# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Hanninen, Mikko' 'Sillanpaa, Reijo' 'Kivela, Henri' 'Lehtonen, Ari' _publ_contact_author_name 'Lehtonen, Ari' _publ_contact_author_email ari.lehtonen@utu.fi _publ_section_title ; Imidotungsten(VI) complexes with chelating amino and imino phenolates ; _publ_requested_category FM # Attachment '- 4_WNPhCl3-LiPr.cif' data_WNPhCl3-LiPr _database_code_depnum_ccdc_archive 'CCDC 797991' #TrackingRef '- 4_WNPhCl3-LiPr.cif' _audit_creation_date 2010-10-14T17:04:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C24 H35 Cl3 N2 O W), C7 H8' _chemical_formula_sum 'C55 H78 Cl6 N4 O2 W2' _chemical_formula_weight 1407.59 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.15330(40) _cell_length_b 21.67530(100) _cell_length_c 13.67660(50) _cell_angle_alpha 90.000 _cell_angle_beta 102.8943(25) _cell_angle_gamma 90.000 _cell_volume 2933.990(209) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5038 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2008)' _exptl_absorpt_correction_T_min 0.5036 _exptl_absorpt_correction_T_max 0.7457 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.777226E-1 _diffrn_orient_matrix_ub_12 0.150119E-1 _diffrn_orient_matrix_ub_13 -0.530834E-1 _diffrn_orient_matrix_ub_21 0.503588E-1 _diffrn_orient_matrix_ub_22 -0.10747E-1 _diffrn_orient_matrix_ub_23 -0.527146E-1 _diffrn_orient_matrix_ub_31 -0.403964E-1 _diffrn_orient_matrix_ub_32 -0.422803E-1 _diffrn_orient_matrix_ub_33 -0.54483E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_unetI/netI 0.0544 _diffrn_reflns_number 13972 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 5083 _reflns_number_gt 4128 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0000P)^2^+37.7363P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5083 _refine_ls_number_parameters 327 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.072 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.189 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.154 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.54252(4) 0.236358(18) -0.00924(3) 0.03252(14) Uani 1 1 d . . . Cl1 Cl 0.3459(3) 0.17618(13) -0.03215(19) 0.0476(6) Uani 1 1 d . . . Cl2 Cl 0.4057(3) 0.32237(12) 0.00892(19) 0.0471(6) Uani 1 1 d . . . Cl3 Cl 0.7316(3) 0.30185(13) 0.0452(2) 0.0553(7) Uani 1 1 d . . . O1 O 0.6465(6) 0.1643(3) 0.0106(4) 0.0340(15) Uani 1 1 d . . . N1 N 0.5429(8) 0.2489(3) -0.1336(6) 0.0326(18) Uani 1 1 d . . . N8 N 0.5658(9) 0.2299(4) 0.1645(6) 0.047(2) Uani 1 1 d . . . H8 H 0.5893 0.2705 0.1824 0.057 Uiso 1 1 calc R . . C1 C 0.6932(8) 0.1194(4) 0.0797(6) 0.0266(19) Uani 1 1 d . . . C2 C 0.7279(9) 0.0622(4) 0.0436(7) 0.030(2) Uani 1 1 d . . . C3 C 0.7769(9) 0.0187(4) 0.1171(7) 0.033(2) Uani 1 1 d . . . H3 H 0.8018 -0.0206 0.0961 0.04 Uiso 1 1 calc R . . C4 C 0.7921(9) 0.0288(4) 0.2197(7) 0.033(2) Uani 1 1 d . A . C5 C 0.7564(9) 0.0866(5) 0.2497(7) 0.036(2) Uani 1 1 d . . . H5 H 0.7652 0.0944 0.3192 0.044 Uiso 1 1 calc R . . C6 C 0.7089(9) 0.1328(5) 0.1819(7) 0.034(2) Uani 1 1 d . . . C7 C 0.6921(11) 0.1977(5) 0.2177(7) 0.045(3) Uani 1 1 d . . . H7A H 0.6931 0.1963 0.2902 0.053 Uiso 1 1 calc R . . H7B H 0.7709 0.2226 0.2097 0.053 Uiso 1 1 calc R . . C9 C 0.4468(10) 0.2227(5) 0.2108(7) 0.047(3) Uani 1 1 d . . . H9 H 0.3647 0.2378 0.1619 0.056 Uiso 1 1 calc R . . C10 C 0.4294(12) 0.1517(6) 0.2277(9) 0.062(3) Uani 1 1 d . . . H10A H 0.4291 0.1294 0.1653 0.093 Uiso 1 1 calc R . . H10B H 0.3439 0.1444 0.2477 0.093 Uiso 1 1 calc R . . H10C H 0.5045 0.1369 0.2806 0.093 Uiso 1 1 calc R . . C11 C 0.4600(13) 0.2580(6) 0.3054(9) 0.068(4) Uani 1 1 d . . . H11A H 0.5391 0.2433 0.3548 0.102 Uiso 1 1 calc R . . H11B H 0.3786 0.2521 0.3317 0.102 Uiso 1 1 calc R . . H11C H 0.4709 0.302 0.2923 0.102 Uiso 1 1 calc R . . C12 C 0.7157(9) 0.0488(4) -0.0684(6) 0.029(2) Uani 1 1 d . . . C13 C 0.5676(10) 0.0521(5) -0.1231(8) 0.047(3) Uani 1 1 d . . . H13A H 0.5153 0.0223 -0.0934 0.07 Uiso 1 1 calc R . . H13B H 0.5594 0.0423 -0.1941 0.07 Uiso 1 1 calc R . . H13C H 0.5331 0.0938 -0.1168 0.07 Uiso 1 1 calc R . . C14 C 0.7704(12) -0.0156(4) -0.0843(7) 0.046(3) Uani 1 1 d . . . H14A H 0.8657 -0.0182 -0.0495 0.069 Uiso 1 1 calc R . . H14B H 0.7621 -0.0227 -0.1562 0.069 Uiso 1 1 calc R . . H14C H 0.7185 -0.0468 -0.0574 0.069 Uiso 1 1 calc R . . C15 C 0.7976(10) 0.0958(4) -0.1132(7) 0.035(2) Uani 1 1 d . . . H15A H 0.7628 0.1373 -0.1063 0.053 Uiso 1 1 calc R . . H15B H 0.7901 0.0865 -0.1843 0.053 Uiso 1 1 calc R . . H15C H 0.8927 0.0936 -0.0776 0.053 Uiso 1 1 calc R . . C16 C 0.8515(10) -0.0201(5) 0.2983(7) 0.040(2) Uani 1 1 d D . . C17A C 0.7735(19) -0.0275(8) 0.3767(12) 0.055(5) Uani 0.721(18) 1 d P A 2 H17A H 0.8119 -0.0614 0.4216 0.083 Uiso 0.721(18) 1 calc PR A 2 H17B H 0.6792 -0.037 0.3452 0.083 Uiso 0.721(18) 1 calc PR A 2 H17C H 0.7776 0.0108 0.4153 0.083 Uiso 0.721(18) 1 calc PR A 2 C18A C 0.9986(16) -0.0018(9) 0.3478(16) 0.072(7) Uani 0.721(18) 1 d P A 2 H18A H 1.0379 -0.0328 0.398 0.108 Uiso 0.721(18) 1 calc PR A 2 H18B H 0.999 0.0385 0.3804 0.108 Uiso 0.721(18) 1 calc PR A 2 H18C H 1.052 0.0005 0.2965 0.108 Uiso 0.721(18) 1 calc PR A 2 C19A C 0.8661(18) -0.0852(6) 0.2513(11) 0.051(5) Uani 0.721(18) 1 d P A 2 H19A H 0.9249 -0.0819 0.2037 0.076 Uiso 0.721(18) 1 calc PR A 2 H19B H 0.7768 -0.1 0.2164 0.076 Uiso 0.721(18) 1 calc PR A 2 H19C H 0.9057 -0.1143 0.3047 0.076 Uiso 0.721(18) 1 calc PR A 2 C17B C 0.858(5) 0.006(2) 0.404(2) 0.065(14) Uiso 0.279(18) 1 d PD A 3 H17D H 0.8866 -0.0266 0.4539 0.098 Uiso 0.279(18) 1 calc PR A 3 H17E H 0.768 0.0209 0.4083 0.098 Uiso 0.279(18) 1 calc PR A 3 H17F H 0.9224 0.0402 0.417 0.098 Uiso 0.279(18) 1 calc PR A 3 C18B C 0.991(3) -0.036(3) 0.286(5) 0.086(18) Uiso 0.279(18) 1 d PD A 3 H18D H 1.021 -0.0747 0.3225 0.129 Uiso 0.279(18) 1 calc PR A 3 H18E H 1.0539 -0.003 0.3134 0.129 Uiso 0.279(18) 1 calc PR A 3 H18F H 0.9898 -0.042 0.2149 0.129 Uiso 0.279(18) 1 calc PR A 3 C19B C 0.745(4) -0.0722(18) 0.284(3) 0.048(11) Uiso 0.279(18) 1 d P A 3 H19D H 0.7163 -0.0822 0.2128 0.072 Uiso 0.279(18) 1 calc PR A 3 H19E H 0.6673 -0.0586 0.3097 0.072 Uiso 0.279(18) 1 calc PR A 3 H19F H 0.7852 -0.1089 0.3213 0.072 Uiso 0.279(18) 1 calc PR A 3 C20 C 0.5516(9) 0.2699(4) -0.2293(7) 0.033(2) Uani 1 1 d . . . C21 C 0.5400(9) 0.3327(5) -0.2489(8) 0.040(2) Uani 1 1 d . . . H21 H 0.5291 0.3606 -0.1977 0.048 Uiso 1 1 calc R . . C22 C 0.5444(10) 0.3540(5) -0.3414(8) 0.046(3) Uani 1 1 d . . . H22 H 0.5331 0.3968 -0.3558 0.055 Uiso 1 1 calc R . . C23 C 0.5651(10) 0.3136(6) -0.4151(8) 0.055(3) Uani 1 1 d . . . H23 H 0.5679 0.3287 -0.4799 0.066 Uiso 1 1 calc R . . C24 C 0.5813(11) 0.2530(6) -0.3945(8) 0.051(3) Uani 1 1 d . . . H24 H 0.5993 0.2259 -0.4445 0.062 Uiso 1 1 calc R . . C25 C 0.5721(10) 0.2288(5) -0.3010(7) 0.045(3) Uani 1 1 d . . . H25 H 0.5798 0.1857 -0.2878 0.054 Uiso 1 1 calc R . . C36 C 0.890(4) 0.5807(19) -0.069(3) 0.136(17) Uiso 0.5 1 d PD B -1 H36A H 0.9009 0.6137 -0.0187 0.205 Uiso 0.5 1 calc PR B -1 H36B H 0.794 0.571 -0.0923 0.205 Uiso 0.5 1 calc PR B -1 H36C H 0.9271 0.5942 -0.1256 0.205 Uiso 0.5 1 calc PR B -1 C30 C 0.999(4) 0.416(2) -0.007(3) 0.136 Uiso 0.5 1 d PD B -1 H30 H 0.9773 0.3741 -0.0245 0.164 Uiso 0.5 1 calc PR B -1 C31 C 1.106(4) 0.434(2) 0.067(3) 0.136 Uiso 0.5 1 d PD B -1 H31 H 1.1592 0.4009 0.101 0.164 Uiso 0.5 1 calc PR B -1 C32 C 1.149(4) 0.4913(19) 0.100(3) 0.136 Uiso 0.5 1 d PD B -1 H32 H 1.2267 0.4977 0.1519 0.164 Uiso 0.5 1 calc PR B -1 C33 C 1.073(5) 0.539(2) 0.053(3) 0.136 Uiso 0.5 1 d PD B -1 H33 H 1.095 0.5803 0.0712 0.164 Uiso 0.5 1 calc PR B -1 C34 C 0.965(4) 0.524(2) -0.022(3) 0.136 Uiso 0.5 1 d PD B -1 C35 C 0.926(5) 0.466(2) -0.053(4) 0.136 Uiso 0.5 1 d PD B -1 H35 H 0.8495 0.4591 -0.1068 0.164 Uiso 0.5 1 calc PR B -1 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 0.0361(2) 0.0345(2) 0.0288(2) 0.00233(18) 0.01113(15) 0.00859(19) Cl1 0.0408(14) 0.0619(17) 0.0427(14) -0.0108(13) 0.0147(12) -0.0081(12) Cl2 0.0547(15) 0.0452(15) 0.0435(14) 0.0056(12) 0.0158(12) 0.0230(12) Cl3 0.0494(16) 0.0552(17) 0.0647(18) -0.0163(14) 0.0195(14) -0.0083(13) O1 0.043(4) 0.033(4) 0.028(3) -0.004(3) 0.013(3) 0.002(3) N1 0.036(4) 0.030(4) 0.034(4) 0.006(3) 0.012(3) 0.011(3) N8 0.054(5) 0.055(6) 0.034(4) 0.004(4) 0.011(4) 0.029(5) C1 0.018(4) 0.037(5) 0.024(4) 0.005(4) 0.002(3) 0.008(4) C2 0.029(5) 0.034(5) 0.030(5) -0.001(4) 0.013(4) -0.002(4) C3 0.039(5) 0.030(5) 0.031(5) 0.001(4) 0.009(4) -0.001(4) C4 0.031(5) 0.037(5) 0.029(5) 0.008(4) 0.005(4) -0.005(4) C5 0.034(5) 0.050(6) 0.024(5) 0.001(4) 0.005(4) 0.005(5) C6 0.029(5) 0.045(6) 0.029(5) -0.005(4) 0.006(4) 0.006(4) C7 0.052(6) 0.050(6) 0.030(5) -0.009(5) 0.005(5) 0.019(5) C9 0.035(5) 0.072(8) 0.035(5) 0.012(5) 0.011(4) 0.005(5) C10 0.043(6) 0.078(9) 0.065(8) 0.000(7) 0.015(6) -0.010(6) C11 0.065(8) 0.095(10) 0.047(7) -0.022(7) 0.018(6) 0.010(7) C12 0.032(5) 0.030(5) 0.028(5) 0.001(4) 0.010(4) -0.002(4) C13 0.041(6) 0.062(7) 0.037(6) -0.009(5) 0.009(5) -0.012(5) C14 0.074(8) 0.034(6) 0.031(5) -0.007(4) 0.014(5) 0.002(5) C15 0.041(6) 0.042(6) 0.026(5) -0.002(4) 0.017(4) -0.003(4) C16 0.044(6) 0.041(6) 0.031(5) 0.004(4) 0.003(4) -0.005(5) C17A 0.077(12) 0.046(10) 0.050(10) 0.023(8) 0.029(9) 0.022(9) C18A 0.039(9) 0.074(13) 0.090(15) 0.053(12) -0.014(9) 0.007(8) C19A 0.083(12) 0.026(8) 0.039(8) 0.008(6) 0.005(8) 0.016(7) C20 0.024(4) 0.044(6) 0.032(5) 0.010(4) 0.012(4) 0.003(4) C21 0.034(5) 0.041(6) 0.047(6) 0.008(5) 0.014(5) 0.000(4) C22 0.034(5) 0.046(6) 0.060(7) 0.016(6) 0.013(5) 0.003(5) C23 0.037(6) 0.082(9) 0.045(6) 0.030(6) 0.009(5) 0.011(6) C24 0.051(7) 0.072(9) 0.033(5) 0.007(5) 0.013(5) 0.019(6) C25 0.048(6) 0.051(7) 0.033(5) 0.005(5) 0.005(5) 0.011(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.723(7) . ? W1 O1 1.870(6) . ? W1 N8 2.339(8) . ? W1 Cl1 2.347(3) . ? W1 Cl3 2.370(3) . ? W1 Cl2 2.371(2) . ? O1 C1 1.365(10) . ? N1 C20 1.406(11) . ? N8 C9 1.493(13) . ? N8 C7 1.498(12) . ? N8 H8 0.93 . ? C1 C6 1.402(12) . ? C1 C2 1.409(12) . ? C2 C3 1.387(12) . ? C2 C12 1.536(12) . ? C3 C4 1.394(12) . ? C3 H3 0.95 . ? C4 C5 1.392(13) . ? C4 C16 1.535(13) . ? C5 C6 1.377(13) . ? C5 H5 0.95 . ? C6 C7 1.513(13) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C9 C11 1.483(15) . ? C9 C10 1.573(16) . ? C9 H9 1 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C13 1.524(13) . ? C12 C15 1.526(12) . ? C12 C14 1.536(13) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17A 1.477(17) . ? C16 C18B 1.507(19) . ? C16 C17B 1.540(19) . ? C16 C19B 1.54(4) . ? C16 C18A 1.547(19) . ? C16 C19A 1.571(17) . ? C17A H17A 0.98 . ? C17A H17B 0.98 . ? C17A H17C 0.98 . ? C18A H18A 0.98 . ? C18A H18B 0.98 . ? C18A H18C 0.98 . ? C19A H19A 0.98 . ? C19A H19B 0.98 . ? C19A H19C 0.98 . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? C18B H18D 0.98 . ? C18B H18E 0.98 . ? C18B H18F 0.98 . ? C19B H19D 0.98 . ? C19B H19E 0.98 . ? C19B H19F 0.98 . ? C20 C25 1.375(14) . ? C20 C21 1.388(13) . ? C21 C22 1.358(14) . ? C21 H21 0.95 . ? C22 C23 1.385(16) . ? C22 H22 0.95 . ? C23 C24 1.347(15) . ? C23 H23 0.95 . ? C24 C25 1.405(14) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? C36 C34 1.50(2) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C30 C31 1.366(19) . ? C30 C35 1.38(2) . ? C30 H30 0.95 . ? C31 C32 1.361(19) . ? C31 H31 0.95 . ? C32 C33 1.36(2) . ? C32 H32 0.95 . ? C33 C34 1.366(18) . ? C33 H33 0.95 . ? C34 C35 1.368(18) . ? C35 H35 0.95 . ? 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 O1 98.6(3) . . ? N1 W1 N8 171.9(4) . . ? O1 W1 N8 82.9(3) . . ? N1 W1 Cl1 98.3(3) . . ? O1 W1 Cl1 89.5(2) . . ? N8 W1 Cl1 89.6(2) . . ? N1 W1 Cl3 92.0(3) . . ? O1 W1 Cl3 93.6(2) . . ? N8 W1 Cl3 80.0(3) . . ? Cl1 W1 Cl3 168.61(9) . . ? N1 W1 Cl2 96.3(2) . . ? O1 W1 Cl2 165.06(19) . . ? N8 W1 Cl2 82.5(2) . . ? Cl1 W1 Cl2 87.15(10) . . ? Cl3 W1 Cl2 87.04(10) . . ? C1 O1 W1 142.5(5) . . ? C20 N1 W1 169.7(7) . . ? C9 N8 C7 115.6(8) . . ? C9 N8 W1 122.0(6) . . ? C7 N8 W1 113.7(6) . . ? C9 N8 H8 99.9 . . ? C7 N8 H8 99.9 . . ? W1 N8 H8 99.9 . . ? O1 C1 C6 119.2(8) . . ? O1 C1 C2 117.5(7) . . ? C6 C1 C2 123.3(8) . . ? C3 C2 C1 115.0(8) . . ? C3 C2 C12 122.0(8) . . ? C1 C2 C12 122.9(8) . . ? C2 C3 C4 124.3(9) . . ? C2 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? C5 C4 C3 117.5(8) . . ? C5 C4 C16 120.2(8) . . ? C3 C4 C16 122.3(9) . . ? C6 C5 C4 122.1(9) . . ? C6 C5 H5 119 . . ? C4 C5 H5 119 . . ? C5 C6 C1 117.8(9) . . ? C5 C6 C7 120.4(8) . . ? C1 C6 C7 121.3(9) . . ? N8 C7 C6 115.0(8) . . ? N8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? N8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C11 C9 N8 113.1(9) . . ? C11 C9 C10 111.6(10) . . ? N8 C9 C10 107.0(9) . . ? C11 C9 H9 108.3 . . ? N8 C9 H9 108.3 . . ? C10 C9 H9 108.3 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C15 109.8(8) . . ? C13 C12 C14 108.8(8) . . ? C15 C12 C14 107.6(8) . . ? C13 C12 C2 109.4(7) . . ? C15 C12 C2 110.2(7) . . ? C14 C12 C2 111.1(7) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17A C16 C18B 136(2) . . ? C17A C16 C4 113.2(10) . . ? C18B C16 C4 108(2) . . ? C17A C16 C17B 43.5(19) . . ? C18B C16 C17B 110(3) . . ? C4 C16 C17B 109.4(19) . . ? C17A C16 C19B 62.5(17) . . ? C18B C16 C19B 118(3) . . ? C4 C16 C19B 105.3(16) . . ? C17B C16 C19B 105(3) . . ? C17A C16 C18A 109.4(13) . . ? C18B C16 C18A 43(2) . . ? C4 C16 C18A 108.6(9) . . ? C17B C16 C18A 70(2) . . ? C19B C16 C18A 145.2(17) . . ? C17A C16 C19A 108.3(11) . . ? C18B C16 C19A 64(2) . . ? C4 C16 C19A 113.0(9) . . ? C17B C16 C19A 137(2) . . ? C19B C16 C19A 54.5(16) . . ? C18A C16 C19A 103.9(12) . . ? C16 C17A H17A 109.5 . . ? C16 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C16 C18A H18A 109.5 . . ? C16 C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C16 C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C16 C19A H19A 109.5 . . ? C16 C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C16 C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C16 C17B H17D 109.5 . . ? C16 C17B H17E 109.5 . . ? C16 C17B H17F 109.5 . . ? C16 C18B H18D 109.5 . . ? C16 C18B H18E 109.5 . . ? C16 C18B H18F 109.5 . . ? C16 C19B H19D 109.5 . . ? C16 C19B H19E 109.5 . . ? C16 C19B H19F 109.5 . . ? C25 C20 C21 121.2(9) . . ? C25 C20 N1 120.4(9) . . ? C21 C20 N1 118.4(8) . . ? C22 C21 C20 119.7(10) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.4(10) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 119.7(10) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 121.7(11) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C20 C25 C24 117.3(10) . . ? C20 C25 H25 121.3 . . ? C24 C25 H25 121.3 . . ? C31 C30 C35 112(5) . . ? C31 C30 H30 124 . . ? C35 C30 H30 124 . . ? C32 C31 C30 130(5) . . ? C32 C31 H31 114.9 . . ? C30 C31 H31 114.9 . . ? C33 C32 C31 116(5) . . ? C33 C32 H32 122.2 . . ? C31 C32 H32 122.2 . . ? C32 C33 C34 117(5) . . ? C32 C33 H33 121.3 . . ? C34 C33 H33 121.3 . . ? C33 C34 C35 125(4) . . ? C33 C34 C36 112(4) . . ? C35 C34 C36 123(4) . . ? C34 C35 C30 120(5) . . ? C34 C35 H35 120.2 . . ? C30 C35 H35 120.2 . . ? 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 N1 W1 O1 C1 -174.7(9) . . . . ? N8 W1 O1 C1 13.3(9) . . . . ? Cl1 W1 O1 C1 -76.3(9) . . . . ? Cl3 W1 O1 C1 92.7(9) . . . . ? Cl2 W1 O1 C1 0.7(15) . . . . ? O1 W1 N1 C20 -127(4) . . . . ? N8 W1 N1 C20 -26(5) . . . . ? Cl1 W1 N1 C20 142(4) . . . . ? Cl3 W1 N1 C20 -33(4) . . . . ? Cl2 W1 N1 C20 54(4) . . . . ? N1 W1 N8 C9 140(2) . . . . ? O1 W1 N8 C9 -118.4(8) . . . . ? Cl1 W1 N8 C9 -28.8(8) . . . . ? Cl3 W1 N8 C9 146.6(8) . . . . ? Cl2 W1 N8 C9 58.3(7) . . . . ? N1 W1 N8 C7 -74(2) . . . . ? O1 W1 N8 C7 27.7(7) . . . . ? Cl1 W1 N8 C7 117.3(7) . . . . ? Cl3 W1 N8 C7 -67.2(7) . . . . ? Cl2 W1 N8 C7 -155.5(7) . . . . ? W1 O1 C1 C6 -25.8(14) . . . . ? W1 O1 C1 C2 156.5(7) . . . . ? O1 C1 C2 C3 178.9(8) . . . . ? C6 C1 C2 C3 1.3(13) . . . . ? O1 C1 C2 C12 0.1(12) . . . . ? C6 C1 C2 C12 -177.4(8) . . . . ? C1 C2 C3 C4 0.1(13) . . . . ? C12 C2 C3 C4 178.9(8) . . . . ? C2 C3 C4 C5 -0.5(14) . . . . ? C2 C3 C4 C16 -177.8(9) . . . . ? C3 C4 C5 C6 -0.6(14) . . . . ? C16 C4 C5 C6 176.8(9) . . . . ? C4 C5 C6 C1 1.9(14) . . . . ? C4 C5 C6 C7 -170.3(9) . . . . ? O1 C1 C6 C5 -179.8(8) . . . . ? C2 C1 C6 C5 -2.3(14) . . . . ? O1 C1 C6 C7 -7.7(13) . . . . ? C2 C1 C6 C7 169.8(9) . . . . ? C9 N8 C7 C6 91.3(11) . . . . ? W1 N8 C7 C6 -57.1(11) . . . . ? C5 C6 C7 N8 -138.5(9) . . . . ? C1 C6 C7 N8 49.6(13) . . . . ? C7 N8 C9 C11 72.2(12) . . . . ? W1 N8 C9 C11 -142.2(8) . . . . ? C7 N8 C9 C10 -51.1(11) . . . . ? W1 N8 C9 C10 94.5(9) . . . . ? C3 C2 C12 C13 117.3(10) . . . . ? C1 C2 C12 C13 -64.1(11) . . . . ? C3 C2 C12 C15 -122.0(9) . . . . ? C1 C2 C12 C15 56.7(11) . . . . ? C3 C2 C12 C14 -2.8(12) . . . . ? C1 C2 C12 C14 175.8(8) . . . . ? C5 C4 C16 C17A 48.1(14) . . . . ? C3 C4 C16 C17A -134.6(12) . . . . ? C5 C4 C16 C18B -119(3) . . . . ? C3 C4 C16 C18B 58(3) . . . . ? C5 C4 C16 C17B 1(2) . . . . ? C3 C4 C16 C17B 179(2) . . . . ? C5 C4 C16 C19B 114.3(18) . . . . ? C3 C4 C16 C19B -68.5(19) . . . . ? C5 C4 C16 C18A -73.6(14) . . . . ? C3 C4 C16 C18A 103.7(14) . . . . ? C5 C4 C16 C19A 171.7(10) . . . . ? C3 C4 C16 C19A -11.1(14) . . . . ? W1 N1 C20 C25 153(3) . . . . ? W1 N1 C20 C21 -26(4) . . . . ? C25 C20 C21 C22 2.3(14) . . . . ? N1 C20 C21 C22 -178.2(9) . . . . ? C20 C21 C22 C23 -2.3(15) . . . . ? C21 C22 C23 C24 -0.2(16) . . . . ? C22 C23 C24 C25 2.7(17) . . . . ? C21 C20 C25 C24 0.2(14) . . . . ? N1 C20 C25 C24 -179.3(9) . . . . ? C23 C24 C25 C20 -2.7(16) . . . . ? C35 C30 C31 C32 0.0(14) . . . . ? C30 C31 C32 C33 1(2) . . . . ? C31 C32 C33 C34 -1(3) . . . . ? C32 C33 C34 C35 0(3) . . . . ? C32 C33 C34 C36 -179.4(15) . . . . ? C33 C34 C35 C30 1(3) . . . . ? C36 C34 C35 C30 -179.8(13) . . . . ? C31 C30 C35 C34 -1(2) . . . . ? # END of CIF # Attachment '- 5_WNPhCl3L-ON.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-02-26 at 11:20:20 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : C:\Program Files\wingx\files\archive.reqdat # CIF files read : import struct data_import _database_code_depnum_ccdc_archive 'CCDC 797992' #TrackingRef '- 5_WNPhCl3L-ON.cif' _audit_creation_date 2010-02-26T11:20:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H31 Cl3 N2 O W' _chemical_formula_sum 'C27 H31 Cl3 N2 O W' _chemical_formula_weight 689.74 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/n_1 _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_Int_Tables_number 14 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 13.780(5) _cell_length_b 14.203(5) _cell_length_c 14.757(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 105.262(5) _cell_angle_gamma 90.000(5) _cell_volume 2786.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6927 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.7 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.455 _exptl_absorpt_correction_T_min 0.5345 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2008)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.512378E-1 _diffrn_orient_matrix_ub_12 0.69829E-2 _diffrn_orient_matrix_ub_13 -0.240688E-1 _diffrn_orient_matrix_ub_21 -0.254772E-1 _diffrn_orient_matrix_ub_22 0.682264E-1 _diffrn_orient_matrix_ub_23 0.25042E-1 _diffrn_orient_matrix_ub_31 0.280113E-1 _diffrn_orient_matrix_ub_32 0.748272E-1 _diffrn_orient_matrix_ub_33 -0.205868E-1 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_number 18167 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5464 _reflns_number_gt 4949 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0000P)^2^+3.0891P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5464 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.568 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.280943(8) 0.434092(8) 0.103173(8) 0.01651(5) Uani 1 1 d . . . Cl1 Cl 0.24933(6) 0.50343(6) 0.23736(5) 0.02721(18) Uani 1 1 d . . . Cl3 Cl 0.33703(6) 0.39787(6) -0.03094(5) 0.02902(18) Uani 1 1 d . . . Cl2 Cl 0.16869(6) 0.54000(6) 0.01101(5) 0.02737(18) Uani 1 1 d . . . N1 N 0.19610(17) 0.34240(18) 0.09701(16) 0.0194(5) Uani 1 1 d . . . N8 N 0.40091(18) 0.55288(17) 0.12189(17) 0.0188(5) Uani 1 1 d . . . O1 O 0.39343(14) 0.37093(14) 0.17864(13) 0.0196(4) Uani 1 1 d . . . C3 C 0.6442(2) 0.3075(2) 0.30965(18) 0.0176(6) Uani 1 1 d . . . H3 H 0.6781 0.2574 0.3447 0.021 Uiso 1 1 calc R . . C2 C 0.5408(2) 0.2991(2) 0.27160(18) 0.0164(6) Uani 1 1 d . . . C14 C 0.3734(3) 0.6667(3) -0.0072(2) 0.0308(8) Uani 1 1 d . . . H14 H 0.387 0.6197 -0.046 0.037 Uiso 1 1 calc R . . C4 C 0.7004(2) 0.3867(2) 0.29844(19) 0.0183(6) Uani 1 1 d . . . C7 C 0.4950(2) 0.5431(2) 0.1651(2) 0.0187(6) Uani 1 1 d . . . H7 H 0.5357 0.5955 0.1663 0.022 Uiso 1 1 calc R . . C26 C -0.0310(3) 0.1472(3) 0.0853(2) 0.0341(9) Uani 1 1 d . . . H26 H -0.0823 0.1038 0.0824 0.041 Uiso 1 1 calc R . . C6 C 0.5440(2) 0.4596(2) 0.2117(2) 0.0180(6) Uani 1 1 d . . . C19 C 0.8155(2) 0.3846(2) 0.3381(2) 0.0249(7) Uani 1 1 d . . . C9 C 0.3751(2) 0.6471(2) 0.0847(2) 0.0189(6) Uani 1 1 d . . . C24 C 0.1413(2) 0.1803(2) 0.0916(2) 0.0277(7) Uani 1 1 d . . . H24 H 0.2057 0.1596 0.093 0.033 Uiso 1 1 calc R . . C23 C 0.1215(2) 0.2757(2) 0.09408(19) 0.0180(6) Uani 1 1 d . . . C16 C 0.4395(2) 0.1643(2) 0.1865(2) 0.0221(7) Uani 1 1 d . . . H16A H 0.494 0.1493 0.1597 0.033 Uiso 1 1 calc R . . H16B H 0.3942 0.207 0.1458 0.033 Uiso 1 1 calc R . . H16C H 0.4043 0.1076 0.1936 0.033 Uiso 1 1 calc R . . C10 C 0.3541(2) 0.7156(2) 0.1426(2) 0.0264(7) Uani 1 1 d . . . H10 H 0.355 0.7013 0.2043 0.032 Uiso 1 1 calc R . . C1 C 0.4928(2) 0.3768(2) 0.22074(19) 0.0168(6) Uani 1 1 d . . . C5 C 0.6487(2) 0.4630(2) 0.25067(19) 0.0197(6) Uani 1 1 d . . . H5 H 0.6838 0.5174 0.2442 0.024 Uiso 1 1 calc R . . C27 C -0.0505(2) 0.2419(3) 0.0882(2) 0.0320(8) Uani 1 1 d . . . H27 H -0.1151 0.2621 0.0868 0.038 Uiso 1 1 calc R . . C28 C 0.0251(2) 0.3075(3) 0.0932(2) 0.0258(7) Uani 1 1 d . . . H28 H 0.012 0.3715 0.0959 0.031 Uiso 1 1 calc R . . C15 C 0.4814(2) 0.2105(2) 0.28312(19) 0.0175(6) Uani 1 1 d . . . C18 C 0.3955(2) 0.2360(2) 0.3277(2) 0.0238(7) Uani 1 1 d . . . H18A H 0.3653 0.1793 0.343 0.036 Uiso 1 1 calc R . . H18B H 0.3458 0.2725 0.284 0.036 Uiso 1 1 calc R . . H18C H 0.422 0.272 0.3838 0.036 Uiso 1 1 calc R . . C11 C 0.3316(3) 0.8066(3) 0.1080(3) 0.0332(8) Uani 1 1 d . . . H11 H 0.3171 0.8535 0.1465 0.04 Uiso 1 1 calc R . . C22 C 0.8416(2) 0.3756(3) 0.4450(2) 0.0337(9) Uani 1 1 d . . . H22A H 0.9134 0.3729 0.4696 0.051 Uiso 1 1 calc R . . H22B H 0.8121 0.3192 0.4616 0.051 Uiso 1 1 calc R . . H22C H 0.8158 0.4291 0.4709 0.051 Uiso 1 1 calc R . . C17 C 0.5484(2) 0.1381(2) 0.3474(2) 0.0230(7) Uani 1 1 d . . . H17A H 0.6029 0.1206 0.3216 0.035 Uiso 1 1 calc R . . H17B H 0.5094 0.0832 0.3524 0.035 Uiso 1 1 calc R . . H17C H 0.5749 0.1649 0.4087 0.035 Uiso 1 1 calc R . . C12 C 0.3308(2) 0.8266(2) 0.0161(3) 0.0327(8) Uani 1 1 d . . . H12 H 0.3165 0.8873 -0.0071 0.039 Uiso 1 1 calc R . . C25 C 0.0646(3) 0.1160(3) 0.0869(3) 0.0365(9) Uani 1 1 d . . . H25 H 0.0774 0.0519 0.0848 0.044 Uiso 1 1 calc R . . C13 C 0.3511(3) 0.7572(3) -0.0408(2) 0.0344(9) Uani 1 1 d . . . H13 H 0.3499 0.7711 -0.1026 0.041 Uiso 1 1 calc R . . C21 C 0.8570(2) 0.2996(3) 0.2966(3) 0.0382(9) Uani 1 1 d . . . H21A H 0.8399 0.305 0.2294 0.057 Uiso 1 1 calc R . . H21B H 0.8283 0.2429 0.3137 0.057 Uiso 1 1 calc R . . H21C H 0.9288 0.2976 0.3206 0.057 Uiso 1 1 calc R . . C20 C 0.8643(2) 0.4735(3) 0.3119(3) 0.0402(10) Uani 1 1 d . . . H20A H 0.8493 0.4786 0.2448 0.06 Uiso 1 1 calc R . . H20B H 0.9358 0.4702 0.3378 0.06 Uiso 1 1 calc R . . H20C H 0.8384 0.5276 0.3368 0.06 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 0.01505(7) 0.01320(8) 0.02038(7) 0.00086(5) 0.00310(4) 0.00124(5) Cl1 0.0300(4) 0.0264(5) 0.0278(4) -0.0048(3) 0.0120(3) -0.0011(3) Cl3 0.0376(5) 0.0242(4) 0.0294(4) -0.0061(3) 0.0160(3) -0.0034(4) Cl2 0.0233(4) 0.0191(4) 0.0336(4) 0.0043(3) -0.0032(3) 0.0032(3) N1 0.0174(13) 0.0199(15) 0.0206(12) 0.0002(11) 0.0046(10) 0.0048(11) N8 0.0211(14) 0.0138(14) 0.0224(13) -0.0001(10) 0.0074(10) 0.0023(10) O1 0.0174(10) 0.0154(11) 0.0245(11) 0.0033(9) 0.0026(8) 0.0002(9) C3 0.0181(15) 0.0192(17) 0.0153(13) 0.0027(12) 0.0041(11) 0.0033(13) C2 0.0191(15) 0.0162(16) 0.0151(13) -0.0011(12) 0.0069(11) 0.0016(12) C14 0.038(2) 0.026(2) 0.0321(18) 0.0043(15) 0.0155(14) 0.0068(16) C4 0.0185(15) 0.0197(17) 0.0173(14) 0.0014(12) 0.0056(11) -0.0009(13) C7 0.0221(16) 0.0129(16) 0.0219(15) 0.0003(12) 0.0072(12) -0.0022(12) C26 0.0303(19) 0.039(2) 0.0294(18) 0.0092(16) 0.0021(14) -0.0165(17) C6 0.0201(15) 0.0140(16) 0.0208(14) 0.0026(12) 0.0071(11) 0.0026(12) C19 0.0160(15) 0.0275(19) 0.0293(17) 0.0116(14) 0.0027(12) -0.0015(13) C9 0.0166(15) 0.0138(16) 0.0263(15) 0.0040(12) 0.0056(11) -0.0011(12) C24 0.0213(16) 0.0213(19) 0.0376(18) 0.0011(15) 0.0023(13) 0.0020(14) C23 0.0185(15) 0.0181(16) 0.0161(14) 0.0037(12) 0.0020(11) -0.0046(12) C16 0.0231(16) 0.0184(17) 0.0233(15) -0.0017(13) 0.0035(12) -0.0016(13) C10 0.0312(18) 0.0196(18) 0.0303(17) 0.0011(14) 0.0114(13) 0.0000(14) C1 0.0152(14) 0.0177(16) 0.0178(14) -0.0021(12) 0.0051(11) 0.0015(12) C5 0.0224(16) 0.0173(16) 0.0207(15) 0.0017(12) 0.0078(12) -0.0042(13) C27 0.0220(17) 0.045(2) 0.0317(18) 0.0012(16) 0.0110(13) -0.0044(16) C28 0.0213(16) 0.0292(19) 0.0264(16) 0.0024(14) 0.0056(12) 0.0025(14) C15 0.0192(15) 0.0143(16) 0.0186(14) -0.0020(12) 0.0045(11) -0.0010(12) C18 0.0259(17) 0.0213(18) 0.0278(16) 0.0044(14) 0.0133(13) 0.0001(14) C11 0.0318(19) 0.0202(19) 0.053(2) -0.0008(17) 0.0207(16) 0.0047(15) C22 0.0275(18) 0.036(2) 0.0317(18) 0.0062(16) -0.0033(14) -0.0056(16) C17 0.0251(16) 0.0180(17) 0.0248(16) 0.0056(13) 0.0044(12) -0.0021(13) C12 0.0284(18) 0.0170(18) 0.054(2) 0.0143(16) 0.0128(15) 0.0024(14) C25 0.039(2) 0.021(2) 0.043(2) 0.0048(16) 0.0000(16) -0.0051(16) C13 0.038(2) 0.032(2) 0.0350(19) 0.0167(16) 0.0124(15) 0.0040(17) C21 0.0199(17) 0.048(3) 0.048(2) 0.0030(19) 0.0117(15) 0.0075(17) C20 0.0188(18) 0.041(2) 0.056(2) 0.0196(19) 0.0010(16) -0.0062(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.736(3) . ? W1 O1 1.8812(19) . ? W1 Cl2 2.3232(9) . ? W1 N8 2.327(3) . ? W1 Cl1 2.3527(10) . ? W1 Cl3 2.3630(10) . ? N1 C23 1.390(4) . ? N8 C7 1.294(4) . ? N8 C9 1.455(4) . ? O1 C1 1.349(3) . ? C3 C2 1.392(4) . ? C3 C4 1.400(4) . ? C2 C1 1.400(4) . ? C2 C15 1.534(4) . ? C14 C9 1.379(4) . ? C14 C13 1.383(5) . ? C4 C5 1.383(4) . ? C4 C19 1.540(4) . ? C7 C6 1.445(4) . ? C26 C27 1.375(5) . ? C26 C25 1.384(5) . ? C6 C1 1.396(4) . ? C6 C5 1.407(4) . ? C19 C20 1.526(5) . ? C19 C22 1.529(4) . ? C19 C21 1.531(5) . ? C9 C10 1.374(4) . ? C24 C23 1.384(4) . ? C24 C25 1.384(5) . ? C23 C28 1.400(4) . ? C16 C15 1.538(4) . ? C10 C11 1.395(5) . ? C27 C28 1.385(5) . ? C15 C17 1.534(4) . ? C15 C18 1.541(4) . ? C11 C12 1.383(5) . ? C12 C13 1.370(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 O1 96.42(10) . . ? N1 W1 Cl2 96.87(8) . . ? O1 W1 Cl2 166.70(6) . . ? N1 W1 N8 175.91(9) . . ? O1 W1 N8 80.01(9) . . ? Cl2 W1 N8 86.72(7) . . ? N1 W1 Cl1 94.97(8) . . ? O1 W1 Cl1 90.44(7) . . ? Cl2 W1 Cl1 88.82(4) . . ? N8 W1 Cl1 83.09(7) . . ? N1 W1 Cl3 99.04(8) . . ? O1 W1 Cl3 89.53(7) . . ? Cl2 W1 Cl3 87.98(4) . . ? N8 W1 Cl3 83.02(7) . . ? Cl1 W1 Cl3 165.91(3) . . ? C23 N1 W1 174.2(2) . . ? C7 N8 C9 113.5(2) . . ? C7 N8 W1 124.7(2) . . ? C9 N8 W1 121.78(18) . . ? C1 O1 W1 145.22(19) . . ? C2 C3 C4 124.1(3) . . ? C3 C2 C1 115.9(3) . . ? C3 C2 C15 123.0(3) . . ? C1 C2 C15 121.0(2) . . ? C9 C14 C13 119.0(3) . . ? C5 C4 C3 117.6(3) . . ? C5 C4 C19 123.3(3) . . ? C3 C4 C19 119.1(3) . . ? N8 C7 C6 127.2(3) . . ? C27 C26 C25 120.4(3) . . ? C1 C6 C5 118.7(3) . . ? C1 C6 C7 123.5(3) . . ? C5 C6 C7 117.8(3) . . ? C20 C19 C22 109.3(3) . . ? C20 C19 C21 108.4(3) . . ? C22 C19 C21 109.6(3) . . ? C20 C19 C4 111.5(3) . . ? C22 C19 C4 109.4(3) . . ? C21 C19 C4 108.6(3) . . ? C10 C9 C14 121.2(3) . . ? C10 C9 N8 119.1(3) . . ? C14 C9 N8 119.7(3) . . ? C23 C24 C25 119.6(3) . . ? C24 C23 N1 121.2(3) . . ? C24 C23 C28 120.6(3) . . ? N1 C23 C28 118.2(3) . . ? C9 C10 C11 119.4(3) . . ? O1 C1 C6 119.0(3) . . ? O1 C1 C2 118.5(3) . . ? C6 C1 C2 122.4(3) . . ? C4 C5 C6 121.1(3) . . ? C26 C27 C28 120.6(3) . . ? C27 C28 C23 118.8(3) . . ? C17 C15 C2 111.5(2) . . ? C17 C15 C16 107.7(2) . . ? C2 C15 C16 109.2(2) . . ? C17 C15 C18 107.3(2) . . ? C2 C15 C18 110.3(2) . . ? C16 C15 C18 110.7(2) . . ? C12 C11 C10 119.5(3) . . ? C13 C12 C11 120.2(3) . . ? C24 C25 C26 120.0(3) . . ? C12 C13 C14 120.7(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 O1 W1 N1 C23 134(2) . . . . ? Cl2 W1 N1 C23 -47(2) . . . . ? N8 W1 N1 C23 104(2) . . . . ? Cl1 W1 N1 C23 43(2) . . . . ? Cl3 W1 N1 C23 -136(2) . . . . ? N1 W1 N8 C7 33.8(15) . . . . ? O1 W1 N8 C7 4.1(2) . . . . ? Cl2 W1 N8 C7 -175.0(2) . . . . ? Cl1 W1 N8 C7 95.8(2) . . . . ? Cl3 W1 N8 C7 -86.6(2) . . . . ? N1 W1 N8 C9 -146.2(13) . . . . ? O1 W1 N8 C9 -175.9(2) . . . . ? Cl2 W1 N8 C9 5.0(2) . . . . ? Cl1 W1 N8 C9 -84.2(2) . . . . ? Cl3 W1 N8 C9 93.4(2) . . . . ? N1 W1 O1 C1 177.9(3) . . . . ? Cl2 W1 O1 C1 -0.3(6) . . . . ? N8 W1 O1 C1 -4.1(3) . . . . ? Cl1 W1 O1 C1 -87.0(3) . . . . ? Cl3 W1 O1 C1 78.9(3) . . . . ? C4 C3 C2 C1 -1.1(4) . . . . ? C4 C3 C2 C15 178.6(3) . . . . ? C2 C3 C4 C5 3.5(4) . . . . ? C2 C3 C4 C19 -175.7(3) . . . . ? C9 N8 C7 C6 178.3(3) . . . . ? W1 N8 C7 C6 -1.7(4) . . . . ? N8 C7 C6 C1 -3.7(5) . . . . ? N8 C7 C6 C5 177.0(3) . . . . ? C5 C4 C19 C20 -3.9(4) . . . . ? C3 C4 C19 C20 175.2(3) . . . . ? C5 C4 C19 C22 117.1(3) . . . . ? C3 C4 C19 C22 -63.8(4) . . . . ? C5 C4 C19 C21 -123.3(3) . . . . ? C3 C4 C19 C21 55.8(4) . . . . ? C13 C14 C9 C10 0.6(5) . . . . ? C13 C14 C9 N8 -178.4(3) . . . . ? C7 N8 C9 C10 -84.5(3) . . . . ? W1 N8 C9 C10 95.5(3) . . . . ? C7 N8 C9 C14 94.6(3) . . . . ? W1 N8 C9 C14 -85.4(3) . . . . ? C25 C24 C23 N1 -178.8(3) . . . . ? C25 C24 C23 C28 0.8(5) . . . . ? W1 N1 C23 C24 -168.9(19) . . . . ? W1 N1 C23 C28 11(2) . . . . ? C14 C9 C10 C11 -0.5(5) . . . . ? N8 C9 C10 C11 178.5(3) . . . . ? W1 O1 C1 C6 0.6(5) . . . . ? W1 O1 C1 C2 -179.0(2) . . . . ? C5 C6 C1 O1 -175.9(3) . . . . ? C7 C6 C1 O1 4.8(4) . . . . ? C5 C6 C1 C2 3.6(4) . . . . ? C7 C6 C1 C2 -175.6(3) . . . . ? C3 C2 C1 O1 177.0(2) . . . . ? C15 C2 C1 O1 -2.7(4) . . . . ? C3 C2 C1 C6 -2.6(4) . . . . ? C15 C2 C1 C6 177.7(3) . . . . ? C3 C4 C5 C6 -2.4(4) . . . . ? C19 C4 C5 C6 176.7(3) . . . . ? C1 C6 C5 C4 -1.0(4) . . . . ? C7 C6 C5 C4 178.3(3) . . . . ? C25 C26 C27 C28 -0.4(5) . . . . ? C26 C27 C28 C23 0.8(5) . . . . ? C24 C23 C28 C27 -1.0(4) . . . . ? N1 C23 C28 C27 178.6(3) . . . . ? C3 C2 C15 C17 4.6(4) . . . . ? C1 C2 C15 C17 -175.7(3) . . . . ? C3 C2 C15 C16 -114.3(3) . . . . ? C1 C2 C15 C16 65.3(3) . . . . ? C3 C2 C15 C18 123.8(3) . . . . ? C1 C2 C15 C18 -56.5(3) . . . . ? C9 C10 C11 C12 -0.1(5) . . . . ? C10 C11 C12 C13 0.7(5) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C27 C26 C25 C24 0.1(5) . . . . ? C11 C12 C13 C14 -0.6(5) . . . . ? C9 C14 C13 C12 -0.1(5) . . . . ? # END of CIF