0995(5) 0.080 Uiso 1 d R . H23B H 0.9406(14) 0.5286(5) 0.0417(5) 0.080 Uiso 1 d R . H23C H 1.0504(14) 0.5139(5) 0.1117(5) 0.080 Uiso 1 d R . C24 C 0.6663(14) 0.8008(7) 0.4055(5) 0.045(3) Uani 1 d . . H24A H 0.5846(14) 0.8360(7) 0.3854(5) 0.080 Uiso 1 d R . H24B H 0.7280(14) 0.7862(7) 0.3724(5) 0.080 Uiso 1 d R . C25 C 1.1194(15) 0.9242(7) 0.3811(5) 0.048(3) Uani 1 d . . H25A H 1.1449(15) 0.9354(7) 0.3383(5) 0.080 Uiso 1 d R . H25B H 1.0161(15) 0.8987(7) 0.3740(5) 0.080 Uiso 1 d 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 0.0107(2) 0.00924(14) 0.0192(2) -0.00020(13) 0.00450(10) -0.00086(13) Cl1 0.0121(11) 0.0218(10) 0.0339(11) 0.0006(8) 0.0067(8) -0.0040(8) Cl2 0.0280(13) 0.0212(10) 0.0286(10) -0.0074(8) 0.0103(9) 0.0012(9) Cl3 0.0191(11) 0.0221(10) 0.0209(9) 0.0008(8) 0.0028(7) 0.0022(8) Cl4 0.054(2) 0.0410(15) 0.054(2) 0.0079(13) 0.0081(13) 0.0051(13) Cl5 0.066(2) 0.044(2) 0.049(2) -0.0026(13) 0.0118(14) -0.0032(14) Cl6 0.059(2) 0.047(2) 0.069(2) -0.025(2) -0.012(2) 0.018(2) Cl7 0.046(2) 0.0346(14) 0.078(2) 0.0062(14) -0.0052(14) 0.0079(13) N1 0.011(4) 0.013(3) 0.025(3) 0.001(3) 0.001(3) -0.004(3) N2 0.008(3) 0.014(3) 0.017(3) -0.002(2) 0.006(2) -0.002(3) C1 0.022(5) 0.018(4) 0.024(4) 0.008(3) 0.003(3) 0.011(4) C2 0.014(5) 0.017(4) 0.023(4) 0.005(3) 0.000(3) -0.002(3) C3 0.024(5) 0.018(4) 0.033(5) -0.001(4) 0.010(4) 0.005(4) C4 0.020(5) 0.012(4) 0.037(5) 0.009(3) -0.001(4) -0.002(3) C5 0.019(5) 0.017(4) 0.027(4) 0.004(3) 0.001(3) -0.002(3) C6 0.039(6) 0.038(5) 0.015(4) -0.007(4) -0.001(4) 0.005(5) C7 0.061(8) 0.053(7) 0.025(5) 0.001(5) 0.001(5) 0.013(6) C8 0.026(6) 0.035(5) 0.032(5) 0.003(4) 0.003(4) -0.008(4) C9 0.022(5) 0.027(5) 0.051(6) 0.000(4) 0.010(4) 0.015(4) C10 0.039(7) 0.016(4) 0.065(7) 0.002(5) 0.009(5) -0.009(4) C11 0.041(7) 0.044(6) 0.034(5) 0.008(5) 0.017(4) -0.014(5) C12 0.014(5) 0.020(4) 0.032(4) -0.001(3) 0.015(3) 0.001(3) C13 0.017(5) 0.028(5) 0.032(5) 0.004(4) 0.009(4) -0.003(4) C14 0.020(5) 0.031(5) 0.032(5) 0.009(4) 0.009(4) 0.000(4) C15 0.022(5) 0.013(4) 0.033(5) 0.007(3) 0.004(4) -0.005(3) C16 0.013(4) 0.014(4) 0.022(4) 0.002(3) -0.002(3) 0.002(3) C17 0.020(5) 0.034(6) 0.054(6) 0.012(5) 0.016(5) -0.012(4) C18 0.029(5) 0.016(4) 0.015(4) -0.001(3) 0.009(3) -0.002(4) C19 0.023(5) 0.022(4) 0.028(4) -0.002(3) 0.011(4) 0.005(4) C20 0.026(5) 0.015(4) 0.030(5) -0.002(3) 0.006(4) 0.006(4) C21 0.023(5) 0.010(4) 0.025(4) 0.002(3) 0.007(3) -0.002(3) C22 0.016(4) 0.012(4) 0.019(4) 0.006(3) -0.002(3) -0.002(3) C23 0.051(7) 0.011(4) 0.046(6) -0.008(4) 0.023(5) 0.001(4) C24 0.045(7) 0.057(7) 0.035(6) 0.009(5) 0.013(5) 0.004(6) C25 0.045(7) 0.049(7) 0.041(6) -0.012(5) -0.011(5) 0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N2 2.163(6) . ? W1 N1 2.164(7) . ? W1 C4 2.243(8) . ? W1 C5 2.307(8) . ? W1 C3 2.344(9) . ? W1 C1 2.436(8) . ? W1 C2 2.453(8) . ? W1 Cl2 2.470(2) . ? W1 Cl1 2.487(2) . ? W1 Cl3 2.533(2) . ? Cl4 C24 1.755(12) . ? Cl5 C24 1.754(12) . ? Cl6 C25 1.735(11) . ? Cl7 C25 1.751(11) . ? N1 C12 1.333(10) . ? N1 C16 1.370(10) . ? N2 C18 1.332(10) . ? N2 C22 1.362(10) . ? C1 C2 1.405(12) . ? C1 C5 1.419(12) . ? C1 C6 1.494(12) . ? C2 C3 1.425(12) . ? C2 C8 1.494(12) . ? C3 C4 1.439(13) . ? C3 C9 1.489(12) . ? C4 C5 1.473(13) . ? C4 C10 1.508(12) . ? C5 C11 1.482(13) . ? C6 C7 1.537(12) . ? C12 C13 1.382(12) . ? C13 C14 1.402(13) . ? C14 C15 1.375(13) . ? C14 C17 1.507(12) . ? C15 C16 1.393(11) . ? C16 C22 1.465(12) . ? C18 C19 1.391(11) . ? C19 C20 1.383(13) . ? C20 C21 1.373(12) . ? C20 C23 1.516(11) . ? C21 C22 1.395(11) . ? 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 N2 W1 N1 75.8(2) . . ? N2 W1 C4 127.0(3) . . ? N1 W1 C4 126.1(3) . . ? N2 W1 C5 89.5(3) . . ? N1 W1 C5 127.4(3) . . ? C4 W1 C5 37.8(3) . . ? N2 W1 C3 128.3(3) . . ? N1 W1 C3 89.9(3) . . ? C4 W1 C3 36.5(3) . . ? C5 W1 C3 60.6(3) . . ? N2 W1 C1 73.4(3) . . ? N1 W1 C1 93.2(3) . . ? C4 W1 C1 59.3(3) . . ? C5 W1 C1 34.7(3) . . ? C3 W1 C1 57.8(3) . . ? N2 W1 C2 94.4(3) . . ? N1 W1 C2 73.2(3) . . ? C4 W1 C2 58.6(3) . . ? C5 W1 C2 57.7(3) . . ? C3 W1 C2 34.5(3) . . ? C1 W1 C2 33.4(3) . . ? N2 W1 Cl2 149.7(2) . . ? N1 W1 Cl2 91.1(2) . . ? C4 W1 Cl2 82.8(2) . . ? C5 W1 Cl2 119.6(2) . . ? C3 W1 Cl2 77.9(2) . . ? C1 W1 Cl2 135.4(2) . . ? C2 W1 Cl2 108.0(2) . . ? N2 W1 Cl1 92.8(2) . . ? N1 W1 Cl1 151.0(2) . . ? C4 W1 Cl1 82.1(2) . . ? C5 W1 Cl1 78.1(2) . . ? C3 W1 Cl1 117.5(2) . . ? C1 W1 Cl1 109.3(2) . . ? C2 W1 Cl1 135.1(2) . . ? Cl2 W1 Cl1 85.67(7) . . ? N2 W1 Cl3 72.5(2) . . ? N1 W1 Cl3 74.4(2) . . ? C4 W1 Cl3 152.1(2) . . ? C5 W1 Cl3 148.1(2) . . ? C3 W1 Cl3 150.5(2) . . ? C1 W1 Cl3 145.7(2) . . ? C2 W1 Cl3 147.1(2) . . ? Cl2 W1 Cl3 77.68(7) . . ? Cl1 W1 Cl3 76.74(7) . . ? C12 N1 C16 118.8(7) . . ? C12 N1 W1 125.2(5) . . ? C16 N1 W1 116.0(5) . . ? C18 N2 C22 119.0(7) . . ? C18 N2 W1 124.5(5) . . ? C22 N2 W1 116.4(5) . . ? C2 C1 C5 109.1(8) . . ? C2 C1 C6 124.7(8) . . ? C5 C1 C6 125.7(8) . . ? C2 C1 W1 74.0(5) . . ? C5 C1 W1 67.7(5) . . ? C6 C1 W1 130.5(6) . . ? C1 C2 C3 109.5(8) . . ? C1 C2 C8 125.3(8) . . ? C3 C2 C8 124.8(8) . . ? C1 C2 W1 72.6(5) . . ? C3 C2 W1 68.6(5) . . ? C8 C2 W1 130.7(6) . . ? C2 C3 C4 107.3(7) . . ? C2 C3 C9 125.7(9) . . ? C4 C3 C9 125.6(8) . . ? C2 C3 W1 77.0(5) . . ? C4 C3 W1 68.0(5) . . ? C9 C3 W1 130.8(6) . . ? C3 C4 C5 107.3(7) . . ? C3 C4 C10 126.4(9) . . ? C5 C4 C10 124.9(8) . . ? C3 C4 W1 75.6(5) . . ? C5 C4 W1 73.5(5) . . ? C10 C4 W1 127.3(7) . . ? C1 C5 C4 106.8(7) . . ? C1 C5 C11 125.5(8) . . ? C4 C5 C11 125.5(8) . . ? C1 C5 W1 77.7(5) . . ? C4 C5 W1 68.8(4) . . ? C11 C5 W1 131.9(6) . . ? C1 C6 C7 108.7(8) . . ? N1 C12 C13 123.0(8) . . ? C12 C13 C14 119.1(8) . . ? C15 C14 C13 117.9(8) . . ? C15 C14 C17 121.7(9) . . ? C13 C14 C17 120.5(9) . . ? C14 C15 C16 120.9(8) . . ? N1 C16 C15 120.3(8) . . ? N1 C16 C22 115.9(7) . . ? C15 C16 C22 123.7(7) . . ? N2 C18 C19 122.5(8) . . ? C20 C19 C18 119.5(8) . . ? C21 C20 C19 117.7(8) . . ? C21 C20 C23 120.4(8) . . ? C19 C20 C23 121.9(8) . . ? C20 C21 C22 121.2(8) . . ? N2 C22 C21 120.1(7) . . ? N2 C22 C16 115.9(7) . . ? C21 C22 C16 123.9(7) . . ? Cl5 C24 Cl4 112.2(6) . . ? Cl6 C25 Cl7 112.3(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 W1 N1 C12 -179.9(7) . . . . ? C4 W1 N1 C12 -54.2(8) . . . . ? C5 W1 N1 C12 -101.8(7) . . . . ? C3 W1 N1 C12 -50.2(7) . . . . ? C1 W1 N1 C12 -107.9(7) . . . . ? C2 W1 N1 C12 -80.8(7) . . . . ? Cl2 W1 N1 C12 27.7(7) . . . . ? Cl1 W1 N1 C12 110.7(7) . . . . ? Cl3 W1 N1 C12 104.6(7) . . . . ? N2 W1 N1 C16 2.0(5) . . . . ? C4 W1 N1 C16 127.7(6) . . . . ? C5 W1 N1 C16 80.1(6) . . . . ? C3 W1 N1 C16 131.7(6) . . . . ? C1 W1 N1 C16 74.0(6) . . . . ? C2 W1 N1 C16 101.1(6) . . . . ? Cl2 W1 N1 C16 -150.4(5) . . . . ? Cl1 W1 N1 C16 -67.4(7) . . . . ? Cl3 W1 N1 C16 -73.5(5) . . . . ? N1 W1 N2 C18 -177.6(7) . . . . ? C4 W1 N2 C18 57.6(7) . . . . ? C5 W1 N2 C18 53.4(6) . . . . ? C3 W1 N2 C18 104.1(7) . . . . ? C1 W1 N2 C18 84.7(6) . . . . ? C2 W1 N2 C18 111.0(6) . . . . ? Cl2 W1 N2 C18 -110.8(6) . . . . ? Cl1 W1 N2 C18 -24.6(6) . . . . ? Cl3 W1 N2 C18 -99.8(6) . . . . ? N1 W1 N2 C22 -1.0(5) . . . . ? C4 W1 N2 C22 -125.8(6) . . . . ? C5 W1 N2 C22 -130.0(6) . . . . ? C3 W1 N2 C22 -79.3(6) . . . . ? C1 W1 N2 C22 -98.8(6) . . . . ? C2 W1 N2 C22 -72.4(6) . . . . ? Cl2 W1 N2 C22 65.8(7) . . . . ? Cl1 W1 N2 C22 152.0(5) . . . . ? Cl3 W1 N2 C22 76.8(5) . . . . ? N2 W1 C1 C2 126.5(5) . . . . ? N1 W1 C1 C2 52.3(5) . . . . ? C4 W1 C1 C2 -78.5(5) . . . . ? C5 W1 C1 C2 -119.1(7) . . . . ? C3 W1 C1 C2 -35.5(5) . . . . ? C2 W1 C1 C2 0.000(2) . . . . ? Cl2 W1 C1 C2 -42.4(6) . . . . ? Cl1 W1 C1 C2 -146.4(4) . . . . ? Cl3 W1 C1 C2 119.0(5) . . . . ? N2 W1 C1 C5 -114.4(5) . . . . ? N1 W1 C1 C5 171.5(5) . . . . ? C4 W1 C1 C5 40.7(5) . . . . ? C5 W1 C1 C5 0.000(3) . . . . ? C3 W1 C1 C5 83.7(6) . . . . ? C2 W1 C1 C5 119.1(7) . . . . ? Cl2 W1 C1 C5 76.7(6) . . . . ? Cl1 W1 C1 C5 -27.2(5) . . . . ? Cl3 W1 C1 C5 -121.9(5) . . . . ? N2 W1 C1 C6 4.3(8) . . . . ? N1 W1 C1 C6 -69.9(9) . . . . ? C4 W1 C1 C6 159.3(10) . . . . ? C5 W1 C1 C6 118.6(10) . . . . ? C3 W1 C1 C6 -157.7(10) . . . . ? C2 W1 C1 C6 -122.2(11) . . . . ? Cl2 W1 C1 C6 -164.7(7) . . . . ? Cl1 W1 C1 C6 91.4(8) . . . . ? Cl3 W1 C1 C6 -3.2(11) . . . . ? C5 C1 C2 C3 0.1(9) . . . . ? C6 C1 C2 C3 -172.6(8) . . . . ? W1 C1 C2 C3 58.9(6) . . . . ? C5 C1 C2 C8 173.3(8) . . . . ? C6 C1 C2 C8 0.6(13) . . . . ? W1 C1 C2 C8 -128.0(8) . . . . ? C5 C1 C2 W1 -58.8(6) . . . . ? C6 C1 C2 W1 128.5(8) . . . . ? W1 C1 C2 W1 0.000(1) . . . . ? N2 W1 C2 C1 -50.6(5) . . . . ? N1 W1 C2 C1 -124.3(5) . . . . ? C4 W1 C2 C1 80.7(6) . . . . ? C5 W1 C2 C1 36.0(5) . . . . ? C3 W1 C2 C1 119.9(7) . . . . ? C1 W1 C2 C1 0.000(2) . . . . ? Cl2 W1 C2 C1 150.1(4) . . . . ? Cl1 W1 C2 C1 47.8(6) . . . . ? Cl3 W1 C2 C1 -114.7(5) . . . . ? N2 W1 C2 C3 -170.4(5) . . . . ? N1 W1 C2 C3 115.8(5) . . . . ? C4 W1 C2 C3 -39.1(5) . . . . ? C5 W1 C2 C3 -83.9(5) . . . . ? C3 W1 C2 C3 0.000(4) . . . . ? C1 W1 C2 C3 -119.9(7) . . . . ? Cl2 W1 C2 C3 30.3(5) . . . . ? Cl1 W1 C2 C3 -72.1(6) . . . . ? Cl3 W1 C2 C3 125.5(5) . . . . ? N2 W1 C2 C8 71.4(8) . . . . ? N1 W1 C2 C8 -2.4(8) . . . . ? C4 W1 C2 C8 -157.3(9) . . . . ? C5 W1 C2 C8 158.0(9) . . . . ? C3 W1 C2 C8 -118.2(10) . . . . ? C1 W1 C2 C8 122.0(10) . . . . ? Cl2 W1 C2 C8 -87.9(8) . . . . ? Cl1 W1 C2 C8 169.7(7) . . . . ? Cl3 W1 C2 C8 7.3(10) . . . . ? C1 C2 C3 C4 0.2(9) . . . . ? C8 C2 C3 C4 -173.0(8) . . . . ? W1 C2 C3 C4 61.6(6) . . . . ? C1 C2 C3 C9 167.4(8) . . . . ? C8 C2 C3 C9 -5.8(14) . . . . ? W1 C2 C3 C9 -131.2(9) . . . . ? C1 C2 C3 W1 -61.4(6) . . . . ? C8 C2 C3 W1 125.4(8) . . . . ? W1 C2 C3 W1 0.000(2) . . . . ? N2 W1 C3 C2 12.2(6) . . . . ? N1 W1 C3 C2 -59.5(5) . . . . ? C4 W1 C3 C2 115.0(7) . . . . ? C5 W1 C3 C2 74.9(5) . . . . ? C1 W1 C3 C2 34.4(5) . . . . ? C2 W1 C3 C2 0.000(4) . . . . ? Cl2 W1 C3 C2 -150.6(5) . . . . ? Cl1 W1 C3 C2 130.8(4) . . . . ? Cl3 W1 C3 C2 -116.0(5) . . . . ? N2 W1 C3 C4 -102.9(5) . . . . ? N1 W1 C3 C4 -174.6(5) . . . . ? C4 W1 C3 C4 0.0 . . . . ? C5 W1 C3 C4 -40.2(5) . . . . ? C1 W1 C3 C4 -80.7(6) . . . . ? C2 W1 C3 C4 -115.0(7) . . . . ? Cl2 W1 C3 C4 94.3(5) . . . . ? Cl1 W1 C3 C4 15.7(6) . . . . ? Cl3 W1 C3 C4 129.0(5) . . . . ? N2 W1 C3 C9 138.4(8) . . . . ? N1 W1 C3 C9 66.7(9) . . . . ? C4 W1 C3 C9 -118.8(11) . . . . ? C5 W1 C3 C9 -159.0(10) . . . . ? C1 W1 C3 C9 160.6(10) . . . . ? C2 W1 C3 C9 126.2(11) . . . . ? Cl2 W1 C3 C9 -24.4(8) . . . . ? Cl1 W1 C3 C9 -103.0(8) . . . . ? Cl3 W1 C3 C9 10.2(12) . . . . ? C2 C3 C4 C5 -0.4(9) . . . . ? C9 C3 C4 C5 -167.6(8) . . . . ? W1 C3 C4 C5 67.2(5) . . . . ? C2 C3 C4 C10 166.4(9) . . . . ? C9 C3 C4 C10 -0.8(15) . . . . ? W1 C3 C4 C10 -126.0(10) . . . . ? C2 C3 C4 W1 -67.6(6) . . . . ? C9 C3 C4 W1 125.2(9) . . . . ? W1 C3 C4 W1 0.0 . . . . ? N2 W1 C4 C3 106.5(5) . . . . ? N1 W1 C4 C3 6.7(7) . . . . ? C5 W1 C4 C3 113.4(7) . . . . ? C3 W1 C4 C3 0.0 . . . . ? C1 W1 C4 C3 76.1(5) . . . . ? C2 W1 C4 C3 36.9(5) . . . . ? Cl2 W1 C4 C3 -79.3(5) . . . . ? Cl1 W1 C4 C3 -165.9(5) . . . . ? Cl3 W1 C4 C3 -125.1(5) . . . . ? N2 W1 C4 C5 -6.8(6) . . . . ? N1 W1 C4 C5 -106.6(5) . . . . ? C5 W1 C4 C5 0.000(4) . . . . ? C3 W1 C4 C5 -113.4(7) . . . . ? C1 W1 C4 C5 -37.3(5) . . . . ? C2 W1 C4 C5 -76.5(5) . . . . ? Cl2 W1 C4 C5 167.3(5) . . . . ? Cl1 W1 C4 C5 80.7(5) . . . . ? Cl3 W1 C4 C5 121.5(5) . . . . ? N2 W1 C4 C10 -128.4(8) . . . . ? N1 W1 C4 C10 131.8(8) . . . . ? C5 W1 C4 C10 -121.6(11) . . . . ? C3 W1 C4 C10 125.1(11) . . . . ? C1 W1 C4 C10 -158.8(10) . . . . ? C2 W1 C4 C10 162.0(10) . . . . ? Cl2 W1 C4 C10 45.8(9) . . . . ? Cl1 W1 C4 C10 -40.8(8) . . . . ? Cl3 W1 C4 C10 0.0(13) . . . . ? C2 C1 C5 C4 -0.4(9) . . . . ? C6 C1 C5 C4 172.2(8) . . . . ? W1 C1 C5 C4 -63.1(5) . . . . ? C2 C1 C5 C11 -164.2(8) . . . . ? C6 C1 C5 C11 8.4(14) . . . . ? W1 C1 C5 C11 133.1(9) . . . . ? C2 C1 C5 W1 62.7(6) . . . . ? C6 C1 C5 W1 -124.7(8) . . . . ? W1 C1 C5 W1 0.000(2) . . . . ? C3 C4 C5 C1 0.5(9) . . . . ? C10 C4 C5 C1 -166.6(8) . . . . ? W1 C4 C5 C1 69.1(6) . . . . ? C3 C4 C5 C11 164.3(9) . . . . ? C10 C4 C5 C11 -2.8(14) . . . . ? W1 C4 C5 C11 -127.1(9) . . . . ? C3 C4 C5 W1 -68.6(6) . . . . ? C10 C4 C5 W1 124.3(9) . . . . ? W1 C4 C5 W1 0.000(3) . . . . ? N2 W1 C5 C1 60.8(5) . . . . ? N1 W1 C5 C1 -10.7(6) . . . . ? C4 W1 C5 C1 -113.7(7) . . . . ? C3 W1 C5 C1 -74.9(5) . . . . ? C1 W1 C5 C1 0.000(3) . . . . ? C2 W1 C5 C1 -34.7(5) . . . . ? Cl2 W1 C5 C1 -128.2(4) . . . . ? Cl1 W1 C5 C1 153.8(5) . . . . ? Cl3 W1 C5 C1 115.2(5) . . . . ? N2 W1 C5 C4 174.6(5) . . . . ? N1 W1 C5 C4 103.0(5) . . . . ? C4 W1 C5 C4 0.000(5) . . . . ? C3 W1 C5 C4 38.8(5) . . . . ? C1 W1 C5 C4 113.7(7) . . . . ? C2 W1 C5 C4 79.0(5) . . . . ? Cl2 W1 C5 C4 -14.5(5) . . . . ? Cl1 W1 C5 C4 -92.5(5) . . . . ? Cl3 W1 C5 C4 -131.1(5) . . . . ? N2 W1 C5 C11 -66.1(9) . . . . ? N1 W1 C5 C11 -137.7(8) . . . . ? C4 W1 C5 C11 119.3(11) . . . . ? C3 W1 C5 C11 158.1(10) . . . . ? C1 W1 C5 C11 -127.0(11) . . . . ? C2 W1 C5 C11 -161.7(10) . . . . ? Cl2 W1 C5 C11 104.8(9) . . . . ? Cl1 W1 C5 C11 26.8(9) . . . . ? Cl3 W1 C5 C11 -11.8(12) . . . . ? C2 C1 C6 C7 83.3(11) . . . . ? C5 C1 C6 C7 -88.2(11) . . . . ? W1 C1 C6 C7 -178.1(7) . . . . ? C16 N1 C12 C13 0.8(13) . . . . ? W1 N1 C12 C13 -177.2(6) . . . . ? N1 C12 C13 C14 1.5(14) . . . . ? C12 C13 C14 C15 -2.4(13) . . . . ? C12 C13 C14 C17 176.7(9) . . . . ? C13 C14 C15 C16 1.3(13) . . . . ? C17 C14 C15 C16 -177.9(8) . . . . ? C12 N1 C16 C15 -2.0(11) . . . . ? W1 N1 C16 C15 176.2(6) . . . . ? C12 N1 C16 C22 179.1(7) . . . . ? W1 N1 C16 C22 -2.7(9) . . . . ? C14 C15 C16 N1 1.0(12) . . . . ? C14 C15 C16 C22 179.7(8) . . . . ? C22 N2 C18 C19 1.3(12) . . . . ? W1 N2 C18 C19 177.8(6) . . . . ? N2 C18 C19 C20 -1.3(13) . . . . ? C18 C19 C20 C21 -0.4(13) . . . . ? C18 C19 C20 C23 -179.9(9) . . . . ? C19 C20 C21 C22 2.2(13) . . . . ? C23 C20 C21 C22 -178.3(8) . . . . ? C18 N2 C22 C21 0.6(11) . . . . ? W1 N2 C22 C21 -176.2(6) . . . . ? C18 N2 C22 C16 176.7(7) . . . . ? W1 N2 C22 C16 -0.1(9) . . . . ? C20 C21 C22 N2 -2.4(12) . . . . ? C20 C21 C22 C16 -178.2(8) . . . . ? N1 C16 C22 N2 1.8(10) . . . . ? C15 C16 C22 N2 -177.0(7) . . . . ? N1 C16 C22 C21 177.8(7) . . . . ? C15 C16 C22 C21 -1.0(12) . . . . ? _refine_diff_density_max 1.508 _refine_diff_density_min -2.734 _refine_diff_density_rms 0.163 # CIF-file generated for Complex 2-Me+BPh4- data_complex_2Me+BPh4- _audit_creation_method SHELXL #========================================================== _publ_contact_author_name 'Peter Burger' _publ_contact_author_address ; 'Anorg.-Chem Inst., University of Zuerich, Winterthurerstr. 190, 8057 Zuerich' ; _publ_contact_author_email 'chburger@aci.unizh.ch' _publ_contact_author_fax '+41 1 635 6802' _publ_contact_author_phone '+41 1 635 4692' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' loop_ _publ_author_name 'Peter Burger' 'Christian Cremer' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural Cp*W(Me-bipy)Cl2+BPh4- _chemical_formula_sum 'C46 H47 B Cl2 N2 W' _chemical_formula_weight 893.42 _chemical_melting_point n/a _chemical_compound_source synthesis 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' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _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 11.6720(10) _cell_length_b 16.362(2) _cell_length_c 21.122(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.610(10) _cell_angle_gamma 90.00 _cell_volume 3977.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5000 _exptl_crystal_description 'rectangular parallelepiped' _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method n/a _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 3.074 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.44 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS Image Plate system' _diffrn_measurement_method 'Image Plate with incremental Phi-angle' _diffrn_reflns_number 7678 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.91 _reflns_number_total 7678 _reflns_number_observed 5722 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE IPDS Program Package' _computing_cell_refinement 'STOE IPDS Program Package' _computing_data_reduction 'STOE IPDS Program Package' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1988)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Platon (Spek, 1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993);' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0100P)^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 'riding model' _refine_ls_extinction_method n/a _refine_ls_extinction_coef n/a _refine_ls_number_reflns 7678 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_obs 0.0192 _refine_ls_wR_factor_all 0.0372 _refine_ls_wR_factor_obs 0.0363 _refine_ls_goodness_of_fit_all 0.991 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 0.991 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.708652(12) 0.143574(9) 0.055386(6) 0.02541(3) Uani 1 d . . Cl1 Cl 0.73723(7) 0.17999(5) -0.04872(4) 0.0396(2) Uani 1 d . . Cl2 Cl 0.85180(7) 0.04415(5) 0.04556(4) 0.0411(2) Uani 1 d . . N1 N 0.6257(2) 0.0454(2) 0.09655(11) 0.0276(5) Uani 1 d . . N2 N 0.5272(2) 0.1522(2) 0.01675(10) 0.0270(5) Uani 1 d . . B1 B 0.7279(3) -0.0933(2) -0.3034(2) 0.0304(8) Uani 1 d . . C1 C 0.6959(3) 0.2095(2) 0.1504(2) 0.0403(8) Uani 1 d . . C2 C 0.8110(3) 0.1810(2) 0.15386(15) 0.0423(8) Uani 1 d . . C3 C 0.8608(3) 0.2238(2) 0.1079(2) 0.0451(9) Uani 1 d . . C4 C 0.7803(4) 0.2802(2) 0.0775(2) 0.0520(10) Uani 1 d . . C5 C 0.6755(3) 0.2708(2) 0.1030(2) 0.0476(9) Uani 1 d . . C6 C 0.6122(4) 0.1882(3) 0.1949(2) 0.084(2) Uani 1 d . . H6A H 0.6238(4) 0.2246(3) 0.2310(2) 0.080 Uiso 1 d R . H6B H 0.5338(4) 0.1932(3) 0.1726(2) 0.080 Uiso 1 d R . H6C H 0.6258(4) 0.1329(3) 0.2096(2) 0.080 Uiso 1 d R . C7 C 0.8751(4) 0.1260(3) 0.2049(2) 0.083(2) Uani 1 d . . H7A H 0.9100(4) 0.1581(3) 0.2410(2) 0.080 Uiso 1 d R . H7B H 0.8214(4) 0.0878(3) 0.2182(2) 0.080 Uiso 1 d R . H7C H 0.9344(4) 0.0968(3) 0.1878(2) 0.080 Uiso 1 d R . C8 C 0.9852(3) 0.2170(3) 0.0974(2) 0.093(2) Uani 1 d . . H8A H 1.0323(3) 0.2559(3) 0.1240(2) 0.080 Uiso 1 d R . H8B H 1.0132(3) 0.1628(3) 0.1083(2) 0.080 Uiso 1 d R . H8C H 0.9892(3) 0.2277(3) 0.0531(2) 0.080 Uiso 1 d R . C9 C 0.8023(5) 0.3444(3) 0.0307(2) 0.100(2) Uani 1 d . . H9A H 0.8310(5) 0.3930(3) 0.0535(2) 0.080 Uiso 1 d R . H9B H 0.8587(5) 0.3249(3) 0.0061(2) 0.080 Uiso 1 d R . H9C H 0.7311(5) 0.3566(3) 0.0025(2) 0.080 Uiso 1 d R . C10 C 0.5724(4) 0.3239(3) 0.0878(3) 0.096(2) Uani 1 d . . H10A H 0.5827(4) 0.3717(3) 0.1145(3) 0.080 Uiso 1 d R . H10B H 0.5625(4) 0.3399(3) 0.0434(3) 0.080 Uiso 1 d R . H10C H 0.5048(4) 0.2945(3) 0.0955(3) 0.080 Uiso 1 d R . C11 C 0.6831(3) -0.0132(2) 0.1359(2) 0.0366(7) Uani 1 d . . H11A H 0.7664(3) -0.0144(2) 0.1419(2) 0.080 Uiso 1 d R . C12 C 0.6269(3) -0.0701(2) 0.16685(15) 0.0378(8) Uani 1 d . . H12A H 0.6714(3) -0.1098(2) 0.19402(15) 0.080 Uiso 1 d R . C13 C 0.5069(3) -0.0711(2) 0.15973(13) 0.0302(7) Uani 1 d . . C14 C 0.4473(3) -0.0128(2) 0.11942(13) 0.0288(6) Uani 1 d . . H14A H 0.3639(3) -0.0116(2) 0.11288(13) 0.080 Uiso 1 d R . C15 C 0.5067(2) 0.0433(2) 0.08850(13) 0.0258(6) Uani 1 d . . C16 C 0.4442(3) -0.1335(2) 0.19268(14) 0.0390(7) Uani 1 d . . H16A H 0.4996(3) -0.1683(2) 0.21844(14) 0.080 Uiso 1 d R . H16B H 0.3974(3) -0.1065(2) 0.21964(14) 0.080 Uiso 1 d R . H16C H 0.3952(3) -0.1658(2) 0.16116(14) 0.080 Uiso 1 d R . C17 C 0.4794(3) 0.2076(2) -0.02831(14) 0.0319(7) Uani 1 d . . H17A H 0.5305(3) 0.2417(2) -0.04798(14) 0.080 Uiso 1 d R . C18 C 0.3620(3) 0.2168(2) -0.04692(15) 0.0351(7) Uani 1 d . . H18A H 0.3328(3) 0.2560(2) -0.07944(15) 0.080 Uiso 1 d R . C19 C 0.2848(3) 0.1699(2) -0.01893(15) 0.0338(7) Uani 1 d . . C20 C 0.3320(3) 0.1131(2) 0.02705(14) 0.0318(7) Uani 1 d . . H20A H 0.2816(3) 0.0794(2) 0.04752(14) 0.080 Uiso 1 d R . C21 C 0.4511(2) 0.1046(2) 0.04324(13) 0.0255(6) Uani 1 d . . C22 C 0.1559(3) 0.1795(2) -0.0390(2) 0.0503(9) Uani 1 d . . H22A H 0.1163(3) 0.1424(2) -0.0148(2) 0.080 Uiso 1 d R . H22B H 0.1339(3) 0.2346(2) -0.0310(2) 0.080 Uiso 1 d R . H22C H 0.1351(3) 0.1676(2) -0.0840(2) 0.080 Uiso 1 d R . C23 C 0.7786(3) -0.0878(2) -0.37230(15) 0.0349(7) Uani 1 d . . C24 C 0.8983(3) -0.0868(2) -0.3724(2) 0.0474(9) Uani 1 d . . H24A H 0.9504(3) -0.0894(2) -0.3322(2) 0.080 Uiso 1 d R . C25 C 0.9449(4) -0.0826(2) -0.4288(2) 0.0563(10) Uani 1 d . . H25A H 1.0276(4) -0.0832(2) -0.4270(2) 0.080 Uiso 1 d R . C26 C 0.8730(4) -0.0769(2) -0.4868(2) 0.0609(11) Uani 1 d . . H26A H 0.9052(4) -0.0736(2) -0.5257(2) 0.080 Uiso 1 d R . C27 C 0.7561(4) -0.0762(2) -0.4893(2) 0.0561(10) Uani 1 d . . H27A H 0.7053(4) -0.0727(2) -0.5300(2) 0.080 Uiso 1 d R . C28 C 0.7087(4) -0.0809(2) -0.43226(15) 0.0402(9) Uani 1 d . . H28A H 0.6259(4) -0.0790(2) -0.43477(15) 0.080 Uiso 1 d R . C29 C 0.7890(3) -0.0182(2) -0.25723(14) 0.0296(7) Uani 1 d . . C30 C 0.8231(3) -0.0236(2) -0.19080(15) 0.0352(7) Uani 1 d . . H30A H 0.8148(3) -0.0750(2) -0.17008(15) 0.080 Uiso 1 d R . C31 C 0.8694(3) 0.0425(2) -0.1530(2) 0.0414(8) Uani 1 d . . H31A H 0.8929(3) 0.0356(2) -0.1075(2) 0.080 Uiso 1 d R . C32 C 0.8814(3) 0.1182(2) -0.1804(2) 0.0415(9) Uani 1 d . . H32A H 0.9108(3) 0.1643(2) -0.1546(2) 0.080 Uiso 1 d R . C33 C 0.8496(3) 0.1255(2) -0.2467(2) 0.0409(9) Uani 1 d . . H33A H 0.8585(3) 0.1770(2) -0.2671(2) 0.080 Uiso 1 d R . C34 C 0.8055(3) 0.0589(2) -0.28293(15) 0.0361(7) Uani 1 d . . H34A H 0.7849(3) 0.0660(2) -0.32852(15) 0.080 Uiso 1 d R . C35 C 0.5859(3) -0.0809(2) -0.31866(13) 0.0301(7) Uani 1 d . . C36 C 0.5117(2) -0.1460(2) -0.33874(13) 0.0353(6) Uani 1 d . . H36A H 0.5441(2) -0.1998(2) -0.34024(13) 0.080 Uiso 1 d R . C37 C 0.3927(3) -0.1362(3) -0.35677(14) 0.0403(8) Uani 1 d . . H37A H 0.3453(3) -0.1825(3) -0.37162(14) 0.080 Uiso 1 d R . C38 C 0.3419(3) -0.0611(2) -0.3537(2) 0.0433(8) Uani 1 d . . H38A H 0.2594(3) -0.0543(2) -0.3655(2) 0.080 Uiso 1 d R . C39 C 0.4130(3) 0.0046(2) -0.3327(2) 0.0489(9) Uani 1 d . . H39A H 0.3798(3) 0.0579(2) -0.3303(2) 0.080 Uiso 1 d R . C40 C 0.5316(3) -0.0060(2) -0.3157(2) 0.0418(8) Uani 1 d . . H40A H 0.5786(3) 0.0405(2) -0.3009(2) 0.080 Uiso 1 d R . C41 C 0.7578(2) -0.1814(2) -0.26775(15) 0.0322(7) Uani 1 d . . C42 C 0.7048(3) -0.2027(2) -0.2147(2) 0.0390(8) Uani 1 d . . H42A H 0.6501(3) -0.1651(2) -0.2016(2) 0.080 Uiso 1 d R . C43 C 0.7276(3) -0.2746(2) -0.1805(2) 0.0442(9) Uani 1 d . . H43A H 0.6892(3) -0.2858(2) -0.1446(2) 0.080 Uiso 1 d R . C44 C 0.8053(3) -0.3302(2) -0.1979(2) 0.0463(9) Uani 1 d . . H44A H 0.8229(3) -0.3798(2) -0.1740(2) 0.080 Uiso 1 d R . C45 C 0.8576(3) -0.3129(2) -0.2504(2) 0.0426(8) Uani 1 d . . H45A H 0.9106(3) -0.3515(2) -0.2639(2) 0.080 Uiso 1 d R . C46 C 0.8339(3) -0.2403(2) -0.2839(2) 0.0371(8) Uani 1 d . . H46A H 0.8720(3) -0.2302(2) -0.3201(2) 0.080 Uiso 1 d 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 0.02418(5) 0.02959(6) 0.02225(5) -0.00364(8) 0.00327(4) 0.00037(8) Cl1 0.0417(4) 0.0532(5) 0.0254(4) -0.0007(3) 0.0096(3) 0.0012(4) Cl2 0.0338(4) 0.0446(5) 0.0462(5) -0.0028(4) 0.0106(4) 0.0097(4) N1 0.0244(12) 0.0312(14) 0.0261(13) -0.0009(11) 0.0011(10) 0.0026(11) N2 0.0274(11) 0.0269(14) 0.0258(11) 0.0010(12) 0.0018(9) 0.0014(12) B1 0.032(2) 0.034(2) 0.027(2) 0.0027(15) 0.0078(14) 0.000(2) C1 0.047(2) 0.044(2) 0.033(2) -0.020(2) 0.016(2) -0.012(2) C2 0.049(2) 0.046(2) 0.028(2) -0.0110(15) -0.0049(15) 0.004(2) C3 0.036(2) 0.058(2) 0.043(2) -0.022(2) 0.012(2) -0.012(2) C4 0.081(3) 0.043(2) 0.033(2) -0.006(2) 0.012(2) -0.023(2) C5 0.043(2) 0.037(2) 0.057(2) -0.021(2) -0.006(2) 0.005(2) C6 0.104(4) 0.090(4) 0.075(3) -0.047(3) 0.061(3) -0.043(3) C7 0.112(4) 0.069(4) 0.049(2) -0.007(2) -0.038(2) 0.011(3) C8 0.040(2) 0.129(5) 0.115(4) -0.069(4) 0.030(3) -0.036(3) C9 0.183(6) 0.065(3) 0.052(2) -0.004(2) 0.015(3) -0.064(4) C10 0.086(3) 0.064(3) 0.122(4) -0.056(3) -0.030(3) 0.030(3) C11 0.032(2) 0.038(2) 0.039(2) 0.0063(15) 0.0022(14) 0.0081(15) C12 0.038(2) 0.040(2) 0.033(2) 0.0070(15) -0.0003(14) 0.008(2) C13 0.040(2) 0.027(2) 0.0222(14) -0.0027(12) 0.0002(13) 0.0006(14) C14 0.032(2) 0.025(2) 0.0275(15) 0.0019(12) 0.0012(12) 0.0028(13) C15 0.0253(14) 0.024(2) 0.0263(14) -0.0012(12) 0.0001(12) 0.0030(12) C16 0.048(2) 0.035(2) 0.032(2) 0.005(2) 0.0024(13) -0.002(2) C17 0.034(2) 0.030(2) 0.031(2) 0.0080(13) 0.0020(13) 0.0059(14) C18 0.038(2) 0.032(2) 0.033(2) 0.0045(14) 0.0012(14) 0.0040(14) C19 0.031(2) 0.031(2) 0.038(2) 0.0023(13) 0.0014(13) 0.0085(13) C20 0.028(2) 0.032(2) 0.034(2) 0.0008(13) 0.0031(13) 0.0000(13) C21 0.0268(14) 0.0232(14) 0.0256(14) -0.0006(12) 0.0023(12) 0.0017(12) C22 0.032(2) 0.057(2) 0.060(2) 0.012(2) 0.001(2) 0.013(2) C23 0.042(2) 0.030(2) 0.033(2) -0.0018(14) 0.0091(14) -0.0035(15) C24 0.047(2) 0.056(2) 0.044(2) -0.004(2) 0.020(2) -0.005(2) C25 0.060(2) 0.059(3) 0.059(2) -0.010(2) 0.034(2) -0.009(2) C26 0.090(3) 0.049(2) 0.053(2) -0.009(2) 0.041(2) -0.013(2) C27 0.089(3) 0.047(2) 0.036(2) 0.002(2) 0.021(2) -0.009(2) C28 0.052(2) 0.037(2) 0.032(2) -0.0009(15) 0.009(2) -0.009(2) C29 0.027(2) 0.035(2) 0.027(2) 0.0010(13) 0.0045(12) 0.0021(14) C30 0.035(2) 0.038(2) 0.032(2) -0.0014(14) 0.0035(14) 0.0034(15) C31 0.038(2) 0.054(2) 0.030(2) -0.002(2) -0.0006(14) 0.008(2) C32 0.030(2) 0.048(2) 0.045(2) -0.009(2) -0.0008(15) -0.0037(15) C33 0.034(2) 0.039(2) 0.048(2) 0.001(2) 0.0035(15) -0.0075(15) C34 0.032(2) 0.043(2) 0.032(2) 0.0026(15) 0.0021(13) -0.0065(15) C35 0.031(2) 0.037(2) 0.0226(14) -0.0006(13) 0.0042(12) 0.0006(14) C36 0.0354(15) 0.036(2) 0.0342(15) -0.001(2) 0.0054(12) -0.002(2) C37 0.035(2) 0.045(2) 0.039(2) -0.006(2) -0.0003(13) -0.006(2) C38 0.030(2) 0.051(2) 0.045(2) 0.001(2) -0.0039(15) 0.002(2) C39 0.040(2) 0.041(2) 0.061(2) -0.003(2) -0.006(2) 0.010(2) C40 0.036(2) 0.037(2) 0.051(2) -0.009(2) 0.000(2) 0.000(2) C41 0.0226(15) 0.038(2) 0.034(2) -0.0080(14) -0.0005(13) -0.0073(13) C42 0.028(2) 0.042(2) 0.048(2) 0.009(2) 0.0077(15) -0.0025(15) C43 0.031(2) 0.051(2) 0.050(2) 0.013(2) 0.003(2) -0.010(2) C44 0.031(2) 0.039(2) 0.063(2) 0.006(2) -0.010(2) -0.0090(15) C45 0.027(2) 0.036(2) 0.061(2) -0.013(2) -0.005(2) -0.0013(15) C46 0.027(2) 0.041(2) 0.041(2) -0.010(2) -0.0021(14) -0.0030(14) _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 N1 2.134(2) . ? W1 N2 2.143(2) . ? W1 C2 2.302(3) . ? W1 C1 2.306(3) . ? W1 C3 2.334(3) . ? W1 Cl1 2.3551(8) . ? W1 Cl2 2.3658(8) . ? W1 C5 2.371(3) . ? W1 C4 2.406(4) . ? N1 C11 1.369(4) . ? N1 C15 1.371(3) . ? N2 C17 1.366(3) . ? N2 C21 1.369(4) . ? B1 C41 1.637(5) . ? B1 C35 1.647(4) . ? B1 C29 1.654(5) . ? B1 C23 1.663(4) . ? C1 C5 1.409(5) . ? C1 C2 1.413(5) . ? C1 C6 1.505(5) . ? C2 C3 1.400(5) . ? C2 C7 1.504(5) . ? C3 C4 1.395(5) . ? C3 C8 1.509(5) . ? C4 C5 1.425(5) . ? C4 C9 1.492(5) . ? C5 C10 1.476(5) . ? C11 C12 1.365(4) . ? C12 C13 1.384(4) . ? C13 C14 1.385(4) . ? C13 C16 1.495(4) . ? C14 C15 1.379(4) . ? C15 C21 1.460(4) . ? C17 C18 1.369(4) . ? C18 C19 1.388(4) . ? C19 C20 1.390(4) . ? C19 C22 1.502(4) . ? C20 C21 1.382(4) . ? C23 C28 1.392(4) . ? C23 C24 1.398(5) . ? C24 C25 1.391(5) . ? C25 C26 1.367(6) . ? C26 C27 1.357(6) . ? C27 C28 1.410(5) . ? C29 C30 1.396(4) . ? C29 C34 1.400(4) . ? C30 C31 1.399(5) . ? C31 C32 1.384(5) . ? C32 C33 1.392(5) . ? C33 C34 1.381(4) . ? C35 C40 1.386(4) . ? C35 C36 1.393(4) . ? C36 C37 1.386(4) . ? C37 C38 1.371(5) . ? C38 C39 1.385(5) . ? C39 C40 1.381(5) . ? C41 C46 1.391(4) . ? C41 C42 1.410(4) . ? C42 C43 1.383(5) . ? C43 C44 1.378(5) . ? C44 C45 1.381(5) . ? C45 C46 1.386(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W1 N2 73.61(9) . . ? N1 W1 C2 91.97(11) . . ? N2 W1 C2 131.09(11) . . ? N1 W1 C1 84.14(11) . . ? N2 W1 C1 95.59(11) . . ? C2 W1 C1 35.71(12) . . ? N1 W1 C3 126.20(11) . . ? N2 W1 C3 140.28(12) . . ? C2 W1 C3 35.14(12) . . ? C1 W1 C3 58.54(12) . . ? N1 W1 Cl1 135.68(7) . . ? N2 W1 Cl1 85.00(6) . . ? C2 W1 Cl1 130.04(10) . . ? C1 W1 Cl1 137.25(10) . . ? C3 W1 Cl1 94.94(9) . . ? N1 W1 Cl2 83.87(7) . . ? N2 W1 Cl2 132.77(7) . . ? C2 W1 Cl2 89.70(9) . . ? C1 W1 Cl2 123.20(10) . . ? C3 W1 Cl2 86.32(9) . . ? Cl1 W1 Cl2 83.10(3) . . ? N1 W1 C5 111.77(12) . . ? N2 W1 C5 83.30(11) . . ? C2 W1 C5 58.66(12) . . ? C1 W1 C5 35.03(13) . . ? C3 W1 C5 58.00(12) . . ? Cl1 W1 C5 103.44(11) . . ? Cl2 W1 C5 143.93(9) . . ? N1 W1 C4 141.94(11) . . ? N2 W1 C4 107.61(13) . . ? C2 W1 C4 57.74(13) . . ? C1 W1 C4 57.80(12) . . ? C3 W1 C4 34.20(13) . . ? Cl1 W1 C4 81.20(8) . . ? Cl2 W1 C4 115.36(11) . . ? C5 W1 C4 34.71(13) . . ? C11 N1 C15 116.1(3) . . ? C11 N1 W1 124.5(2) . . ? C15 N1 W1 119.2(2) . . ? C17 N2 C21 116.4(2) . . ? C17 N2 W1 124.9(2) . . ? C21 N2 W1 118.3(2) . . ? C41 B1 C35 109.2(3) . . ? C41 B1 C29 110.2(2) . . ? C35 B1 C29 110.2(3) . . ? C41 B1 C23 111.7(3) . . ? C35 B1 C23 108.4(2) . . ? C29 B1 C23 107.1(2) . . ? C5 C1 C2 108.5(3) . . ? C5 C1 C6 124.0(4) . . ? C2 C1 C6 127.0(4) . . ? C5 C1 W1 75.0(2) . . ? C2 C1 W1 72.0(2) . . ? C6 C1 W1 125.3(2) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 C7 125.6(4) . . ? C1 C2 C7 126.1(4) . . ? C3 C2 W1 73.7(2) . . ? C1 C2 W1 72.3(2) . . ? C7 C2 W1 127.5(3) . . ? C4 C3 C2 108.9(3) . . ? C4 C3 C8 124.8(4) . . ? C2 C3 C8 125.9(4) . . ? C4 C3 W1 75.7(2) . . ? C2 C3 W1 71.2(2) . . ? C8 C3 W1 124.3(2) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 C9 126.4(4) . . ? C5 C4 C9 125.4(4) . . ? C3 C4 W1 70.1(2) . . ? C5 C4 W1 71.3(2) . . ? C9 C4 W1 128.2(3) . . ? C1 C5 C4 107.0(3) . . ? C1 C5 C10 127.4(4) . . ? C4 C5 C10 125.0(4) . . ? C1 C5 W1 70.0(2) . . ? C4 C5 W1 74.0(2) . . ? C10 C5 W1 127.5(3) . . ? C12 C11 N1 122.9(3) . . ? C11 C12 C13 120.9(3) . . ? C12 C13 C14 117.0(3) . . ? C12 C13 C16 121.6(3) . . ? C14 C13 C16 121.5(3) . . ? C15 C14 C13 120.6(3) . . ? N1 C15 C14 122.5(3) . . ? N1 C15 C21 113.2(3) . . ? C14 C15 C21 124.3(3) . . ? N2 C17 C18 123.1(3) . . ? C17 C18 C19 120.5(3) . . ? C18 C19 C20 117.2(3) . . ? C18 C19 C22 120.9(3) . . ? C20 C19 C22 121.9(3) . . ? C21 C20 C19 120.3(3) . . ? N2 C21 C20 122.4(3) . . ? N2 C21 C15 114.2(2) . . ? C20 C21 C15 123.4(3) . . ? C28 C23 C24 115.6(3) . . ? C28 C23 B1 124.1(3) . . ? C24 C23 B1 120.3(3) . . ? C25 C24 C23 122.4(4) . . ? C26 C25 C24 120.1(4) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C28 120.1(4) . . ? C23 C28 C27 121.9(4) . . ? C30 C29 C34 114.3(3) . . ? C30 C29 B1 124.6(3) . . ? C34 C29 B1 121.0(3) . . ? C29 C30 C31 122.9(3) . . ? C32 C31 C30 120.6(3) . . ? C31 C32 C33 118.0(3) . . ? C34 C33 C32 120.1(3) . . ? C33 C34 C29 124.0(3) . . ? C40 C35 C36 115.1(3) . . ? C40 C35 B1 123.5(3) . . ? C36 C35 B1 121.3(3) . . ? C37 C36 C35 122.6(4) . . ? C38 C37 C36 120.8(3) . . ? C37 C38 C39 118.0(3) . . ? C40 C39 C38 120.4(3) . . ? C39 C40 C35 123.1(3) . . ? C46 C41 C42 114.0(3) . . ? C46 C41 B1 126.4(3) . . ? C42 C41 B1 119.6(3) . . ? C43 C42 C41 123.6(3) . . ? C44 C43 C42 119.9(3) . . ? C43 C44 C45 118.6(3) . . ? C44 C45 C46 120.5(3) . . ? C45 C46 C41 123.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 W1 N1 C11 175.7(3) . . . . ? C2 W1 N1 C11 -51.8(3) . . . . ? C1 W1 N1 C11 -86.7(3) . . . . ? C3 W1 N1 C11 -43.2(3) . . . . ? Cl1 W1 N1 C11 111.3(2) . . . . ? Cl2 W1 N1 C11 37.7(2) . . . . ? C5 W1 N1 C11 -108.7(3) . . . . ? C4 W1 N1 C11 -86.5(3) . . . . ? N2 W1 N1 C15 -10.4(2) . . . . ? C2 W1 N1 C15 122.1(2) . . . . ? C1 W1 N1 C15 87.2(2) . . . . ? C3 W1 N1 C15 130.7(2) . . . . ? Cl1 W1 N1 C15 -74.8(2) . . . . ? Cl2 W1 N1 C15 -148.4(2) . . . . ? C5 W1 N1 C15 65.2(2) . . . . ? C4 W1 N1 C15 87.4(3) . . . . ? N1 W1 N2 C17 -176.4(2) . . . . ? C2 W1 N2 C17 105.7(2) . . . . ? C1 W1 N2 C17 101.4(2) . . . . ? C3 W1 N2 C17 56.1(3) . . . . ? Cl1 W1 N2 C17 -35.6(2) . . . . ? Cl2 W1 N2 C17 -111.5(2) . . . . ? C5 W1 N2 C17 68.5(2) . . . . ? C4 W1 N2 C17 43.5(2) . . . . ? N1 W1 N2 C21 10.6(2) . . . . ? C2 W1 N2 C21 -67.4(3) . . . . ? C1 W1 N2 C21 -71.6(2) . . . . ? C3 W1 N2 C21 -116.9(2) . . . . ? Cl1 W1 N2 C21 151.3(2) . . . . ? Cl2 W1 N2 C21 75.5(2) . . . . ? C5 W1 N2 C21 -104.5(2) . . . . ? C4 W1 N2 C21 -129.6(2) . . . . ? N1 W1 C1 C5 -142.7(2) . . . . ? N2 W1 C1 C5 -69.9(2) . . . . ? C2 W1 C1 C5 115.6(3) . . . . ? C3 W1 C1 C5 77.9(2) . . . . ? Cl1 W1 C1 C5 18.8(3) . . . . ? Cl2 W1 C1 C5 138.5(2) . . . . ? C5 W1 C1 C5 0.0 . . . . ? C4 W1 C1 C5 37.4(2) . . . . ? N1 W1 C1 C2 101.7(2) . . . . ? N2 W1 C1 C2 174.5(2) . . . . ? C2 W1 C1 C2 0.0 . . . . ? C3 W1 C1 C2 -37.7(2) . . . . ? Cl1 W1 C1 C2 -96.8(2) . . . . ? Cl2 W1 C1 C2 22.9(2) . . . . ? C5 W1 C1 C2 -115.6(3) . . . . ? C4 W1 C1 C2 -78.2(2) . . . . ? N1 W1 C1 C6 -21.4(4) . . . . ? N2 W1 C1 C6 51.4(4) . . . . ? C2 W1 C1 C6 -123.1(5) . . . . ? C3 W1 C1 C6 -160.8(4) . . . . ? Cl1 W1 C1 C6 140.1(3) . . . . ? Cl2 W1 C1 C6 -100.1(4) . . . . ? C5 W1 C1 C6 121.3(5) . . . . ? C4 W1 C1 C6 158.8(4) . . . . ? C5 C1 C2 C3 -0.9(4) . . . . ? C6 C1 C2 C3 -173.2(3) . . . . ? W1 C1 C2 C3 65.8(2) . . . . ? C5 C1 C2 C7 169.3(3) . . . . ? C6 C1 C2 C7 -2.9(6) . . . . ? W1 C1 C2 C7 -123.9(4) . . . . ? C5 C1 C2 W1 -66.7(2) . . . . ? C6 C1 C2 W1 121.0(3) . . . . ? W1 C1 C2 W1 0.0 . . . . ? N1 W1 C2 C3 167.9(2) . . . . ? N2 W1 C2 C3 -122.3(2) . . . . ? C1 W1 C2 C3 -115.0(3) . . . . ? C3 W1 C2 C3 0.0 . . . . ? Cl1 W1 C2 C3 3.3(3) . . . . ? Cl2 W1 C2 C3 84.0(2) . . . . ? C5 W1 C2 C3 -77.7(2) . . . . ? C4 W1 C2 C3 -36.6(2) . . . . ? N1 W1 C2 C1 -77.1(2) . . . . ? N2 W1 C2 C1 -7.3(3) . . . . ? C1 W1 C2 C1 0.0 . . . . ? C3 W1 C2 C1 115.0(3) . . . . ? Cl1 W1 C2 C1 118.3(2) . . . . ? Cl2 W1 C2 C1 -161.0(2) . . . . ? C5 W1 C2 C1 37.3(2) . . . . ? C4 W1 C2 C1 78.4(2) . . . . ? N1 W1 C2 C7 45.2(4) . . . . ? N2 W1 C2 C7 115.1(4) . . . . ? C1 W1 C2 C7 122.3(5) . . . . ? C3 W1 C2 C7 -122.6(5) . . . . ? Cl1 W1 C2 C7 -119.3(4) . . . . ? Cl2 W1 C2 C7 -38.6(4) . . . . ? C5 W1 C2 C7 159.7(4) . . . . ? C4 W1 C2 C7 -159.3(4) . . . . ? C1 C2 C3 C4 2.0(4) . . . . ? C7 C2 C3 C4 -168.3(3) . . . . ? W1 C2 C3 C4 66.9(2) . . . . ? C1 C2 C3 C8 175.9(3) . . . . ? C7 C2 C3 C8 5.6(6) . . . . ? W1 C2 C3 C8 -119.2(4) . . . . ? C1 C2 C3 W1 -64.9(2) . . . . ? C7 C2 C3 W1 124.8(4) . . . . ? W1 C2 C3 W1 0.0 . . . . ? N1 W1 C3 C4 -131.2(2) . . . . ? N2 W1 C3 C4 -21.7(3) . . . . ? C2 W1 C3 C4 -116.1(3) . . . . ? C1 W1 C3 C4 -77.8(2) . . . . ? Cl1 W1 C3 C4 66.4(2) . . . . ? Cl2 W1 C3 C4 149.1(2) . . . . ? C5 W1 C3 C4 -36.4(2) . . . . ? C4 W1 C3 C4 0.0 . . . . ? N1 W1 C3 C2 -15.1(3) . . . . ? N2 W1 C3 C2 94.4(3) . . . . ? C2 W1 C3 C2 0.0 . . . . ? C1 W1 C3 C2 38.3(2) . . . . ? Cl1 W1 C3 C2 -177.5(2) . . . . ? Cl2 W1 C3 C2 -94.7(2) . . . . ? C5 W1 C3 C2 79.8(2) . . . . ? C4 W1 C3 C2 116.1(3) . . . . ? N1 W1 C3 C8 106.1(4) . . . . ? N2 W1 C3 C8 -144.4(3) . . . . ? C2 W1 C3 C8 121.2(5) . . . . ? C1 W1 C3 C8 159.5(4) . . . . ? Cl1 W1 C3 C8 -56.3(4) . . . . ? Cl2 W1 C3 C8 26.4(4) . . . . ? C5 W1 C3 C8 -159.1(4) . . . . ? C4 W1 C3 C8 -122.7(5) . . . . ? C2 C3 C4 C5 -2.4(4) . . . . ? C8 C3 C4 C5 -176.3(3) . . . . ? W1 C3 C4 C5 61.6(2) . . . . ? C2 C3 C4 C9 172.7(3) . . . . ? C8 C3 C4 C9 -1.3(6) . . . . ? W1 C3 C4 C9 -123.4(4) . . . . ? C2 C3 C4 W1 -64.0(2) . . . . ? C8 C3 C4 W1 122.1(3) . . . . ? W1 C3 C4 W1 0.0 . . . . ? N1 W1 C4 C3 79.9(3) . . . . ? N2 W1 C4 C3 165.6(2) . . . . ? C2 W1 C4 C3 37.7(2) . . . . ? C1 W1 C4 C3 80.2(2) . . . . ? C3 W1 C4 C3 0.0 . . . . ? Cl1 W1 C4 C3 -112.5(2) . . . . ? Cl2 W1 C4 C3 -34.5(2) . . . . ? C5 W1 C4 C3 117.9(3) . . . . ? N1 W1 C4 C5 -38.0(3) . . . . ? N2 W1 C4 C5 47.7(2) . . . . ? C2 W1 C4 C5 -80.3(2) . . . . ? C1 W1 C4 C5 -37.8(2) . . . . ? C3 W1 C4 C5 -117.9(3) . . . . ? Cl1 W1 C4 C5 129.5(2) . . . . ? Cl2 W1 C4 C5 -152.5(2) . . . . ? C5 W1 C4 C5 0.0 . . . . ? N1 W1 C4 C9 -158.9(4) . . . . ? N2 W1 C4 C9 -73.2(5) . . . . ? C2 W1 C4 C9 158.9(5) . . . . ? C1 W1 C4 C9 -158.6(5) . . . . ? C3 W1 C4 C9 121.2(5) . . . . ? Cl1 W1 C4 C9 8.7(4) . . . . ? Cl2 W1 C4 C9 86.7(4) . . . . ? C5 W1 C4 C9 -120.8(5) . . . . ? C2 C1 C5 C4 -0.5(4) . . . . ? C6 C1 C5 C4 172.0(3) . . . . ? W1 C1 C5 C4 -65.2(2) . . . . ? C2 C1 C5 C10 -172.8(3) . . . . ? C6 C1 C5 C10 -0.3(6) . . . . ? W1 C1 C5 C10 122.5(4) . . . . ? C2 C1 C5 W1 64.7(2) . . . . ? C6 C1 C5 W1 -122.7(3) . . . . ? W1 C1 C5 W1 0.0 . . . . ? C3 C4 C5 C1 1.7(4) . . . . ? C9 C4 C5 C1 -173.4(3) . . . . ? W1 C4 C5 C1 62.5(2) . . . . ? C3 C4 C5 C10 174.3(3) . . . . ? C9 C4 C5 C10 -0.8(6) . . . . ? W1 C4 C5 C10 -124.9(4) . . . . ? C3 C4 C5 W1 -60.8(2) . . . . ? C9 C4 C5 W1 124.1(4) . . . . ? W1 C4 C5 W1 0.0 . . . . ? N1 W1 C5 C1 40.4(2) . . . . ? N2 W1 C5 C1 109.8(2) . . . . ? C2 W1 C5 C1 -38.0(2) . . . . ? C1 W1 C5 C1 0.0 . . . . ? C3 W1 C5 C1 -79.6(2) . . . . ? Cl1 W1 C5 C1 -167.0(2) . . . . ? Cl2 W1 C5 C1 -70.2(3) . . . . ? C4 W1 C5 C1 -115.4(3) . . . . ? N1 W1 C5 C4 155.9(2) . . . . ? N2 W1 C5 C4 -134.8(2) . . . . ? C2 W1 C5 C4 77.4(2) . . . . ? C1 W1 C5 C4 115.4(3) . . . . ? C3 W1 C5 C4 35.8(2) . . . . ? Cl1 W1 C5 C4 -51.6(2) . . . . ? Cl2 W1 C5 C4 45.2(3) . . . . ? C4 W1 C5 C4 0.0 . . . . ? N1 W1 C5 C10 -81.9(4) . . . . ? N2 W1 C5 C10 -12.6(4) . . . . ? C2 W1 C5 C10 -160.4(5) . . . . ? C1 W1 C5 C10 -122.4(5) . . . . ? C3 W1 C5 C10 158.0(5) . . . . ? Cl1 W1 C5 C10 70.6(4) . . . . ? Cl2 W1 C5 C10 167.4(4) . . . . ? C4 W1 C5 C10 122.2(5) . . . . ? C15 N1 C11 C12 -1.2(4) . . . . ? W1 N1 C11 C12 172.9(2) . . . . ? N1 C11 C12 C13 -0.1(5) . . . . ? C11 C12 C13 C14 0.8(5) . . . . ? C11 C12 C13 C16 179.3(3) . . . . ? C12 C13 C14 C15 -0.3(4) . . . . ? C16 C13 C14 C15 -178.8(3) . . . . ? C11 N1 C15 C14 1.7(4) . . . . ? W1 N1 C15 C14 -172.7(2) . . . . ? C11 N1 C15 C21 -176.8(2) . . . . ? W1 N1 C15 C21 8.8(3) . . . . ? C13 C14 C15 N1 -1.0(4) . . . . ? C13 C14 C15 C21 177.4(3) . . . . ? C21 N2 C17 C18 0.1(4) . . . . ? W1 N2 C17 C18 -173.0(2) . . . . ? N2 C17 C18 C19 1.5(5) . . . . ? C17 C18 C19 C20 -1.4(5) . . . . ? C17 C18 C19 C22 180.0(3) . . . . ? C18 C19 C20 C21 -0.2(4) . . . . ? C22 C19 C20 C21 178.4(3) . . . . ? C17 N2 C21 C20 -1.8(4) . . . . ? W1 N2 C21 C20 171.8(2) . . . . ? C17 N2 C21 C15 176.8(2) . . . . ? W1 N2 C21 C15 -9.6(3) . . . . ? C19 C20 C21 N2 1.8(4) . . . . ? C19 C20 C21 C15 -176.6(3) . . . . ? N1 C15 C21 N2 0.6(4) . . . . ? C14 C15 C21 N2 -178.0(3) . . . . ? N1 C15 C21 C20 179.2(3) . . . . ? C14 C15 C21 C20 0.6(5) . . . . ? C41 B1 C23 C28 115.4(3) . . . . ? C35 B1 C23 C28 -5.0(4) . . . . ? C29 B1 C23 C28 -123.9(3) . . . . ? C41 B1 C23 C24 -67.0(4) . . . . ? C35 B1 C23 C24 172.6(3) . . . . ? C29 B1 C23 C24 53.7(4) . . . . ? C28 C23 C24 C25 -2.5(5) . . . . ? B1 C23 C24 C25 179.7(3) . . . . ? C23 C24 C25 C26 1.8(6) . . . . ? C24 C25 C26 C27 -0.7(6) . . . . ? C25 C26 C27 C28 0.4(6) . . . . ? C24 C23 C28 C27 2.2(5) . . . . ? B1 C23 C28 C27 179.9(3) . . . . ? C26 C27 C28 C23 -1.2(6) . . . . ? C41 B1 C29 C30 -21.8(4) . . . . ? C35 B1 C29 C30 98.8(3) . . . . ? C23 B1 C29 C30 -143.5(3) . . . . ? C41 B1 C29 C34 161.3(3) . . . . ? C35 B1 C29 C34 -78.2(3) . . . . ? C23 B1 C29 C34 39.5(4) . . . . ? C34 C29 C30 C31 0.4(5) . . . . ? B1 C29 C30 C31 -176.7(3) . . . . ? C29 C30 C31 C32 1.2(5) . . . . ? C30 C31 C32 C33 -2.0(5) . . . . ? C31 C32 C33 C34 1.2(5) . . . . ? C32 C33 C34 C29 0.4(5) . . . . ? C30 C29 C34 C33 -1.2(5) . . . . ? B1 C29 C34 C33 176.0(3) . . . . ? C41 B1 C35 C40 144.5(3) . . . . ? C29 B1 C35 C40 23.3(4) . . . . ? C23 B1 C35 C40 -93.6(3) . . . . ? C41 B1 C35 C36 -38.7(4) . . . . ? C29 B1 C35 C36 -159.8(3) . . . . ? C23 B1 C35 C36 83.3(3) . . . . ? C40 C35 C36 C37 2.3(4) . . . . ? B1 C35 C36 C37 -174.8(3) . . . . ? C35 C36 C37 C38 -2.0(5) . . . . ? C36 C37 C38 C39 0.7(5) . . . . ? C37 C38 C39 C40 0.2(6) . . . . ? C38 C39 C40 C35 0.2(6) . . . . ? C36 C35 C40 C39 -1.4(5) . . . . ? B1 C35 C40 C39 175.6(3) . . . . ? C35 B1 C41 C46 131.5(3) . . . . ? C29 B1 C41 C46 -107.3(3) . . . . ? C23 B1 C41 C46 11.6(4) . . . . ? C35 B1 C41 C42 -49.1(3) . . . . ? C29 B1 C41 C42 72.0(3) . . . . ? C23 B1 C41 C42 -169.1(3) . . . . ? C46 C41 C42 C43 1.5(4) . . . . ? B1 C41 C42 C43 -177.9(3) . . . . ? C41 C42 C43 C44 -0.4(5) . . . . ? C42 C43 C44 C45 -1.0(5) . . . . ? C43 C44 C45 C46 1.3(5) . . . . ? C44 C45 C46 C41 -0.1(5) . . . . ? C42 C41 C46 C45 -1.2(4) . . . . ? B1 C41 C46 C45 178.2(3) . . . . ? _refine_diff_density_max 0.336 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.064 # CIF-file generated for Complex 4-Me+BPh4- data_4_Me+BPh4- _audit_creation_method SHELXL #========================================================== _publ_contact_author_name 'Peter Burger' _publ_contact_author_address ; 'Anorg.-Chem Inst., University of Zuerich, Winterthurerstr. 190, 8057 Zuerich' ; _publ_contact_author_email 'chburger@aci.unizh.ch' _publ_contact_author_fax '+41 1 635 6802' _publ_contact_author_phone '+41 1 635 4692' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' loop_ _publ_author_name 'Peter Burger' 'Christian Cremer' _chemical_name_systematic ; ? ; _chemical_formula_structural 'Cp*W(Me-bipy)(CO)Cl2+ BPh4- * C2H4Cl2' _chemical_formula_sum 'C49 H51 B Cl4 N2 O W' _chemical_formula_weight 1020.38 _chemical_melting_point n/a _chemical_compound_source synthesis 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.428(2) _cell_length_b 9.2642(6) _cell_length_c 23.646(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.132(9) _cell_angle_gamma 90.00 _cell_volume 4448.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5000 _exptl_crystal_description 'rect. parallelepiped' _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method n/a _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 2.876 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.64 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'STOE IPDS' _diffrn_measurement_method 'Image Plate' _diffrn_reflns_number 8462 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.89 _reflns_number_total 8462 _reflns_number_observed 6344 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE IPDS PROGRAM PACKAGE' _computing_cell_refinement 'STOE IPDS PROGRAM PACKAGE' _computing_data_reduction 'STOE IPDS PROGRAM PACKAGE' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1988)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1998)' _computing_publication_material 'SHELXL-93, Platon (Spek, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Atom Cl3 in the C2H4Cl2 solvent molecule is disordered, refined with two split positions and occupation factors of 0.45 and 0.55; the CO ligand (atoms C23a,b and O1a,b) and Cl ligand Cl1a,b are positionally disordered and were refined with two split positions with an occupation factor of 0.45 and 0.55). Cl atom Cl2a,b is also disordered and was refined with two split positions (occ. factor of 0.45 and .55). Atoms C23 and O1 were refined isotropically with identical displacement parameters (EADP card) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^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 'riding model' _refine_ls_extinction_method n/a _refine_ls_extinction_coef n/a _refine_ls_number_reflns 8462 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_obs 0.0280 _refine_ls_wR_factor_all 0.0770 _refine_ls_wR_factor_obs 0.0668 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max -0.657 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.608957(8) 0.08924(2) 0.701535(8) 0.02280(6) Uani 1 d . . B1 B 0.7372(3) 0.3206(6) 0.4308(2) 0.0286(12) Uani 1 d . . N1 N 0.5591(2) 0.0054(5) 0.7564(2) 0.0256(8) Uani 1 d . . N2 N 0.6665(2) 0.1657(5) 0.7964(2) 0.0272(9) Uani 1 d . . O1A O 0.5614(4) -0.1462(10) 0.5953(4) 0.054(2) Uiso 0.564(6) d P . O1B O 0.7236(4) 0.1184(10) 0.6691(4) 0.054(2) Uiso 0.564(6) d P . Cl1A Cl 0.5734(2) -0.1103(4) 0.6305(2) 0.0439(11) Uani 0.436(6) d P . Cl1B Cl 0.70824(13) 0.0978(3) 0.68542(10) 0.0284(7) Uani 0.564(6) d P . Cl2A Cl 0.6844(3) -0.0992(7) 0.7585(2) 0.0441(12) Uani 0.436(6) d P . Cl2B Cl 0.6596(2) -0.1456(4) 0.7459(2) 0.0303(7) Uani 0.564(6) d P . Cl3A Cl 0.9795(6) 0.2522(13) 0.3961(9) 0.146(5) Uani 0.45(3) d P . Cl3B Cl 0.9725(5) 0.2268(18) 0.4213(8) 0.153(6) Uani 0.55(3) d P . Cl4 Cl 0.9150(2) 0.0224(3) 0.29061(14) 0.1181(10) Uani 1 d . . C1 C 0.5175(3) 0.2489(8) 0.6784(3) 0.059(2) Uani 1 d . . C2 C 0.5109(3) 0.1735(6) 0.6240(3) 0.0451(14) Uani 1 d . . C3 C 0.5642(3) 0.2189(6) 0.6103(2) 0.0388(13) Uani 1 d . . C4 C 0.6026(3) 0.3190(5) 0.6573(2) 0.0362(12) Uani 1 d . . C5 C 0.5729(3) 0.3380(6) 0.6985(2) 0.0379(12) Uiso 1 d . . C6 C 0.4667(5) 0.2501(11) 0.7036(5) 0.115(4) Uani 1 d . . H6A H 0.4362(5) 0.3276(11) 0.6846(5) 0.080 Uiso 1 d R . H6B H 0.4433(5) 0.1600(11) 0.6945(5) 0.080 Uiso 1 d R . H6C H 0.4879(5) 0.2643(11) 0.7480(5) 0.080 Uiso 1 d R . C7 C 0.4506(3) 0.0935(9) 0.5800(4) 0.085(3) Uani 1 d . . H7A H 0.4184(3) 0.1610(9) 0.5535(4) 0.080 Uiso 1 d R . H7B H 0.4626(3) 0.0288(9) 0.5549(4) 0.080 Uiso 1 d R . H7C H 0.4325(3) 0.0393(9) 0.6036(4) 0.080 Uiso 1 d R . C8 C 0.5716(4) 0.1890(8) 0.5510(3) 0.070(2) Uani 1 d . . H8A H 0.5478(4) 0.2601(8) 0.5201(3) 0.080 Uiso 1 d R . H8B H 0.6174(4) 0.1926(8) 0.5595(3) 0.080 Uiso 1 d R . H8C H 0.5544(4) 0.0948(8) 0.5358(3) 0.080 Uiso 1 d R . C9 C 0.6543(4) 0.4179(9) 0.6549(4) 0.075(2) Uani 1 d . . H9A H 0.6342(4) 0.5048(9) 0.6330(4) 0.080 Uiso 1 d R . H9B H 0.6854(4) 0.4415(9) 0.6965(4) 0.080 Uiso 1 d R . H9C H 0.6766(4) 0.3700(9) 0.6334(4) 0.080 Uiso 1 d R . C10 C 0.5908(5) 0.4454(8) 0.7491(3) 0.094(3) Uani 1 d . . H10A H 0.5678(5) 0.5339(8) 0.7324(3) 0.080 Uiso 1 d R . H10B H 0.5788(5) 0.4101(8) 0.7810(3) 0.080 Uiso 1 d R . H10C H 0.6375(5) 0.4625(8) 0.7667(3) 0.080 Uiso 1 d R . C11 C 0.5086(2) -0.0879(6) 0.7352(2) 0.0314(10) Uani 1 d . . H11A H 0.4902(2) -0.1149(6) 0.6919(2) 0.080 Uiso 1 d R . C12 C 0.4821(2) -0.1454(6) 0.7728(2) 0.0365(12) Uani 1 d . . H12A H 0.4452(2) -0.2098(6) 0.7554(2) 0.080 Uiso 1 d R . C13 C 0.5083(2) -0.1119(7) 0.8358(2) 0.0378(13) Uani 1 d . . C14 C 0.5611(2) -0.0178(6) 0.8577(2) 0.0350(12) Uani 1 d . . H14A H 0.5809(2) 0.0081(6) 0.9011(2) 0.080 Uiso 1 d R . C15 C 0.5859(2) 0.0399(5) 0.8183(2) 0.0236(10) Uani 1 d . . C16 C 0.4813(3) -0.1716(8) 0.8789(3) 0.053(2) Uani 1 d . . H16A H 0.5062(3) -0.1351(8) 0.9203(3) 0.080 Uiso 1 d R . H16B H 0.4360(3) -0.1440(8) 0.8646(3) 0.080 Uiso 1 d R . H16C H 0.4845(3) -0.2750(8) 0.8792(3) 0.080 Uiso 1 d R . C17 C 0.7222(2) 0.2439(7) 0.8142(2) 0.0376(12) Uani 1 d . . H17A H 0.7393(2) 0.2635(7) 0.7840(2) 0.080 Uiso 1 d R . C18 C 0.7552(2) 0.2965(6) 0.8739(2) 0.0372(12) Uani 1 d . . H18A H 0.7955(2) 0.3493(6) 0.8853(2) 0.080 Uiso 1 d R . C19 C 0.7303(2) 0.2729(6) 0.9181(2) 0.0297(10) Uani 1 d . . C20 C 0.6746(2) 0.1894(6) 0.9001(2) 0.0285(10) Uani 1 d . . H20A H 0.6569(2) 0.1683(6) 0.9298(2) 0.080 Uiso 1 d R . C21 C 0.6434(2) 0.1358(5) 0.8401(2) 0.0236(10) Uani 1 d . . C22 C 0.7631(3) 0.3379(7) 0.9823(2) 0.0380(12) Uani 1 d . . H22A H 0.7394(3) 0.3106(7) 1.0063(2) 0.080 Uiso 1 d R . H22B H 0.8076(3) 0.3040(7) 1.0028(2) 0.080 Uiso 1 d R . H22C H 0.7630(3) 0.4412(7) 0.9788(2) 0.080 Uiso 1 d R . C23A C 0.5760(8) -0.0469(19) 0.6350(7) 0.054(2) Uiso 0.564(6) d P . C23B C 0.6808(11) 0.1184(23) 0.6754(9) 0.054(2) Uiso 0.436(6) d P . C24 C 0.7832(2) 0.2182(6) 0.4898(2) 0.0315(11) Uani 1 d . . C25 C 0.8298(2) 0.1249(6) 0.4852(2) 0.0358(12) Uani 1 d . . H25A H 0.8290(2) 0.1099(6) 0.4447(2) 0.080 Uiso 1 d R . C26 C 0.8770(3) 0.0532(7) 0.5356(3) 0.0458(14) Uani 1 d . . H26A H 0.9081(3) -0.0090(7) 0.5297(3) 0.080 Uiso 1 d R . C27 C 0.8792(3) 0.0713(7) 0.5947(3) 0.0490(15) Uani 1 d . . H27A H 0.9127(3) 0.0249(7) 0.6303(3) 0.080 Uiso 1 d R . C28 C 0.8326(3) 0.1570(7) 0.6013(3) 0.0449(14) Uani 1 d . . H28A H 0.8325(3) 0.1676(7) 0.6416(3) 0.080 Uiso 1 d R . C29 C 0.7855(3) 0.2290(7) 0.5497(2) 0.0394(12) Uani 1 d . . H29A H 0.7533(3) 0.2879(7) 0.5556(2) 0.080 Uiso 1 d R . C30 C 0.7185(2) 0.2340(6) 0.3644(2) 0.0322(11) Uani 1 d . . C31 C 0.7206(3) 0.2973(7) 0.3117(2) 0.0411(13) Uani 1 d . . H31A H 0.7334(3) 0.3968(7) 0.3140(2) 0.080 Uiso 1 d R . C32 C 0.7046(3) 0.2232(8) 0.2558(3) 0.053(2) Uani 1 d . . H32A H 0.7073(3) 0.2713(8) 0.2209(3) 0.080 Uiso 1 d R . C33 C 0.6854(3) 0.0819(9) 0.2507(3) 0.053(2) Uani 1 d . . H33A H 0.6747(3) 0.0302(9) 0.2124(3) 0.080 Uiso 1 d R . C34 C 0.6818(3) 0.0144(8) 0.3009(3) 0.051(2) Uani 1 d . . H34A H 0.6678(3) -0.0844(8) 0.2976(3) 0.080 Uiso 1 d R . C35 C 0.6981(2) 0.0898(7) 0.3567(2) 0.0425(12) Uani 1 d . . H35A H 0.6953(2) 0.0408(7) 0.3913(2) 0.080 Uiso 1 d R . C36 C 0.6702(2) 0.3770(5) 0.4350(2) 0.0314(11) Uani 1 d . . C37 C 0.6722(3) 0.4767(6) 0.4803(2) 0.0380(12) Uani 1 d . . H37A H 0.7145(3) 0.5106(6) 0.5099(2) 0.080 Uiso 1 d R . C38 C 0.6165(3) 0.5291(7) 0.4846(3) 0.0448(13) Uani 1 d . . H38A H 0.6208(3) 0.5971(7) 0.5168(3) 0.080 Uiso 1 d R . C39 C 0.5550(3) 0.4837(7) 0.4427(3) 0.0475(15) Uani 1 d . . H39A H 0.5161(3) 0.5203(7) 0.4451(3) 0.080 Uiso 1 d R . C40 C 0.5501(3) 0.3853(7) 0.3976(3) 0.0451(15) Uani 1 d . . H40A H 0.5076(3) 0.3511(7) 0.3687(3) 0.080 Uiso 1 d R . C41 C 0.6064(3) 0.3347(6) 0.3938(2) 0.0388(12) Uani 1 d . . H41A H 0.6016(3) 0.2679(6) 0.3611(2) 0.080 Uiso 1 d R . C42 C 0.7821(2) 0.4648(6) 0.4330(2) 0.0297(10) Uani 1 d . . C43 C 0.8506(3) 0.4679(6) 0.4655(2) 0.0343(11) Uani 1 d . . H43A H 0.8726(3) 0.3830(6) 0.4879(2) 0.080 Uiso 1 d R . C44 C 0.8881(3) 0.5879(8) 0.4670(2) 0.0460(13) Uani 1 d . . H44A H 0.9351(3) 0.5841(8) 0.4900(2) 0.080 Uiso 1 d R . C45 C 0.8589(3) 0.7109(7) 0.4360(3) 0.049(2) Uani 1 d . . H45A H 0.8847(3) 0.7944(7) 0.4371(3) 0.080 Uiso 1 d R . C46 C 0.7912(4) 0.7126(7) 0.4030(3) 0.051(2) Uani 1 d . . H46A H 0.7697(4) 0.7982(7) 0.3808(3) 0.080 Uiso 1 d R . C47 C 0.7539(3) 0.5929(7) 0.4016(2) 0.0421(12) Uani 1 d . . H47A H 0.7069(3) 0.5974(7) 0.3782(2) 0.080 Uiso 1 d R . C48 C 0.8946(4) 0.2345(10) 0.3597(4) 0.081(2) Uani 1 d . . C49 C 0.8737(3) 0.0919(11) 0.3342(5) 0.085(2) Uani 1 d . . H49A H 0.8803(3) 0.0265(11) 0.3678(5) 0.080 Uiso 1 d R . H49B H 0.8273(3) 0.0953(11) 0.3077(5) 0.080 Uiso 1 d 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 0.02488(9) 0.02789(10) 0.01672(8) -0.00108(9) 0.00988(6) -0.00048(10) B1 0.037(3) 0.023(3) 0.022(2) 0.000(2) 0.009(2) -0.004(2) N1 0.021(2) 0.035(2) 0.021(2) 0.000(2) 0.0107(15) -0.005(2) N2 0.031(2) 0.034(2) 0.017(2) -0.002(2) 0.010(2) -0.010(2) Cl1A 0.055(2) 0.044(2) 0.041(2) -0.006(2) 0.0276(15) -0.002(2) Cl1B 0.0393(13) 0.0285(12) 0.0318(11) -0.0003(10) 0.0292(10) -0.0056(12) Cl2A 0.043(3) 0.047(3) 0.052(2) 0.016(2) 0.029(2) 0.024(2) Cl2B 0.029(2) 0.030(2) 0.0360(14) 0.0073(11) 0.0180(13) 0.0019(11) Cl3A 0.139(8) 0.135(7) 0.160(10) -0.070(7) 0.059(7) -0.098(9) Cl3B 0.065(4) 0.193(9) 0.129(8) -0.072(6) -0.029(4) 0.042(5) Cl4 0.172(3) 0.090(2) 0.122(2) -0.026(2) 0.092(2) -0.035(2) C1 0.073(4) 0.058(4) 0.063(4) 0.031(3) 0.045(3) 0.037(4) C2 0.035(3) 0.033(3) 0.046(3) 0.016(3) -0.003(2) 0.006(2) C3 0.057(3) 0.030(3) 0.020(2) 0.004(2) 0.008(2) -0.001(3) C4 0.054(3) 0.018(3) 0.030(2) 0.013(2) 0.011(2) 0.006(2) C6 0.120(7) 0.106(8) 0.170(9) 0.073(7) 0.112(8) 0.081(7) C7 0.047(4) 0.063(5) 0.095(5) 0.018(5) -0.018(4) -0.003(4) C8 0.125(6) 0.059(5) 0.025(3) 0.001(3) 0.032(3) -0.006(4) C9 0.075(5) 0.052(5) 0.079(5) 0.023(4) 0.013(4) -0.002(4) C10 0.166(9) 0.052(5) 0.035(3) 0.007(3) 0.015(4) 0.049(5) C11 0.028(2) 0.037(3) 0.027(2) 0.001(2) 0.009(2) -0.003(2) C12 0.026(2) 0.047(3) 0.037(3) -0.003(2) 0.015(2) -0.010(2) C13 0.029(2) 0.053(4) 0.035(2) 0.006(3) 0.017(2) -0.006(2) C14 0.028(2) 0.052(3) 0.026(2) -0.002(2) 0.012(2) -0.006(2) C15 0.021(2) 0.032(3) 0.020(2) 0.000(2) 0.012(2) -0.002(2) C16 0.043(3) 0.076(5) 0.049(3) 0.006(3) 0.028(3) -0.017(3) C17 0.034(3) 0.054(4) 0.025(2) 0.001(2) 0.012(2) -0.013(3) C18 0.035(3) 0.042(3) 0.028(2) 0.002(2) 0.007(2) -0.014(2) C19 0.032(2) 0.029(3) 0.022(2) 0.003(2) 0.005(2) 0.004(2) C20 0.028(2) 0.036(3) 0.021(2) 0.004(2) 0.010(2) 0.002(2) C21 0.024(2) 0.029(3) 0.019(2) 0.000(2) 0.010(2) -0.001(2) C22 0.037(3) 0.040(3) 0.026(2) -0.006(2) 0.003(2) -0.004(2) C24 0.033(2) 0.034(3) 0.025(2) 0.000(2) 0.010(2) -0.008(2) C25 0.039(3) 0.037(3) 0.031(2) 0.004(2) 0.014(2) 0.001(2) C26 0.042(3) 0.046(4) 0.045(3) 0.013(3) 0.015(2) 0.005(3) C27 0.051(3) 0.049(4) 0.034(3) 0.015(3) 0.006(2) -0.003(3) C28 0.059(4) 0.046(3) 0.028(3) 0.006(2) 0.016(2) -0.004(3) C29 0.045(3) 0.043(3) 0.031(2) 0.003(2) 0.016(2) -0.003(3) C30 0.030(2) 0.032(3) 0.029(2) -0.003(2) 0.007(2) 0.005(2) C31 0.040(3) 0.054(4) 0.026(2) -0.003(2) 0.012(2) 0.003(3) C32 0.052(3) 0.073(5) 0.031(3) -0.010(3) 0.015(2) 0.005(3) C33 0.037(3) 0.072(5) 0.040(3) -0.026(3) 0.007(2) 0.010(3) C34 0.033(3) 0.049(4) 0.056(4) -0.021(3) 0.005(3) 0.003(3) C35 0.037(3) 0.039(3) 0.042(3) -0.007(3) 0.007(2) 0.003(3) C36 0.040(3) 0.027(3) 0.026(2) 0.002(2) 0.013(2) -0.002(2) C37 0.040(3) 0.037(3) 0.037(3) 0.000(2) 0.015(2) -0.002(2) C38 0.061(4) 0.036(3) 0.045(3) 0.008(3) 0.030(3) 0.007(3) C39 0.052(3) 0.042(4) 0.056(3) 0.021(3) 0.031(3) 0.014(3) C40 0.036(3) 0.048(4) 0.051(3) 0.014(3) 0.018(2) 0.001(3) C41 0.041(3) 0.031(3) 0.038(3) 0.000(2) 0.011(2) -0.001(2) C42 0.044(3) 0.028(3) 0.021(2) -0.001(2) 0.018(2) 0.001(2) C43 0.043(3) 0.033(3) 0.030(2) -0.005(2) 0.018(2) -0.009(2) C44 0.053(3) 0.052(4) 0.041(3) -0.004(3) 0.028(2) -0.013(3) C45 0.070(4) 0.043(4) 0.057(4) -0.008(3) 0.048(3) -0.014(3) C46 0.091(5) 0.029(3) 0.057(4) 0.008(3) 0.054(4) 0.008(3) C47 0.062(3) 0.030(3) 0.042(3) 0.007(3) 0.030(3) 0.008(3) C48 0.066(5) 0.078(6) 0.097(6) -0.004(5) 0.034(4) 0.006(5) C49 0.046(4) 0.087(6) 0.120(7) -0.004(6) 0.034(4) -0.006(5) _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 C23A 1.90(2) . ? W1 C23B 1.97(2) . ? W1 N2 2.177(4) . ? W1 N1 2.185(3) . ? W1 C3 2.294(5) . ? W1 C2 2.320(5) . ? W1 C4 2.350(5) . ? W1 C1 2.395(6) . ? W1 Cl1A 2.396(4) . ? W1 Cl2A 2.407(4) . ? W1 Cl1B 2.415(2) . ? W1 C5 2.432(6) . ? B1 C36 1.633(7) . ? B1 C24 1.640(7) . ? B1 C30 1.651(7) . ? B1 C42 1.661(7) . ? N1 C11 1.340(6) . ? N1 C15 1.362(5) . ? N2 C17 1.348(6) . ? N2 C21 1.365(5) . ? O1A Cl1A 0.827(9) . ? O1A C23A 1.25(2) . ? O1B Cl1B 0.645(9) . ? O1B C23B 1.03(2) . ? Cl1A C23A 0.60(2) . ? Cl1B C23B 0.59(2) . ? Cl2A Cl2B 0.664(5) . ? Cl3A Cl3B 0.72(2) . ? Cl3A C48 1.731(13) . ? Cl3B C48 1.737(10) . ? Cl4 C49 1.774(9) . ? C1 C5 1.396(9) . ? C1 C2 1.415(9) . ? C1 C6 1.495(9) . ? C2 C3 1.428(8) . ? C2 C7 1.505(9) . ? C3 C4 1.422(7) . ? C3 C8 1.505(7) . ? C4 C5 1.404(7) . ? C4 C9 1.498(9) . ? C5 C10 1.476(9) . ? C11 C12 1.370(7) . ? C12 C13 1.384(7) . ? C13 C14 1.382(7) . ? C13 C16 1.494(7) . ? C14 C15 1.379(6) . ? C15 C21 1.468(6) . ? C17 C18 1.376(7) . ? C18 C19 1.395(7) . ? C19 C20 1.376(7) . ? C19 C22 1.503(6) . ? C20 C21 1.382(6) . ? C24 C25 1.397(7) . ? C24 C29 1.399(7) . ? C25 C26 1.382(7) . ? C26 C27 1.388(8) . ? C27 C28 1.372(9) . ? C28 C29 1.398(8) . ? C30 C31 1.396(7) . ? C30 C35 1.398(8) . ? C31 C32 1.394(8) . ? C32 C33 1.368(10) . ? C33 C34 1.375(9) . ? C34 C35 1.398(8) . ? C36 C37 1.401(7) . ? C36 C41 1.403(7) . ? C37 C38 1.384(8) . ? C38 C39 1.378(9) . ? C39 C40 1.371(9) . ? C40 C41 1.387(8) . ? C42 C43 1.395(7) . ? C42 C47 1.400(7) . ? C43 C44 1.387(8) . ? C44 C45 1.363(9) . ? C45 C46 1.381(9) . ? C46 C47 1.382(9) . ? C48 C49 1.445(12) . ? 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 C23A W1 C23B 85.0(7) . . ? C23A W1 N2 156.8(5) . . ? C23B W1 N2 94.2(6) . . ? C23A W1 N1 98.0(5) . . ? C23B W1 N1 157.9(6) . . ? N2 W1 N1 74.47(14) . . ? C23A W1 C3 73.1(5) . . ? C23B W1 C3 74.0(6) . . ? N2 W1 C3 129.0(2) . . ? N1 W1 C3 127.9(2) . . ? C23A W1 C2 70.4(5) . . ? C23B W1 C2 109.4(6) . . ? N2 W1 C2 130.8(2) . . ? N1 W1 C2 92.1(2) . . ? C3 W1 C2 36.1(2) . . ? C23A W1 C4 107.6(5) . . ? C23B W1 C4 68.9(6) . . ? N2 W1 C4 93.5(2) . . ? N1 W1 C4 129.6(2) . . ? C3 W1 C4 35.6(2) . . ? C2 W1 C4 59.0(2) . . ? C23A W1 C1 103.1(5) . . ? C23B W1 C1 125.3(6) . . ? N2 W1 C1 96.3(2) . . ? N1 W1 C1 75.6(2) . . ? C3 W1 C1 58.1(2) . . ? C2 W1 C1 34.9(2) . . ? C4 W1 C1 56.9(2) . . ? C23A W1 Cl1A 9.0(5) . . ? C23B W1 Cl1A 87.7(6) . . ? N2 W1 Cl1A 148.09(15) . . ? N1 W1 Cl1A 92.31(14) . . ? C3 W1 Cl1A 82.1(2) . . ? C2 W1 Cl1A 77.5(2) . . ? C4 W1 Cl1A 116.6(2) . . ? C1 W1 Cl1A 108.6(2) . . ? C23A W1 Cl2A 85.2(5) . . ? C23B W1 Cl2A 78.5(6) . . ? N2 W1 Cl2A 72.0(2) . . ? N1 W1 Cl2A 80.0(2) . . ? C3 W1 Cl2A 146.0(2) . . ? C2 W1 Cl2A 153.1(2) . . ? C4 W1 Cl2A 143.3(2) . . ? C1 W1 Cl2A 155.0(2) . . ? Cl1A W1 Cl2A 77.2(2) . . ? C23A W1 Cl1B 87.2(5) . . ? C23B W1 Cl1B 10.3(6) . . ? N2 W1 Cl1B 88.25(11) . . ? N1 W1 Cl1B 147.63(12) . . ? C3 W1 Cl1B 84.2(2) . . ? C2 W1 Cl1B 119.5(2) . . ? C4 W1 Cl1B 77.6(2) . . ? C1 W1 Cl1B 134.5(2) . . ? Cl1A W1 Cl1B 88.25(10) . . ? Cl2A W1 Cl1B 68.61(13) . . ? C23A W1 C5 126.5(5) . . ? C23B W1 C5 99.6(6) . . ? N2 W1 C5 76.5(2) . . ? N1 W1 C5 96.2(2) . . ? C3 W1 C5 57.9(2) . . ? C2 W1 C5 57.8(2) . . ? C4 W1 C5 34.1(2) . . ? C1 W1 C5 33.6(2) . . ? Cl1A W1 C5 134.6(2) . . ? Cl2A W1 C5 148.2(2) . . ? Cl1B W1 C5 106.32(14) . . ? C36 B1 C24 113.3(4) . . ? C36 B1 C30 110.2(4) . . ? C24 B1 C30 110.0(4) . . ? C36 B1 C42 107.6(4) . . ? C24 B1 C42 106.5(4) . . ? C30 B1 C42 109.0(4) . . ? C11 N1 C15 118.1(4) . . ? C11 N1 W1 124.8(3) . . ? C15 N1 W1 116.7(3) . . ? C17 N2 C21 118.1(4) . . ? C17 N2 W1 124.1(3) . . ? C21 N2 W1 117.7(3) . . ? Cl1A O1A C23A 23.5(9) . . ? Cl1B O1B C23B 31.6(12) . . ? C23A Cl1A O1A 122.8(19) . . ? C23A Cl1A W1 30.1(17) . . ? O1A Cl1A W1 152.1(7) . . ? C23B Cl1B O1B 113.3(22) . . ? C23B Cl1B W1 36.7(19) . . ? O1B Cl1B W1 149.9(8) . . ? Cl2B Cl2A W1 87.8(6) . . ? Cl2A Cl2B W1 76.6(6) . . ? Cl3B Cl3A C48 78.5(12) . . ? Cl3A Cl3B C48 77.6(13) . . ? C5 C1 C2 109.6(5) . . ? C5 C1 C6 125.4(7) . . ? C2 C1 C6 124.2(8) . . ? C5 C1 W1 74.7(3) . . ? C2 C1 W1 69.7(3) . . ? C6 C1 W1 129.6(5) . . ? C1 C2 C3 106.6(5) . . ? C1 C2 C7 126.0(7) . . ? C3 C2 C7 125.6(6) . . ? C1 C2 W1 75.5(3) . . ? C3 C2 W1 71.0(3) . . ? C7 C2 W1 130.7(5) . . ? C4 C3 C2 107.6(5) . . ? C4 C3 C8 125.3(6) . . ? C2 C3 C8 126.1(6) . . ? C4 C3 W1 74.3(3) . . ? C2 C3 W1 72.9(3) . . ? C8 C3 W1 127.0(4) . . ? C5 C4 C3 108.4(5) . . ? C5 C4 C9 123.5(6) . . ? C3 C4 C9 126.2(5) . . ? C5 C4 W1 76.2(3) . . ? C3 C4 W1 70.1(3) . . ? C9 C4 W1 132.0(4) . . ? C1 C5 C4 107.8(5) . . ? C1 C5 C10 124.8(6) . . ? C4 C5 C10 127.0(6) . . ? C1 C5 W1 71.7(3) . . ? C4 C5 W1 69.7(3) . . ? C10 C5 W1 130.0(4) . . ? N1 C11 C12 122.5(4) . . ? C11 C12 C13 120.6(5) . . ? C14 C13 C12 116.6(4) . . ? C14 C13 C16 120.6(5) . . ? C12 C13 C16 122.8(5) . . ? C15 C14 C13 121.3(4) . . ? N1 C15 C14 120.8(4) . . ? N1 C15 C21 116.2(4) . . ? C14 C15 C21 122.9(4) . . ? N2 C17 C18 122.3(4) . . ? C17 C18 C19 120.0(5) . . ? C20 C19 C18 117.3(4) . . ? C20 C19 C22 121.8(4) . . ? C18 C19 C22 121.0(5) . . ? C19 C20 C21 121.0(4) . . ? N2 C21 C20 121.1(4) . . ? N2 C21 C15 114.5(4) . . ? C20 C21 C15 124.3(4) . . ? Cl1A C23A O1A 33.7(13) . . ? Cl1A C23A W1 140.9(21) . . ? O1A C23A W1 172.1(13) . . ? Cl1B C23B O1B 35.1(15) . . ? Cl1B C23B W1 133.0(23) . . ? O1B C23B W1 168.0(18) . . ? C25 C24 C29 114.6(5) . . ? C25 C24 B1 120.8(4) . . ? C29 C24 B1 124.1(5) . . ? C26 C25 C24 123.7(5) . . ? C25 C26 C27 119.8(6) . . ? C28 C27 C26 118.8(5) . . ? C27 C28 C29 120.5(5) . . ? C28 C29 C24 122.5(5) . . ? C31 C30 C35 114.8(5) . . ? C31 C30 B1 123.7(5) . . ? C35 C30 B1 121.5(5) . . ? C32 C31 C30 123.2(6) . . ? C33 C32 C31 120.0(6) . . ? C32 C33 C34 119.4(5) . . ? C33 C34 C35 120.1(6) . . ? C34 C35 C30 122.6(6) . . ? C37 C36 C41 114.1(5) . . ? C37 C36 B1 121.8(4) . . ? C41 C36 B1 124.1(4) . . ? C38 C37 C36 123.4(5) . . ? C39 C38 C37 119.9(6) . . ? C40 C39 C38 119.2(5) . . ? C39 C40 C41 120.1(5) . . ? C40 C41 C36 123.3(5) . . ? C43 C42 C47 114.8(5) . . ? C43 C42 B1 123.0(5) . . ? C47 C42 B1 122.2(5) . . ? C44 C43 C42 123.0(5) . . ? C45 C44 C43 120.6(5) . . ? C44 C45 C46 118.4(6) . . ? C45 C46 C47 120.9(6) . . ? C46 C47 C42 122.3(6) . . ? C49 C48 Cl3A 112.9(7) . . ? C49 C48 Cl3B 110.2(8) . . ? Cl3A C48 Cl3B 23.9(6) . . ? C48 C49 Cl4 114.6(6) . . ? _refine_diff_density_max 1.242 _refine_diff_density_min -1.971 _refine_diff_density_rms 0.129