Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christopher Cummins' _publ_contact_author_address ; Department of Chemistry Massachusetts Institute of Technology room 6-435 77 Massachusetts Avenue Cambridge MA 02139-4307 UNITED STATES OF AMERICA ; _publ_contact_author_email CCUMMINS@MIT.EDU _publ_section_title ; 6-Coordinate Tungsten(VI) Tris-N-isopropylanilide Complexes: Products of Terminal Oxo and Nitrido Transformations Effected by Main Group Electrophiles ; loop_ _publ_author_name 'C. Cummins' 'Christopher R. Clough' 'Peter Muller' data_1-(NC(O)CF3)Cl _database_code_depnum_ccdc_archive 'CCDC 675710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common W(NC(O)CF3)(Cl)(N(i-Pr)Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H48 Cl F3 N4 O W' _chemical_formula_weight 817.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Monoclinic _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 18.1298(6) _cell_length_b 10.4918(3) _cell_length_c 19.4084(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.0410(10) _cell_angle_gamma 90.00 _cell_volume 3529.67(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8634 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.06 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 3.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6477 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details sadabs _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73315 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8736 _reflns_number_gt 7001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT 5 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT 5 (Bruker-AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+1.4281P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8736 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.092820(9) 0.843115(14) 0.827802(8) 0.01431(5) Uani 1 1 d . . . Cl1 Cl 0.22243(6) 0.73229(10) 0.86223(5) 0.0215(2) Uani 1 1 d . . . F1 F 0.22661(17) 1.2110(3) 0.94102(16) 0.0419(7) Uani 1 1 d . . . N1 N 0.05460(19) 0.7047(3) 0.87411(16) 0.0174(7) Uani 1 1 d . . . O1 O 0.1605(3) 0.9985(5) 1.01097(18) 0.0765(16) Uani 1 1 d . . . N2 N 0.09959(18) 0.8405(3) 0.72942(16) 0.0157(6) Uani 1 1 d . . . F2 F 0.28647(14) 1.0530(3) 0.91204(13) 0.0336(6) Uani 1 1 d . . . F3 F 0.29957(16) 1.0920(3) 1.02356(14) 0.0422(7) Uani 1 1 d . . . N3 N -0.00352(19) 0.9418(3) 0.79865(17) 0.0173(7) Uani 1 1 d . . . N4 N 0.14119(19) 0.9609(3) 0.89185(17) 0.0206(7) Uani 1 1 d . . . C11 C -0.0236(2) 0.6580(4) 0.8504(2) 0.0195(8) Uani 1 1 d . . . C12 C -0.0439(3) 0.5644(4) 0.7971(2) 0.0229(9) Uani 1 1 d . . . H12 H -0.0064 0.5329 0.7760 0.028 Uiso 1 1 calc R . . C13 C -0.1187(3) 0.5170(4) 0.7748(2) 0.0322(11) Uani 1 1 d . . . C14 C -0.1728(3) 0.5635(4) 0.8061(2) 0.0324(11) Uani 1 1 d . . . H14 H -0.2238 0.5305 0.7911 0.039 Uiso 1 1 calc R . . C15 C -0.1544(3) 0.6566(4) 0.8586(2) 0.0298(10) Uani 1 1 d . . . C16 C -0.0792(2) 0.7049(4) 0.8803(2) 0.0226(9) Uani 1 1 d . . . H16 H -0.0660 0.7702 0.9158 0.027 Uiso 1 1 calc R . . C17 C 0.1030(2) 0.6379(4) 0.9409(2) 0.0247(9) Uani 1 1 d . . . H17 H 0.1554 0.6776 0.9539 0.030 Uiso 1 1 calc R . . C18 C 0.1129(3) 0.4971(4) 0.9253(3) 0.0351(11) Uani 1 1 d . . . H18A H 0.1331 0.4896 0.8838 0.053 Uiso 1 1 calc R . . H18B H 0.0628 0.4540 0.9145 0.053 Uiso 1 1 calc R . . H18C H 0.1490 0.4574 0.9675 0.053 Uiso 1 1 calc R . . C19 C 0.0715(3) 0.6564(5) 1.0051(2) 0.0344(11) Uani 1 1 d . . . H19A H 0.0661 0.7477 1.0131 0.052 Uiso 1 1 calc R . . H19B H 0.1073 0.6184 1.0482 0.052 Uiso 1 1 calc R . . H19C H 0.0211 0.6149 0.9952 0.052 Uiso 1 1 calc R . . C21 C 0.0664(2) 0.7337(4) 0.6847(2) 0.0177(8) Uani 1 1 d . . . C22 C 0.0925(2) 0.6102(4) 0.7056(2) 0.0207(9) Uani 1 1 d . . . H22 H 0.1330 0.5974 0.7489 0.025 Uiso 1 1 calc R . . C23 C 0.0596(3) 0.5055(4) 0.6633(2) 0.0226(9) Uani 1 1 d . . . C24 C 0.0005(2) 0.5266(4) 0.5998(2) 0.0257(9) Uani 1 1 d . . . H24 H -0.0228 0.4558 0.5711 0.031 Uiso 1 1 calc R . . C25 C -0.0251(2) 0.6497(4) 0.5772(2) 0.0250(9) Uani 1 1 d . . . C26 C 0.0087(2) 0.7520(4) 0.6206(2) 0.0207(9) Uani 1 1 d . . . H26 H -0.0082 0.8362 0.6060 0.025 Uiso 1 1 calc R . . C27 C 0.1352(2) 0.9366(4) 0.6923(2) 0.0208(9) Uani 1 1 d . . . H27 H 0.0943 0.9685 0.6491 0.025 Uiso 1 1 calc R . . C28 C 0.1981(3) 0.8733(4) 0.6667(2) 0.0281(10) Uani 1 1 d . . . H28A H 0.1763 0.8004 0.6359 0.042 Uiso 1 1 calc R . . H28B H 0.2396 0.8439 0.7084 0.042 Uiso 1 1 calc R . . H28C H 0.2188 0.9349 0.6392 0.042 Uiso 1 1 calc R . . C29 C 0.1680(3) 1.0504(4) 0.7404(2) 0.0238(9) Uani 1 1 d . . . H29A H 0.1271 1.0903 0.7565 0.036 Uiso 1 1 calc R . . H29B H 0.1887 1.1125 0.7131 0.036 Uiso 1 1 calc R . . H29C H 0.2094 1.0216 0.7824 0.036 Uiso 1 1 calc R . . C31 C -0.0562(2) 0.9456(4) 0.7258(2) 0.0180(8) Uani 1 1 d . . . C32 C -0.0490(2) 1.0389(4) 0.6774(2) 0.0211(9) Uani 1 1 d . . . H32 H -0.0095 1.1014 0.6919 0.025 Uiso 1 1 calc R . . C33 C -0.0999(3) 1.0410(4) 0.6072(2) 0.0257(9) Uani 1 1 d . . . C34 C -0.1572(2) 0.9498(4) 0.5879(2) 0.0271(10) Uani 1 1 d . . . H34 H -0.1919 0.9510 0.5406 0.032 Uiso 1 1 calc R . . C35 C -0.1657(2) 0.8559(4) 0.6360(2) 0.0250(9) Uani 1 1 d . . . C36 C -0.1141(2) 0.8548(4) 0.7055(2) 0.0229(9) Uani 1 1 d . . . H36 H -0.1188 0.7916 0.7390 0.027 Uiso 1 1 calc R . . C37 C -0.0274(2) 1.0275(4) 0.8510(2) 0.0207(8) Uani 1 1 d . . . H37 H -0.0033 0.9939 0.9007 0.025 Uiso 1 1 calc R . . C38 C -0.1147(2) 1.0322(4) 0.8379(2) 0.0254(9) Uani 1 1 d . . . H38A H -0.1342 0.9457 0.8403 0.038 Uiso 1 1 calc R . . H38B H -0.1394 1.0685 0.7902 0.038 Uiso 1 1 calc R . . H38C H -0.1264 1.0853 0.8748 0.038 Uiso 1 1 calc R . . C39 C 0.0036(3) 1.1620(4) 0.8473(2) 0.0264(9) Uani 1 1 d . . . H39A H 0.0595 1.1585 0.8557 0.040 Uiso 1 1 calc R . . H39B H -0.0080 1.2154 0.8843 0.040 Uiso 1 1 calc R . . H39C H -0.0210 1.1985 0.7996 0.040 Uiso 1 1 calc R . . C41 C 0.1782(3) 1.0079(4) 0.9564(2) 0.0293(10) Uani 1 1 d . . . C42 C 0.2485(3) 1.0908(4) 0.9576(2) 0.0294(10) Uani 1 1 d . . . C131 C -0.1408(3) 0.4156(5) 0.7169(3) 0.0495(15) Uani 1 1 d . . . H13A H -0.1524 0.3359 0.7379 0.074 Uiso 1 1 calc R . . H13B H -0.0979 0.4018 0.6966 0.074 Uiso 1 1 calc R . . H13C H -0.1864 0.4435 0.6787 0.074 Uiso 1 1 calc R . . C151 C -0.2136(3) 0.7069(5) 0.8931(3) 0.0408(13) Uani 1 1 d . . . H15A H -0.2656 0.6888 0.8616 0.061 Uiso 1 1 calc R . . H15B H -0.2070 0.7991 0.9002 0.061 Uiso 1 1 calc R . . H15C H -0.2064 0.6652 0.9398 0.061 Uiso 1 1 calc R . . C231 C 0.0883(3) 0.3727(4) 0.6859(2) 0.0322(11) Uani 1 1 d . . . H23A H 0.0499 0.3105 0.6600 0.048 Uiso 1 1 calc R . . H23B H 0.0968 0.3629 0.7379 0.048 Uiso 1 1 calc R . . H23C H 0.1369 0.3584 0.6746 0.048 Uiso 1 1 calc R . . C251 C -0.0894(3) 0.6717(5) 0.5090(2) 0.0357(11) Uani 1 1 d . . . H25A H -0.1382 0.6819 0.5205 0.054 Uiso 1 1 calc R . . H25B H -0.0931 0.5986 0.4767 0.054 Uiso 1 1 calc R . . H25C H -0.0787 0.7490 0.4852 0.054 Uiso 1 1 calc R . . C331 C -0.0893(3) 1.1389(5) 0.5540(2) 0.0368(12) Uani 1 1 d . . . H33A H -0.0441 1.1166 0.5385 0.055 Uiso 1 1 calc R . . H33B H -0.0815 1.2231 0.5769 0.055 Uiso 1 1 calc R . . H33C H -0.1352 1.1406 0.5120 0.055 Uiso 1 1 calc R . . C351 C -0.2281(3) 0.7564(5) 0.6153(3) 0.0367(12) Uani 1 1 d . . . H35A H -0.2514 0.7572 0.5629 0.055 Uiso 1 1 calc R . . H35B H -0.2677 0.7751 0.6390 0.055 Uiso 1 1 calc R . . H35C H -0.2058 0.6722 0.6305 0.055 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 0.01537(8) 0.01304(8) 0.01463(8) -0.00036(6) 0.00459(5) -0.00134(7) Cl1 0.0168(5) 0.0238(5) 0.0225(5) -0.0005(4) 0.0038(4) 0.0026(4) F1 0.0434(18) 0.0241(14) 0.0633(19) 0.0082(14) 0.0236(15) -0.0070(13) N1 0.0170(17) 0.0193(17) 0.0152(15) 0.0023(13) 0.0035(13) -0.0026(14) O1 0.099(4) 0.109(4) 0.0260(19) -0.013(2) 0.025(2) -0.079(3) N2 0.0174(16) 0.0134(15) 0.0174(15) 0.0007(13) 0.0066(13) 0.0005(14) F2 0.0260(14) 0.0415(16) 0.0326(14) -0.0017(12) 0.0074(12) -0.0070(12) F3 0.0329(16) 0.0543(19) 0.0311(15) -0.0123(14) -0.0034(12) -0.0101(14) N3 0.0197(18) 0.0129(16) 0.0200(16) 0.0004(13) 0.0071(14) -0.0002(13) N4 0.0197(18) 0.0186(17) 0.0220(17) -0.0051(14) 0.0038(14) -0.0037(14) C11 0.017(2) 0.019(2) 0.0186(18) 0.0098(17) -0.0006(15) -0.0014(17) C12 0.029(2) 0.016(2) 0.023(2) 0.0012(16) 0.0079(18) -0.0008(18) C13 0.035(3) 0.023(2) 0.030(2) 0.0040(19) -0.005(2) -0.011(2) C14 0.021(2) 0.033(3) 0.038(3) 0.015(2) 0.000(2) -0.006(2) C15 0.026(2) 0.031(2) 0.034(2) 0.019(2) 0.0097(19) 0.003(2) C16 0.027(2) 0.019(2) 0.022(2) 0.0052(17) 0.0074(18) -0.0024(18) C17 0.019(2) 0.034(3) 0.0183(19) 0.0062(18) 0.0022(16) -0.0047(19) C18 0.032(3) 0.028(3) 0.042(3) 0.013(2) 0.005(2) 0.010(2) C19 0.031(3) 0.052(3) 0.017(2) 0.006(2) 0.0035(18) -0.011(2) C21 0.018(2) 0.019(2) 0.0173(18) -0.0001(16) 0.0077(16) 0.0022(16) C22 0.024(2) 0.020(2) 0.0168(19) 0.0001(16) 0.0034(16) -0.0016(17) C23 0.030(2) 0.018(2) 0.021(2) -0.0029(16) 0.0085(18) 0.0015(18) C24 0.028(2) 0.026(2) 0.023(2) -0.0084(18) 0.0073(18) -0.0052(19) C25 0.024(2) 0.028(2) 0.022(2) -0.0027(18) 0.0052(17) 0.0055(19) C26 0.023(2) 0.019(2) 0.020(2) 0.0026(16) 0.0062(17) 0.0036(17) C27 0.026(2) 0.019(2) 0.0198(19) 0.0013(16) 0.0122(17) -0.0007(17) C28 0.029(3) 0.030(3) 0.031(2) -0.0009(19) 0.017(2) -0.0016(19) C29 0.030(2) 0.018(2) 0.025(2) 0.0017(17) 0.0124(19) -0.0036(18) C31 0.019(2) 0.014(2) 0.022(2) 0.0020(15) 0.0081(16) 0.0069(16) C32 0.021(2) 0.017(2) 0.027(2) -0.0012(17) 0.0094(17) 0.0024(17) C33 0.029(2) 0.026(2) 0.024(2) 0.0062(18) 0.0101(18) 0.0094(19) C34 0.019(2) 0.033(3) 0.025(2) 0.0035(19) 0.0006(17) 0.0067(19) C35 0.018(2) 0.029(2) 0.027(2) 0.0026(19) 0.0045(17) 0.0054(18) C36 0.023(2) 0.019(2) 0.026(2) 0.0027(17) 0.0071(17) 0.0027(18) C37 0.024(2) 0.021(2) 0.0181(19) -0.0008(17) 0.0083(17) 0.0012(18) C38 0.024(2) 0.027(2) 0.030(2) 0.0034(19) 0.0146(19) 0.0054(19) C39 0.029(2) 0.023(2) 0.030(2) -0.0081(19) 0.0122(19) 0.0009(19) C41 0.033(3) 0.029(3) 0.023(2) 0.0023(18) 0.0051(19) -0.011(2) C42 0.030(3) 0.027(3) 0.028(2) 0.0020(19) 0.004(2) -0.008(2) C131 0.053(4) 0.038(3) 0.043(3) -0.005(3) -0.007(3) -0.014(3) C151 0.028(3) 0.049(3) 0.050(3) 0.023(3) 0.019(2) 0.009(2) C231 0.045(3) 0.017(2) 0.029(2) -0.0006(18) 0.003(2) 0.002(2) C251 0.035(3) 0.036(3) 0.030(2) -0.005(2) 0.001(2) 0.003(2) C331 0.042(3) 0.037(3) 0.029(2) 0.010(2) 0.006(2) 0.006(2) C351 0.026(3) 0.040(3) 0.035(3) 0.000(2) -0.004(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N4 1.790(3) . ? W1 N1 1.940(3) . ? W1 N2 1.949(3) . ? W1 N3 1.965(3) . ? W1 Cl1 2.5298(10) . ? F1 C42 1.333(5) . ? N1 C11 1.442(5) . ? N1 C17 1.508(5) . ? O1 C41 1.199(5) . ? N2 C21 1.437(5) . ? N2 C27 1.491(5) . ? F2 C42 1.331(5) . ? F3 C42 1.342(5) . ? N3 C31 1.457(5) . ? N3 C37 1.512(5) . ? N4 C41 1.330(5) . ? C11 C16 1.393(6) . ? C11 C12 1.394(6) . ? C12 C13 1.388(6) . ? C13 C14 1.385(7) . ? C13 C131 1.514(6) . ? C14 C15 1.380(7) . ? C15 C16 1.398(6) . ? C15 C151 1.516(7) . ? C17 C19 1.527(6) . ? C17 C18 1.529(6) . ? C21 C26 1.385(5) . ? C21 C22 1.399(5) . ? C22 C23 1.396(5) . ? C23 C24 1.394(6) . ? C23 C231 1.507(6) . ? C24 C25 1.399(6) . ? C25 C26 1.392(6) . ? C25 C251 1.503(6) . ? C27 C29 1.524(5) . ? C27 C28 1.525(6) . ? C31 C36 1.388(6) . ? C31 C32 1.388(5) . ? C32 C33 1.405(6) . ? C33 C34 1.381(6) . ? C33 C331 1.508(6) . ? C34 C35 1.397(6) . ? C35 C36 1.397(6) . ? C35 C351 1.504(6) . ? C37 C39 1.528(6) . ? C37 C38 1.529(6) . ? C41 C42 1.537(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 W1 N1 111.36(14) . . ? N4 W1 N2 122.09(14) . . ? N1 W1 N2 125.25(13) . . ? N4 W1 N3 92.83(14) . . ? N1 W1 N3 96.88(14) . . ? N2 W1 N3 91.78(13) . . ? N4 W1 Cl1 84.60(11) . . ? N1 W1 Cl1 87.92(10) . . ? N2 W1 Cl1 86.10(9) . . ? N3 W1 Cl1 175.12(10) . . ? C11 N1 C17 112.8(3) . . ? C11 N1 W1 123.9(2) . . ? C17 N1 W1 123.3(3) . . ? C21 N2 C27 113.5(3) . . ? C21 N2 W1 117.9(2) . . ? C27 N2 W1 128.6(2) . . ? C31 N3 C37 113.6(3) . . ? C31 N3 W1 124.6(2) . . ? C37 N3 W1 121.7(2) . . ? C41 N4 W1 156.8(3) . . ? C16 C11 C12 119.5(4) . . ? C16 C11 N1 120.7(4) . . ? C12 C11 N1 119.8(4) . . ? C13 C12 C11 120.3(4) . . ? C14 C13 C12 119.3(4) . . ? C14 C13 C131 120.4(4) . . ? C12 C13 C131 120.3(5) . . ? C15 C14 C13 121.6(4) . . ? C14 C15 C16 118.9(4) . . ? C14 C15 C151 121.5(4) . . ? C16 C15 C151 119.6(5) . . ? C11 C16 C15 120.4(4) . . ? N1 C17 C19 112.3(4) . . ? N1 C17 C18 110.6(3) . . ? C19 C17 C18 112.2(4) . . ? C26 C21 C22 119.5(4) . . ? C26 C21 N2 120.4(4) . . ? C22 C21 N2 120.1(3) . . ? C23 C22 C21 120.6(4) . . ? C24 C23 C22 118.7(4) . . ? C24 C23 C231 121.0(4) . . ? C22 C23 C231 120.3(4) . . ? C23 C24 C25 121.5(4) . . ? C26 C25 C24 118.4(4) . . ? C26 C25 C251 120.4(4) . . ? C24 C25 C251 121.2(4) . . ? C21 C26 C25 121.3(4) . . ? N2 C27 C29 112.4(3) . . ? N2 C27 C28 109.5(3) . . ? C29 C27 C28 110.2(4) . . ? C36 C31 C32 120.4(4) . . ? C36 C31 N3 118.9(3) . . ? C32 C31 N3 120.7(4) . . ? C31 C32 C33 120.1(4) . . ? C34 C33 C32 118.7(4) . . ? C34 C33 C331 121.6(4) . . ? C32 C33 C331 119.7(4) . . ? C33 C34 C35 122.0(4) . . ? C34 C35 C36 118.5(4) . . ? C34 C35 C351 122.2(4) . . ? C36 C35 C351 119.4(4) . . ? C31 C36 C35 120.4(4) . . ? N3 C37 C39 109.7(3) . . ? N3 C37 C38 113.2(3) . . ? C39 C37 C38 109.8(3) . . ? O1 C41 N4 127.6(4) . . ? O1 C41 C42 118.0(4) . . ? N4 C41 C42 114.3(4) . . ? F2 C42 F1 107.3(4) . . ? F2 C42 F3 106.8(4) . . ? F1 C42 F3 107.2(4) . . ? F2 C42 C41 114.1(4) . . ? F1 C42 C41 110.2(4) . . ? F3 C42 C41 110.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.302 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.142 #===END data_1-(OCN)(Cl)2 _database_code_depnum_ccdc_archive 'CCDC 675711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common W(OCN)(Cl)2(N(i-Pr)Ar)3 _chemical_melting_point ? _chemical_formula_moiety 'C34 H48 Cl2 N4 O W 2(C8 H16 O2)' _chemical_formula_sum 'C42 H64 Cl2 N4 O3 W' _chemical_formula_weight 927.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 13.3600(12) _cell_length_b 13.3600(12) _cell_length_c 39.556(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6114.5(14) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3905 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 3.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4972 _exptl_absorpt_correction_T_max 0.8891 _exptl_absorpt_process_details sadabs _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10803 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.14 _reflns_number_total 2442 _reflns_number_gt 1981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT 5 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT 5 (Bruker-AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+7.7033P] 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 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2442 _refine_ls_number_parameters 288 _refine_ls_number_restraints 345 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.3333 0.6667 0.366555(12) 0.0422(2) Uani 1 3 d S . . Cl1 Cl 0.2155(4) 0.5037(4) 0.32637(14) 0.0616(12) Uani 0.67 1 d PU A 1 O1X O 0.239(2) 0.5450(17) 0.3320(6) 0.055(5) Uani 0.33 1 d PU A 2 C1X C 0.261(2) 0.5405(18) 0.2990(6) 0.053(4) Uani 0.33 1 d PU A 2 N1X N 0.2656(18) 0.5261(19) 0.2715(5) 0.068(5) Uani 0.33 1 d PU A 2 N2 N 0.3669(4) 0.5603(4) 0.39074(15) 0.0433(13) Uani 1 1 d . A . C1 C 0.4491(6) 0.6093(5) 0.44760(19) 0.0473(17) Uani 1 1 d . A . H1 H 0.3734 0.5848 0.4557 0.057 Uiso 1 1 calc R . . C2 C 0.4668(5) 0.6051(5) 0.41384(19) 0.0458(16) Uani 1 1 d . . . C3 C 0.5402(7) 0.6487(6) 0.4703(2) 0.0551(19) Uani 1 1 d . . . C4 C 0.5752(6) 0.6383(7) 0.4013(2) 0.062(2) Uani 1 1 d . A . H4 H 0.5867 0.6351 0.3777 0.075 Uiso 1 1 calc R . . C5 C 0.3168(7) 0.4322(6) 0.3845(2) 0.066(2) Uani 1 1 d . . . H5 H 0.2399 0.4034 0.3734 0.079 Uiso 1 1 calc R A . C6 C 0.6492(7) 0.6801(8) 0.4579(2) 0.074(3) Uani 1 1 d . A . H6 H 0.7117 0.7043 0.4733 0.089 Uiso 1 1 calc R . . C7 C 0.6691(7) 0.6771(9) 0.4240(3) 0.080(3) Uani 1 1 d . . . C9 C 0.3934(8) 0.4119(8) 0.3595(3) 0.086(3) Uani 1 1 d . A . H9A H 0.4079 0.4603 0.3394 0.128 Uiso 1 1 calc R . . H9B H 0.3539 0.3303 0.3528 0.128 Uiso 1 1 calc R . . H9C H 0.4670 0.4321 0.3704 0.128 Uiso 1 1 calc R . . C10 C 0.5211(9) 0.6571(9) 0.5077(2) 0.081(3) Uani 1 1 d . A . H10A H 0.4996 0.5832 0.5187 0.121 Uiso 1 1 calc R . . H10B H 0.4590 0.6750 0.5108 0.121 Uiso 1 1 calc R . . H10C H 0.5925 0.7184 0.5179 0.121 Uiso 1 1 calc R . . C11 C 0.2959(8) 0.3656(7) 0.4170(3) 0.081(3) Uani 1 1 d . A . H11A H 0.2591 0.3918 0.4334 0.122 Uiso 1 1 calc R . . H11B H 0.3698 0.3787 0.4260 0.122 Uiso 1 1 calc R . . H11C H 0.2452 0.2829 0.4126 0.122 Uiso 1 1 calc R . . C12 C 0.7892(8) 0.7166(13) 0.4105(4) 0.146(6) Uani 1 1 d . A . H12A H 0.8292 0.8002 0.4066 0.219 Uiso 1 1 calc R . . H12B H 0.7836 0.6765 0.3893 0.219 Uiso 1 1 calc R . . H12C H 0.8326 0.6987 0.4271 0.219 Uiso 1 1 calc R . . O1S O 0.326(4) 0.655(4) 0.5671(4) 0.053(5) Uani 0.234(8) 1 d PDU B -1 C1S C 0.417(3) 0.752(3) 0.5871(8) 0.059(7) Uani 0.234(8) 1 d PDU B -1 H1S1 H 0.4059 0.8196 0.5852 0.070 Uiso 0.234(8) 1 calc PR B -1 H1S2 H 0.4935 0.7732 0.5778 0.070 Uiso 0.234(8) 1 calc PR B -1 C2S C 0.411(3) 0.717(3) 0.6266(7) 0.056(7) Uani 0.234(8) 1 d PDU B -1 H2S1 H 0.4822 0.7193 0.6352 0.067 Uiso 0.234(8) 1 calc PR B -1 H2S2 H 0.3837 0.7559 0.6421 0.067 Uiso 0.234(8) 1 calc PR B -1 C3S C 0.315(4) 0.595(4) 0.6137(9) 0.065(7) Uani 0.234(8) 1 d PDU B -1 H3S1 H 0.3498 0.5447 0.6136 0.078 Uiso 0.234(8) 1 calc PR B -1 H3S2 H 0.2537 0.5641 0.6310 0.078 Uiso 0.234(8) 1 calc PR B -1 C4S C 0.258(3) 0.580(4) 0.5807(9) 0.069(7) Uani 0.234(8) 1 d PDU B -1 H4S1 H 0.2401 0.5061 0.5699 0.083 Uiso 0.234(8) 1 calc PR B -1 H4S2 H 0.1864 0.5843 0.5827 0.083 Uiso 0.234(8) 1 calc PR B -1 O1T O 0.247(5) 0.659(6) 0.5688(15) 0.069(7) Uani 0.099(8) 1 d PDU B -2 C1T C 0.324(7) 0.717(5) 0.5984(17) 0.065(7) Uani 0.099(8) 1 d PDU B -2 H1T1 H 0.2920 0.7580 0.6118 0.078 Uiso 0.099(8) 1 calc PR B -2 H1T2 H 0.4017 0.7754 0.5905 0.078 Uiso 0.099(8) 1 calc PR B -2 C2T C 0.331(10) 0.622(8) 0.6218(14) 0.063(8) Uani 0.099(8) 1 d PDU B -2 H2T1 H 0.4102 0.6432 0.6294 0.076 Uiso 0.099(8) 1 calc PR B -2 H2T2 H 0.2746 0.5903 0.6405 0.076 Uiso 0.099(8) 1 calc PR B -2 C3T C 0.291(8) 0.549(5) 0.5882(16) 0.066(7) Uani 0.099(8) 1 d PDU B -2 H3T1 H 0.3578 0.5424 0.5802 0.079 Uiso 0.099(8) 1 calc PR B -2 H3T2 H 0.2302 0.4707 0.5946 0.079 Uiso 0.099(8) 1 calc PR B -2 C4T C 0.248(6) 0.583(7) 0.5586(13) 0.068(8) Uani 0.099(8) 1 d PDU B -2 H4T1 H 0.3005 0.6035 0.5389 0.082 Uiso 0.099(8) 1 calc PR B -2 H4T2 H 0.1694 0.5217 0.5520 0.082 Uiso 0.099(8) 1 calc PR B -2 O2S O 0.337(4) 0.594(5) 0.1534(11) 0.202(14) Uani 0.33 1 d PDU C -1 C5S C 0.394(5) 0.581(5) 0.1840(15) 0.217(15) Uani 0.33 1 d PDU C -1 H5S1 H 0.4399 0.5441 0.1777 0.260 Uiso 0.33 1 calc PR C -1 H5S2 H 0.3351 0.5311 0.2007 0.260 Uiso 0.33 1 calc PR C -1 C6S C 0.479(4) 0.707(6) 0.2006(13) 0.231(16) Uani 0.33 1 d PDU C -1 H6S1 H 0.4430 0.7308 0.2185 0.277 Uiso 0.33 1 calc PR C -1 H6S2 H 0.5563 0.7214 0.2072 0.277 Uiso 0.33 1 calc PR C -1 C7S C 0.471(4) 0.748(5) 0.1639(14) 0.205(15) Uani 0.33 1 d PDU C -1 H7S1 H 0.4777 0.8252 0.1662 0.246 Uiso 0.33 1 calc PR C -1 H7S2 H 0.5408 0.7605 0.1516 0.246 Uiso 0.33 1 calc PR C -1 C8S C 0.371(4) 0.679(7) 0.1417(12) 0.200(16) Uani 0.33 1 d PDU C -1 H8S1 H 0.3145 0.7060 0.1423 0.240 Uiso 0.33 1 calc PR C -1 H8S2 H 0.3954 0.6790 0.1180 0.240 Uiso 0.33 1 calc PR C -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 0.0343(2) 0.0343(2) 0.0581(4) 0.000 0.000 0.01713(11) Cl1 0.060(2) 0.040(2) 0.074(3) -0.0155(18) -0.0230(16) 0.0172(19) O1X 0.094(14) 0.033(11) 0.052(8) 0.006(9) -0.011(10) 0.043(10) C1X 0.066(11) 0.044(10) 0.057(8) 0.005(9) 0.002(10) 0.034(9) N1X 0.072(12) 0.084(13) 0.066(9) -0.024(11) -0.005(10) 0.051(11) N2 0.036(3) 0.032(3) 0.069(4) -0.005(2) -0.009(3) 0.023(2) C1 0.039(4) 0.035(3) 0.070(5) -0.002(3) -0.007(3) 0.021(3) C2 0.033(3) 0.032(3) 0.071(5) -0.010(3) -0.011(3) 0.016(3) C3 0.057(5) 0.048(4) 0.066(5) -0.006(3) -0.018(4) 0.030(4) C4 0.040(4) 0.077(5) 0.079(5) -0.028(4) -0.008(4) 0.036(4) C5 0.050(4) 0.045(4) 0.108(7) -0.027(4) -0.038(4) 0.028(4) C6 0.057(5) 0.085(6) 0.095(7) -0.034(5) -0.039(5) 0.047(5) C7 0.045(5) 0.101(7) 0.106(8) -0.043(6) -0.023(5) 0.045(5) C9 0.085(6) 0.076(6) 0.120(8) -0.057(6) -0.051(6) 0.059(5) C10 0.092(7) 0.080(6) 0.081(6) -0.005(5) -0.025(5) 0.052(6) C11 0.072(6) 0.047(5) 0.124(8) 0.004(5) -0.037(6) 0.029(4) C12 0.046(6) 0.205(15) 0.191(14) -0.086(12) -0.024(7) 0.066(8) O1S 0.041(10) 0.089(14) 0.032(6) 0.028(9) -0.012(9) 0.034(10) C1S 0.052(12) 0.087(14) 0.027(9) 0.021(9) 0.001(9) 0.028(10) C2S 0.048(11) 0.092(14) 0.029(8) 0.024(10) -0.007(8) 0.036(10) C3S 0.050(12) 0.097(13) 0.033(9) 0.032(9) -0.006(9) 0.026(11) C4S 0.049(11) 0.101(14) 0.036(9) 0.027(10) -0.008(9) 0.022(10) O1T 0.051(12) 0.096(15) 0.042(10) 0.023(11) -0.012(10) 0.024(12) C1T 0.050(12) 0.096(13) 0.032(10) 0.028(10) -0.006(10) 0.024(11) C2T 0.049(13) 0.095(15) 0.034(10) 0.026(11) -0.003(11) 0.028(12) C3T 0.049(13) 0.097(14) 0.035(10) 0.025(11) -0.007(11) 0.024(11) C4T 0.052(13) 0.096(15) 0.039(10) 0.025(11) -0.010(11) 0.025(12) O2S 0.13(2) 0.27(3) 0.28(3) -0.11(2) -0.058(18) 0.15(2) C5S 0.15(2) 0.28(3) 0.27(3) -0.11(3) -0.07(2) 0.14(2) C6S 0.16(2) 0.28(3) 0.27(3) -0.11(3) -0.06(2) 0.13(2) C7S 0.14(2) 0.27(3) 0.28(3) -0.12(3) -0.05(2) 0.15(2) C8S 0.12(2) 0.27(3) 0.28(3) -0.11(3) -0.050(18) 0.15(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N2 1.943(5) 3_565 ? W1 N2 1.943(5) . ? W1 N2 1.943(5) 2_665 ? W1 O1X 2.01(2) 3_565 ? W1 O1X 2.01(2) . ? W1 O1X 2.01(2) 2_665 ? W1 Cl1 2.513(4) 3_565 ? W1 Cl1 2.513(4) . ? W1 Cl1 2.513(4) 2_665 ? O1X C1X 1.35(4) . ? C1X N1X 1.11(3) . ? N2 C2 1.475(8) . ? N2 C5 1.514(8) . ? C1 C2 1.362(10) . ? C1 C3 1.386(10) . ? C2 C4 1.378(10) . ? C3 C6 1.388(11) . ? C3 C10 1.516(12) . ? C4 C7 1.413(10) . ? C5 C11 1.507(12) . ? C5 C9 1.541(12) . ? C6 C7 1.371(14) . ? C7 C12 1.513(13) . ? O1S C4S 1.10(5) . ? O1S C1S 1.49(4) . ? C1S C2S 1.62(3) . ? C2S C3S 1.57(5) . ? C3S C4S 1.48(4) . ? O1T C4T 1.10(5) . ? O1T C1T 1.49(4) . ? C1T C2T 1.62(3) . ? C2T C3T 1.57(5) . ? C3T C4T 1.48(4) . ? O2S C8S 1.09(5) . ? O2S C5S 1.49(4) . ? C5S C6S 1.63(3) . ? C6S C7S 1.57(5) . ? C7S C8S 1.48(4) . ? 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 N2 97.8(2) 3_565 . ? N2 W1 N2 97.8(2) 3_565 2_665 ? N2 W1 N2 97.8(2) . 2_665 ? N2 W1 O1X 91.4(7) 3_565 3_565 ? N2 W1 O1X 166.7(7) . 3_565 ? N2 W1 O1X 90.3(8) 2_665 3_565 ? N2 W1 O1X 90.3(8) 3_565 . ? N2 W1 O1X 91.4(7) . . ? N2 W1 O1X 166.7(7) 2_665 . ? O1X W1 O1X 79.0(10) 3_565 . ? N2 W1 O1X 166.7(7) 3_565 2_665 ? N2 W1 O1X 90.3(8) . 2_665 ? N2 W1 O1X 91.4(7) 2_665 2_665 ? O1X W1 O1X 79.0(10) 3_565 2_665 ? O1X W1 O1X 79.0(10) . 2_665 ? N2 W1 Cl1 87.2(2) 3_565 3_565 ? N2 W1 Cl1 170.1(2) . 3_565 ? N2 W1 Cl1 89.9(2) 2_665 3_565 ? O1X W1 Cl1 4.3(7) 3_565 3_565 ? O1X W1 Cl1 80.0(7) . 3_565 ? O1X W1 Cl1 83.2(8) 2_665 3_565 ? N2 W1 Cl1 89.9(2) 3_565 . ? N2 W1 Cl1 87.2(2) . . ? N2 W1 Cl1 170.1(2) 2_665 . ? O1X W1 Cl1 83.2(8) 3_565 . ? O1X W1 Cl1 4.3(8) . . ? O1X W1 Cl1 80.0(7) 2_665 . ? Cl1 W1 Cl1 84.26(19) 3_565 . ? N2 W1 Cl1 170.1(2) 3_565 2_665 ? N2 W1 Cl1 89.9(2) . 2_665 ? N2 W1 Cl1 87.2(2) 2_665 2_665 ? O1X W1 Cl1 80.0(7) 3_565 2_665 ? O1X W1 Cl1 83.2(8) . 2_665 ? O1X W1 Cl1 4.3(7) 2_665 2_665 ? Cl1 W1 Cl1 84.26(19) 3_565 2_665 ? Cl1 W1 Cl1 84.26(19) . 2_665 ? C1X O1X W1 129.3(19) . . ? N1X C1X O1X 172(3) . . ? C2 N2 C5 111.1(5) . . ? C2 N2 W1 120.1(4) . . ? C5 N2 W1 127.8(4) . . ? C2 C1 C3 120.8(7) . . ? C1 C2 C4 121.1(6) . . ? C1 C2 N2 118.9(6) . . ? C4 C2 N2 120.0(7) . . ? C1 C3 C6 118.4(7) . . ? C1 C3 C10 120.8(7) . . ? C6 C3 C10 120.8(7) . . ? C2 C4 C7 119.1(8) . . ? C11 C5 N2 112.0(7) . . ? C11 C5 C9 112.7(7) . . ? N2 C5 C9 110.3(7) . . ? C7 C6 C3 121.7(7) . . ? C6 C7 C4 118.8(8) . . ? C6 C7 C12 121.4(9) . . ? C4 C7 C12 119.8(9) . . ? C4S O1S C1S 118(2) . . ? O1S C1S C2S 111(2) . . ? C3S C2S C1S 83.0(19) . . ? C4S C3S C2S 122(3) . . ? O1S C4S C3S 100(3) . . ? C4T O1T C1T 117(3) . . ? O1T C1T C2T 109(3) . . ? C3T C2T C1T 82(2) . . ? C4T C3T C2T 123(3) . . ? O1T C4T C3T 100(3) . . ? C8S O2S C5S 119(2) . . ? O2S C5S C6S 110(2) . . ? C7S C6S C5S 82(2) . . ? C8S C7S C6S 122(3) . . ? O2S C8S C7S 100(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.017 _refine_diff_density_min -1.728 _refine_diff_density_rms 0.165 #===END data_1-(N=PCl3)(Cl)2 _database_code_depnum_ccdc_archive 'CCDC 675712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common W(N=PCl3)(Cl)2(N(i-Pr)Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H56 Cl5 N4 O P W' _chemical_formula_weight 964.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9389(6) _cell_length_b 13.7357(5) _cell_length_c 18.9527(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.4620(10) _cell_angle_gamma 90.00 _cell_volume 4114.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9852 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.20 _exptl_crystal_description shard _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 3.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7399 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81238 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.88 _reflns_number_total 9806 _reflns_number_gt 8274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT 5 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT 5 (Bruker-AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+10.0260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9806 _refine_ls_number_parameters 452 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.272681(9) 0.961980(11) 0.840279(7) 0.01476(5) Uani 1 1 d . . . Cl1 Cl 0.25289(6) 0.95449(7) 0.96762(5) 0.02131(19) Uani 1 1 d . . . P1 P 0.45052(7) 0.84239(8) 0.91526(6) 0.0243(2) Uani 1 1 d . . . N1 N 0.3074(2) 0.9721(2) 0.74546(16) 0.0174(6) Uani 1 1 d . . . Cl2 Cl 0.36966(7) 1.09443(7) 0.88235(5) 0.0253(2) Uani 1 1 d . . . N2 N 0.1976(2) 0.8495(2) 0.82163(16) 0.0176(6) Uani 1 1 d . . . Cl3 Cl 0.55021(7) 0.93081(9) 0.93566(6) 0.0317(2) Uani 1 1 d . . . N3 N 0.1819(2) 1.0614(2) 0.82633(16) 0.0172(6) Uani 1 1 d . . . Cl4 Cl 0.43472(8) 0.79403(10) 1.01260(6) 0.0390(3) Uani 1 1 d . . . N4 N 0.3755(2) 0.8750(3) 0.86996(17) 0.0239(7) Uani 1 1 d . . . Cl5 Cl 0.50256(8) 0.72499(9) 0.87295(7) 0.0412(3) Uani 1 1 d . . . C11 C 0.2748(3) 1.0481(3) 0.6960(2) 0.0203(8) Uani 1 1 d . . . C12 C 0.2125(3) 1.0256(3) 0.6395(2) 0.0258(9) Uani 1 1 d . . . H12A H 0.1926 0.9606 0.6330 0.031 Uiso 1 1 calc R . . C13 C 0.1794(3) 1.0985(4) 0.5925(2) 0.0304(10) Uani 1 1 d . . . C14 C 0.2094(3) 1.1931(4) 0.6027(2) 0.0314(10) Uani 1 1 d . . . H14A H 0.1872 1.2428 0.5708 0.038 Uiso 1 1 calc R . . C15 C 0.2712(3) 1.2163(3) 0.6587(2) 0.0277(9) Uani 1 1 d . . . C16 C 0.3044(3) 1.1426(3) 0.7047(2) 0.0223(8) Uani 1 1 d . . . H16A H 0.3478 1.1574 0.7424 0.027 Uiso 1 1 calc R . . C17 C 0.3816(2) 0.9189(3) 0.7205(2) 0.0201(8) Uani 1 1 d . . . H17A H 0.3916 0.8587 0.7501 0.024 Uiso 1 1 calc R . . C18 C 0.4616(3) 0.9810(3) 0.7342(2) 0.0289(9) Uani 1 1 d . . . H18A H 0.5090 0.9460 0.7178 0.043 Uiso 1 1 calc R . . H18B H 0.4744 0.9941 0.7853 0.043 Uiso 1 1 calc R . . H18C H 0.4526 1.0426 0.7084 0.043 Uiso 1 1 calc R . . C19 C 0.3648(3) 0.8867(3) 0.6424(2) 0.0282(9) Uani 1 1 d . . . H19A H 0.4146 0.8523 0.6296 0.042 Uiso 1 1 calc R . . H19B H 0.3535 0.9440 0.6119 0.042 Uiso 1 1 calc R . . H19C H 0.3157 0.8432 0.6359 0.042 Uiso 1 1 calc R . . C21 C 0.2009(3) 0.7915(3) 0.75737(19) 0.0188(8) Uani 1 1 d . . . C22 C 0.1379(3) 0.8017(3) 0.6993(2) 0.0208(8) Uani 1 1 d . . . H22A H 0.0929 0.8465 0.7015 0.025 Uiso 1 1 calc R . . C23 C 0.1410(3) 0.7460(3) 0.6378(2) 0.0241(8) Uani 1 1 d . . . C24 C 0.2084(3) 0.6815(3) 0.6356(2) 0.0276(9) Uani 1 1 d . . . H24A H 0.2116 0.6445 0.5937 0.033 Uiso 1 1 calc R . . C25 C 0.2713(3) 0.6701(3) 0.6936(2) 0.0252(9) Uani 1 1 d . . . C26 C 0.2664(3) 0.7255(3) 0.7549(2) 0.0214(8) Uani 1 1 d . . . H26A H 0.3081 0.7178 0.7951 0.026 Uiso 1 1 calc R . . C27 C 0.1469(2) 0.7990(3) 0.8733(2) 0.0209(8) Uani 1 1 d . . . H27A H 0.1354 0.8480 0.9099 0.025 Uiso 1 1 calc R . . C28 C 0.0617(3) 0.7613(3) 0.8380(2) 0.0246(8) Uani 1 1 d . . . H28A H 0.0292 0.8152 0.8142 0.037 Uiso 1 1 calc R . . H28B H 0.0304 0.7331 0.8743 0.037 Uiso 1 1 calc R . . H28C H 0.0709 0.7113 0.8029 0.037 Uiso 1 1 calc R . . C29 C 0.2003(3) 0.7179(3) 0.9117(2) 0.0259(9) Uani 1 1 d . . . H29A H 0.2543 0.7448 0.9340 0.039 Uiso 1 1 calc R . . H29B H 0.2111 0.6675 0.8773 0.039 Uiso 1 1 calc R . . H29C H 0.1699 0.6892 0.9483 0.039 Uiso 1 1 calc R . . C31 C 0.0932(2) 1.0313(3) 0.8145(2) 0.0189(7) Uani 1 1 d . . . C32 C 0.0487(3) 1.0140(3) 0.8717(2) 0.0217(8) Uani 1 1 d . . . H32A H 0.0768 1.0189 0.9189 0.026 Uiso 1 1 calc R . . C33 C -0.0371(3) 0.9893(3) 0.8599(2) 0.0234(8) Uani 1 1 d . . . C34 C -0.0766(3) 0.9829(3) 0.7907(2) 0.0244(9) Uani 1 1 d . . . H34A H -0.1352 0.9677 0.7825 0.029 Uiso 1 1 calc R . . C35 C -0.0328(3) 0.9982(3) 0.7326(2) 0.0232(8) Uani 1 1 d . . . C36 C 0.0522(3) 1.0232(3) 0.7455(2) 0.0217(8) Uani 1 1 d . . . H36A H 0.0828 1.0349 0.7065 0.026 Uiso 1 1 calc R . . C37 C 0.1887(3) 1.1706(3) 0.8376(2) 0.0212(8) Uani 1 1 d . . . H37A H 0.2466 1.1906 0.8284 0.025 Uiso 1 1 calc R . . C38 C 0.1809(3) 1.1963(3) 0.9151(2) 0.0269(9) Uani 1 1 d . . . H38A H 0.2215 1.1577 0.9468 0.040 Uiso 1 1 calc R . . H38B H 0.1233 1.1820 0.9250 0.040 Uiso 1 1 calc R . . H38C H 0.1928 1.2657 0.9230 0.040 Uiso 1 1 calc R . . C39 C 0.1256(3) 1.2273(3) 0.7862(2) 0.0270(9) Uani 1 1 d . . . H39A H 0.1317 1.2085 0.7372 0.041 Uiso 1 1 calc R . . H39B H 0.1364 1.2972 0.7924 0.041 Uiso 1 1 calc R . . H39C H 0.0679 1.2126 0.7958 0.041 Uiso 1 1 calc R . . C131 C 0.1119(4) 1.0741(5) 0.5317(3) 0.0454(13) Uani 1 1 d . . . H13A H 0.0970 1.1328 0.5035 0.068 Uiso 1 1 calc R . . H13B H 0.0617 1.0494 0.5506 0.068 Uiso 1 1 calc R . . H13C H 0.1333 1.0244 0.5016 0.068 Uiso 1 1 calc R . . C151 C 0.2985(3) 1.3206(4) 0.6717(3) 0.0393(12) Uani 1 1 d . . . H15A H 0.3424 1.3238 0.7130 0.059 Uiso 1 1 calc R . . H15B H 0.2498 1.3599 0.6809 0.059 Uiso 1 1 calc R . . H15C H 0.3212 1.3459 0.6296 0.059 Uiso 1 1 calc R . . C231 C 0.0728(3) 0.7560(4) 0.5756(2) 0.0320(10) Uani 1 1 d . . . H23A H 0.0847 0.7120 0.5374 0.048 Uiso 1 1 calc R . . H23B H 0.0711 0.8233 0.5582 0.048 Uiso 1 1 calc R . . H23C H 0.0180 0.7392 0.5905 0.048 Uiso 1 1 calc R . . C251 C 0.3438(3) 0.6012(4) 0.6896(3) 0.0372(11) Uani 1 1 d . . . H25A H 0.3380 0.5708 0.6424 0.056 Uiso 1 1 calc R . . H25B H 0.3433 0.5506 0.7260 0.056 Uiso 1 1 calc R . . H25C H 0.3973 0.6371 0.6976 0.056 Uiso 1 1 calc R . . C331 C -0.0842(3) 0.9664(4) 0.9218(2) 0.0302(10) Uani 1 1 d . . . H33A H -0.1434 0.9518 0.9043 0.045 Uiso 1 1 calc R . . H33B H -0.0817 1.0227 0.9539 0.045 Uiso 1 1 calc R . . H33C H -0.0582 0.9100 0.9477 0.045 Uiso 1 1 calc R . . C351 C -0.0756(3) 0.9867(3) 0.6573(2) 0.0312(10) Uani 1 1 d . . . H35A H -0.0351 1.0011 0.6240 0.047 Uiso 1 1 calc R . . H35B H -0.1235 1.0318 0.6489 0.047 Uiso 1 1 calc R . . H35C H -0.0960 0.9197 0.6500 0.047 Uiso 1 1 calc R . . O1S O 0.3256(4) 1.3995(4) 0.8634(3) 0.0927(18) Uani 1 1 d DU . . C1S C 0.3285(6) 1.4977(5) 0.8729(4) 0.045(2) Uani 0.745(19) 1 d PDU A 1 H1S1 H 0.2763 1.5284 0.8487 0.054 Uiso 0.745(19) 1 calc PR A 1 H1S2 H 0.3778 1.5257 0.8531 0.054 Uiso 0.745(19) 1 calc PR A 1 C1SA C 0.2806(15) 1.472(2) 0.8931(14) 0.064(8) Uani 0.255(19) 1 d PDU A 2 H1S3 H 0.2297 1.4449 0.9105 0.077 Uiso 0.255(19) 1 calc PR A 2 H1S4 H 0.2624 1.5230 0.8571 0.077 Uiso 0.255(19) 1 calc PR A 2 C2S C 0.3362(6) 1.5144(5) 0.9515(4) 0.081(2) Uani 1 1 d DU . . H2SA H 0.2800 1.5248 0.9670 0.097 Uiso 0.745(19) 1 calc PR A 1 H2SB H 0.3725 1.5715 0.9654 0.097 Uiso 0.745(19) 1 calc PR A 1 H2SC H 0.3045 1.5492 0.9853 0.097 Uiso 0.255(19) 1 calc PR A 2 H2SD H 0.3784 1.5587 0.9347 0.097 Uiso 0.255(19) 1 calc PR A 2 C3S C 0.3763(6) 1.4224(6) 0.9830(4) 0.088(3) Uani 1 1 d DU A . H3S1 H 0.4330 1.4357 1.0092 0.106 Uiso 1 1 calc R . . H3S2 H 0.3406 1.3919 1.0159 0.106 Uiso 1 1 calc R . . C4S C 0.3823(5) 1.3603(5) 0.9217(5) 0.089(3) Uani 1 1 d DU A . H4S1 H 0.4410 1.3599 0.9099 0.107 Uiso 1 1 calc R . . H4S2 H 0.3660 1.2928 0.9320 0.107 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 0.01609(8) 0.01667(8) 0.01150(8) -0.00021(5) 0.00170(5) 0.00014(6) Cl1 0.0238(5) 0.0269(5) 0.0135(4) 0.0000(3) 0.0035(3) 0.0005(4) P1 0.0253(5) 0.0249(5) 0.0223(5) 0.0003(4) 0.0017(4) 0.0023(4) N1 0.0207(16) 0.0177(16) 0.0140(14) 0.0001(12) 0.0036(12) -0.0008(12) Cl2 0.0274(5) 0.0248(5) 0.0231(5) -0.0024(4) 0.0007(4) -0.0020(4) N2 0.0201(16) 0.0184(16) 0.0146(14) -0.0001(12) 0.0036(12) -0.0008(13) Cl3 0.0251(5) 0.0382(6) 0.0311(5) -0.0046(5) 0.0017(4) -0.0023(4) N3 0.0197(16) 0.0210(16) 0.0109(14) -0.0010(12) 0.0017(12) 0.0001(12) Cl4 0.0388(6) 0.0490(7) 0.0279(5) 0.0140(5) -0.0012(5) -0.0005(5) N4 0.034(2) 0.0263(18) 0.0137(15) -0.0062(13) 0.0124(14) -0.0143(15) Cl5 0.0391(7) 0.0333(6) 0.0494(7) -0.0094(5) -0.0015(5) 0.0133(5) C11 0.0215(19) 0.026(2) 0.0149(17) 0.0023(15) 0.0059(15) 0.0022(16) C12 0.031(2) 0.030(2) 0.0167(18) 0.0036(16) 0.0046(16) -0.0052(18) C13 0.034(2) 0.039(3) 0.0174(19) 0.0064(18) 0.0027(17) -0.003(2) C14 0.036(3) 0.037(3) 0.023(2) 0.0119(18) 0.0088(18) 0.005(2) C15 0.036(2) 0.025(2) 0.026(2) 0.0047(17) 0.0137(18) 0.0012(18) C16 0.026(2) 0.025(2) 0.0157(17) 0.0001(15) 0.0051(15) -0.0016(16) C17 0.0214(19) 0.0219(19) 0.0178(18) -0.0006(15) 0.0057(15) 0.0021(16) C18 0.021(2) 0.034(2) 0.033(2) -0.0018(18) 0.0066(18) -0.0025(18) C19 0.033(2) 0.032(2) 0.0213(19) -0.0046(17) 0.0098(17) -0.0016(19) C21 0.0235(19) 0.0188(18) 0.0149(17) -0.0018(14) 0.0052(15) -0.0040(15) C22 0.0201(19) 0.0205(19) 0.0225(19) 0.0001(15) 0.0054(15) -0.0026(15) C23 0.026(2) 0.027(2) 0.0200(19) -0.0028(16) 0.0046(16) -0.0108(17) C24 0.033(2) 0.027(2) 0.025(2) -0.0073(17) 0.0092(17) -0.0071(18) C25 0.030(2) 0.0191(19) 0.028(2) -0.0032(16) 0.0081(17) 0.0004(17) C26 0.022(2) 0.0217(19) 0.0205(19) 0.0004(15) 0.0030(15) 0.0002(16) C27 0.022(2) 0.0225(19) 0.0196(18) 0.0000(15) 0.0072(15) -0.0025(16) C28 0.026(2) 0.023(2) 0.026(2) 0.0036(16) 0.0091(17) -0.0038(17) C29 0.031(2) 0.025(2) 0.0224(19) 0.0059(16) 0.0053(17) 0.0004(18) C31 0.0203(19) 0.0163(18) 0.0199(18) 0.0003(14) 0.0019(15) 0.0026(15) C32 0.021(2) 0.024(2) 0.0206(19) -0.0020(15) 0.0023(15) 0.0026(15) C33 0.020(2) 0.026(2) 0.026(2) 0.0004(16) 0.0064(16) 0.0016(16) C34 0.0175(19) 0.023(2) 0.033(2) -0.0034(17) 0.0021(16) 0.0016(15) C35 0.023(2) 0.0209(19) 0.024(2) -0.0018(16) -0.0032(16) 0.0047(16) C36 0.025(2) 0.023(2) 0.0175(18) 0.0008(15) 0.0013(15) 0.0054(16) C37 0.024(2) 0.0178(18) 0.0214(19) -0.0023(15) 0.0006(15) 0.0018(15) C38 0.033(2) 0.026(2) 0.023(2) -0.0068(17) 0.0070(17) 0.0014(18) C39 0.032(2) 0.024(2) 0.026(2) 0.0015(17) 0.0068(18) 0.0056(18) C131 0.046(3) 0.060(3) 0.026(2) 0.014(2) -0.009(2) -0.005(3) C151 0.049(3) 0.028(2) 0.043(3) 0.007(2) 0.016(2) 0.001(2) C231 0.032(2) 0.044(3) 0.019(2) -0.0066(18) -0.0009(17) -0.007(2) C251 0.039(3) 0.032(3) 0.042(3) -0.011(2) 0.010(2) 0.010(2) C331 0.023(2) 0.041(3) 0.028(2) -0.0011(19) 0.0078(17) -0.0032(19) C351 0.033(2) 0.031(2) 0.026(2) 0.0017(18) -0.0089(19) -0.0014(19) O1S 0.102(4) 0.086(4) 0.083(4) -0.020(3) -0.015(3) 0.014(3) C1S 0.051(6) 0.045(4) 0.040(4) 0.013(3) 0.006(3) 0.008(4) C1SA 0.044(13) 0.081(15) 0.063(13) -0.012(10) -0.013(9) 0.022(10) C2S 0.121(7) 0.060(4) 0.055(4) -0.005(3) -0.017(4) 0.028(4) C3S 0.122(7) 0.084(5) 0.057(4) 0.020(4) 0.007(4) 0.051(5) C4S 0.084(6) 0.051(4) 0.122(7) -0.005(4) -0.026(5) 0.025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N1 1.953(3) . ? W1 N2 1.959(3) . ? W1 N3 1.982(3) . ? W1 N4 2.047(4) . ? W1 Cl2 2.4525(10) . ? W1 Cl1 2.4764(9) . ? P1 N4 1.449(4) . ? P1 Cl3 1.9975(16) . ? P1 Cl4 2.0072(16) . ? P1 Cl5 2.0259(16) . ? N1 C11 1.453(5) . ? N1 C17 1.518(5) . ? N2 C21 1.461(5) . ? N2 C27 1.516(5) . ? N3 C31 1.462(5) . ? N3 C37 1.518(5) . ? C11 C16 1.384(6) . ? C11 C12 1.398(6) . ? C12 C13 1.397(6) . ? C13 C14 1.389(7) . ? C13 C131 1.507(6) . ? C14 C15 1.387(7) . ? C15 C16 1.395(6) . ? C15 C151 1.509(6) . ? C17 C18 1.527(6) . ? C17 C19 1.534(5) . ? C21 C26 1.389(6) . ? C21 C22 1.396(5) . ? C22 C23 1.400(5) . ? C23 C24 1.398(6) . ? C23 C231 1.504(6) . ? C24 C25 1.397(6) . ? C25 C26 1.399(5) . ? C25 C251 1.504(6) . ? C27 C28 1.524(6) . ? C27 C29 1.528(6) . ? C31 C36 1.388(5) . ? C31 C32 1.391(6) . ? C32 C33 1.399(6) . ? C33 C34 1.381(6) . ? C33 C331 1.507(6) . ? C34 C35 1.395(6) . ? C35 C36 1.388(6) . ? C35 C351 1.509(6) . ? C37 C39 1.521(6) . ? C37 C38 1.531(5) . ? O1S C1S 1.360(9) . ? O1S C1SA 1.393(15) . ? O1S C4S 1.438(8) . ? C1S C2S 1.497(9) . ? C1SA C2S 1.444(15) . ? C2S C3S 1.503(10) . ? C3S C4S 1.454(10) . ? 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 97.45(13) . . ? N1 W1 N3 96.74(13) . . ? N2 W1 N3 95.80(14) . . ? N1 W1 N4 88.97(13) . . ? N2 W1 N4 92.17(13) . . ? N3 W1 N4 169.50(13) . . ? N1 W1 Cl2 90.26(10) . . ? N2 W1 Cl2 171.34(9) . . ? N3 W1 Cl2 87.18(10) . . ? N4 W1 Cl2 83.98(10) . . ? N1 W1 Cl1 170.76(10) . . ? N2 W1 Cl1 89.48(9) . . ? N3 W1 Cl1 88.59(9) . . ? N4 W1 Cl1 84.65(9) . . ? Cl2 W1 Cl1 82.45(3) . . ? N4 P1 Cl3 120.05(15) . . ? N4 P1 Cl4 117.04(14) . . ? Cl3 P1 Cl4 102.41(7) . . ? N4 P1 Cl5 111.11(15) . . ? Cl3 P1 Cl5 101.78(7) . . ? Cl4 P1 Cl5 101.95(7) . . ? C11 N1 C17 111.9(3) . . ? C11 N1 W1 121.6(2) . . ? C17 N1 W1 125.3(2) . . ? C21 N2 C27 111.7(3) . . ? C21 N2 W1 119.5(2) . . ? C27 N2 W1 127.5(2) . . ? C31 N3 C37 110.5(3) . . ? C31 N3 W1 120.0(2) . . ? C37 N3 W1 128.7(3) . . ? P1 N4 W1 155.9(2) . . ? C16 C11 C12 119.7(4) . . ? C16 C11 N1 120.7(4) . . ? C12 C11 N1 119.7(4) . . ? C13 C12 C11 120.2(4) . . ? C14 C13 C12 119.0(4) . . ? C14 C13 C131 120.9(4) . . ? C12 C13 C131 120.1(4) . . ? C15 C14 C13 121.3(4) . . ? C14 C15 C16 119.0(4) . . ? C14 C15 C151 120.3(4) . . ? C16 C15 C151 120.6(4) . . ? C11 C16 C15 120.7(4) . . ? N1 C17 C18 110.2(3) . . ? N1 C17 C19 113.2(3) . . ? C18 C17 C19 111.2(3) . . ? C26 C21 C22 120.3(4) . . ? C26 C21 N2 119.5(3) . . ? C22 C21 N2 120.2(3) . . ? C21 C22 C23 120.1(4) . . ? C24 C23 C22 118.8(4) . . ? C24 C23 C231 121.0(4) . . ? C22 C23 C231 120.2(4) . . ? C25 C24 C23 121.5(4) . . ? C24 C25 C26 118.8(4) . . ? C24 C25 C251 120.5(4) . . ? C26 C25 C251 120.7(4) . . ? C21 C26 C25 120.4(4) . . ? N2 C27 C28 113.0(3) . . ? N2 C27 C29 109.2(3) . . ? C28 C27 C29 111.7(3) . . ? C36 C31 C32 119.7(4) . . ? C36 C31 N3 119.7(3) . . ? C32 C31 N3 120.6(3) . . ? C31 C32 C33 120.3(4) . . ? C34 C33 C32 118.8(4) . . ? C34 C33 C331 121.0(4) . . ? C32 C33 C331 120.1(4) . . ? C33 C34 C35 121.8(4) . . ? C36 C35 C34 118.4(4) . . ? C36 C35 C351 120.2(4) . . ? C34 C35 C351 121.3(4) . . ? C35 C36 C31 121.0(4) . . ? N3 C37 C39 112.8(3) . . ? N3 C37 C38 110.5(3) . . ? C39 C37 C38 111.5(3) . . ? C1S O1S C1SA 40.9(14) . . ? C1S O1S C4S 105.2(6) . . ? C1SA O1S C4S 105.3(10) . . ? O1S C1S C2S 106.2(6) . . ? O1S C1SA C2S 107.4(11) . . ? C1SA C2S C1S 38.1(14) . . ? C1SA C2S C3S 99.0(11) . . ? C1S C2S C3S 104.1(6) . . ? C4S C3S C2S 104.1(5) . . ? O1S C4S C3S 107.1(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.006 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.140 #===END data_1-(Cl)3 _database_code_depnum_ccdc_archive 'CCDC 675713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common W(Cl)3(N(i-Pr)Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.50 H49 Cl4 N3 W' _chemical_formula_weight 819.41 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7751(3) _cell_length_b 13.3987(3) _cell_length_c 13.5032(4) _cell_angle_alpha 88.8520(10) _cell_angle_beta 71.9870(10) _cell_angle_gamma 83.6570(10) _cell_volume 1842.38(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9584 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description shard _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 3.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6626 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details sadabs _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38272 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9143 _reflns_number_gt 8491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT 5 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT 5 (Bruker-AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+3.3330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9143 _refine_ls_number_parameters 406 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.869777(12) 0.756930(10) 0.667884(11) 0.01664(5) Uani 1 1 d . . . Cl1 Cl 1.03655(8) 0.64904(6) 0.53902(7) 0.02066(16) Uani 1 1 d . . . N1 N 0.7641(3) 0.8506(2) 0.7783(3) 0.0223(6) Uani 1 1 d . . . Cl2 Cl 1.00856(9) 0.70259(7) 0.77656(7) 0.02531(18) Uani 1 1 d . . . N2 N 0.7701(3) 0.6421(2) 0.7127(2) 0.0188(6) Uani 1 1 d . . . Cl3 Cl 1.02872(9) 0.87806(7) 0.60610(8) 0.02455(18) Uani 1 1 d . . . N3 N 0.7883(3) 0.8039(2) 0.5623(2) 0.0174(6) Uani 1 1 d . . . C11 C 0.6753(4) 0.9329(3) 0.7577(3) 0.0230(7) Uani 1 1 d . . . C12 C 0.7209(4) 1.0238(3) 0.7224(3) 0.0255(8) Uani 1 1 d . . . H12 H 0.8115 1.0315 0.7067 0.031 Uiso 1 1 calc R . . C13 C 0.6323(4) 1.1046(3) 0.7098(3) 0.0275(8) Uani 1 1 d . . . C14 C 0.5014(4) 1.0909(3) 0.7315(3) 0.0282(8) Uani 1 1 d . . . H14 H 0.4416 1.1454 0.7226 0.034 Uiso 1 1 calc R . . C15 C 0.4545(4) 0.9992(3) 0.7660(3) 0.0268(8) Uani 1 1 d . . . C16 C 0.5427(4) 0.9198(3) 0.7799(3) 0.0253(8) Uani 1 1 d . . . H16 H 0.5126 0.8570 0.8043 0.030 Uiso 1 1 calc R . . C17 C 0.7768(4) 0.8616(3) 0.8862(3) 0.0304(9) Uani 1 1 d . . . H17 H 0.8158 0.7953 0.9044 0.036 Uiso 1 1 calc R . . C18 C 0.8706(5) 0.9383(4) 0.8866(4) 0.0411(11) Uani 1 1 d . . . H18A H 0.9548 0.9199 0.8330 0.062 Uiso 1 1 calc R . . H18B H 0.8843 0.9393 0.9550 0.062 Uiso 1 1 calc R . . H18C H 0.8332 1.0049 0.8722 0.062 Uiso 1 1 calc R . . C19 C 0.6442(5) 0.8870(4) 0.9684(3) 0.0389(11) Uani 1 1 d . . . H19A H 0.5861 0.8363 0.9662 0.058 Uiso 1 1 calc R . . H19B H 0.6051 0.9532 0.9546 0.058 Uiso 1 1 calc R . . H19C H 0.6562 0.8877 1.0374 0.058 Uiso 1 1 calc R . . C21 C 0.6656(4) 0.6446(3) 0.8112(3) 0.0245(8) Uani 1 1 d . . . C22 C 0.6945(4) 0.6264(3) 0.9033(3) 0.0302(9) Uani 1 1 d . . . H22 H 0.7834 0.6138 0.9025 0.036 Uiso 1 1 calc R . . C23 C 0.5932(5) 0.6265(4) 0.9978(4) 0.0405(11) Uani 1 1 d . . . C24 C 0.4637(5) 0.6447(4) 0.9970(4) 0.0459(13) Uani 1 1 d . . . H24 H 0.3946 0.6448 1.0609 0.055 Uiso 1 1 calc R . . C25 C 0.4326(5) 0.6629(4) 0.9047(4) 0.0452(13) Uani 1 1 d . . . C26 C 0.5354(4) 0.6630(3) 0.8118(4) 0.0318(9) Uani 1 1 d . . . H26 H 0.5166 0.6757 0.7481 0.038 Uiso 1 1 calc R . . C27 C 0.8006(4) 0.5369(3) 0.6651(3) 0.0218(7) Uani 1 1 d . . . H27 H 0.8589 0.5419 0.5919 0.026 Uiso 1 1 calc R . . C28 C 0.6801(4) 0.4916(3) 0.6603(3) 0.0277(8) Uani 1 1 d . . . H28A H 0.6327 0.5367 0.6229 0.042 Uiso 1 1 calc R . . H28B H 0.6227 0.4822 0.7312 0.042 Uiso 1 1 calc R . . H28C H 0.7067 0.4265 0.6238 0.042 Uiso 1 1 calc R . . C29 C 0.8773(4) 0.4687(3) 0.7230(3) 0.0273(8) Uani 1 1 d . . . H29A H 0.9547 0.4997 0.7250 0.041 Uiso 1 1 calc R . . H29B H 0.9052 0.4035 0.6869 0.041 Uiso 1 1 calc R . . H29C H 0.8212 0.4592 0.7943 0.041 Uiso 1 1 calc R . . C31 C 0.7030(3) 0.7424(3) 0.5310(3) 0.0183(7) Uani 1 1 d . . . C32 C 0.5677(3) 0.7641(3) 0.5722(3) 0.0201(7) Uani 1 1 d . . . H32 H 0.5322 0.8167 0.6224 0.024 Uiso 1 1 calc R . . C33 C 0.4838(4) 0.7095(3) 0.5404(3) 0.0219(7) Uani 1 1 d . . . C34 C 0.5381(4) 0.6341(3) 0.4656(3) 0.0236(7) Uani 1 1 d . . . H34 H 0.4814 0.5967 0.4433 0.028 Uiso 1 1 calc R . . C35 C 0.6734(4) 0.6120(3) 0.4222(3) 0.0217(7) Uani 1 1 d . . . C36 C 0.7568(3) 0.6668(3) 0.4562(3) 0.0197(7) Uani 1 1 d . . . H36 H 0.8494 0.6522 0.4282 0.024 Uiso 1 1 calc R . . C37 C 0.8169(4) 0.8934(3) 0.4926(3) 0.0203(7) Uani 1 1 d . . . H37 H 0.8591 0.9400 0.5259 0.024 Uiso 1 1 calc R . . C38 C 0.6932(4) 0.9515(3) 0.4792(3) 0.0247(8) Uani 1 1 d . . . H38A H 0.6320 0.9720 0.5478 0.037 Uiso 1 1 calc R . . H38B H 0.6516 0.9085 0.4439 0.037 Uiso 1 1 calc R . . H38C H 0.7166 1.0112 0.4375 0.037 Uiso 1 1 calc R . . C39 C 0.9155(4) 0.8597(3) 0.3873(3) 0.0279(8) Uani 1 1 d . . . H39A H 0.9937 0.8227 0.3983 0.042 Uiso 1 1 calc R . . H39B H 0.9406 0.9188 0.3449 0.042 Uiso 1 1 calc R . . H39C H 0.8755 0.8161 0.3513 0.042 Uiso 1 1 calc R . . C131 C 0.6826(5) 1.2044(3) 0.6741(4) 0.0362(10) Uani 1 1 d . . . H13A H 0.6112 1.2512 0.6637 0.054 Uiso 1 1 calc R . . H13B H 0.7544 1.1948 0.6084 0.054 Uiso 1 1 calc R . . H13C H 0.7146 1.2320 0.7271 0.054 Uiso 1 1 calc R . . C151 C 0.3105(4) 0.9847(4) 0.7910(4) 0.0339(9) Uani 1 1 d . . . H15A H 0.2616 1.0475 0.7791 0.051 Uiso 1 1 calc R . . H15B H 0.2759 0.9658 0.8641 0.051 Uiso 1 1 calc R . . H15C H 0.3010 0.9315 0.7460 0.051 Uiso 1 1 calc R . . C231 C 0.6238(6) 0.6078(5) 1.0996(4) 0.0562(15) Uani 1 1 d . . . H23A H 0.5875 0.6662 1.1462 0.084 Uiso 1 1 calc R . . H23B H 0.7191 0.5970 1.0856 0.084 Uiso 1 1 calc R . . H23C H 0.5844 0.5482 1.1326 0.084 Uiso 1 1 calc R . . C251 C 0.2930(5) 0.6816(6) 0.9027(6) 0.072(2) Uani 1 1 d . . . H25A H 0.2691 0.7539 0.8984 0.109 Uiso 1 1 calc R . . H25B H 0.2343 0.6558 0.9665 0.109 Uiso 1 1 calc R . . H25C H 0.2847 0.6472 0.8421 0.109 Uiso 1 1 calc R . . C331 C 0.3373(4) 0.7333(3) 0.5878(4) 0.0317(9) Uani 1 1 d . . . H33A H 0.2923 0.6948 0.5512 0.048 Uiso 1 1 calc R . . H33B H 0.3129 0.8053 0.5815 0.048 Uiso 1 1 calc R . . H33C H 0.3116 0.7154 0.6616 0.048 Uiso 1 1 calc R . . C351 C 0.7309(4) 0.5302(3) 0.3411(3) 0.0277(8) Uani 1 1 d . . . H35A H 0.6599 0.4965 0.3300 0.042 Uiso 1 1 calc R . . H35B H 0.7897 0.4813 0.3649 0.042 Uiso 1 1 calc R . . H35C H 0.7804 0.5595 0.2757 0.042 Uiso 1 1 calc R . . C1W C 0.0354(3) 0.3488(2) 0.95709(19) 0.017(2) Uani 0.25 1 d PDU A -1 H1W1 H -0.0260 0.3256 1.0220 0.021 Uiso 0.25 1 calc PR A -1 H1W2 H 0.1237 0.3376 0.9660 0.021 Uiso 0.25 1 calc PR A -1 Cl1W Cl 0.0040(3) 0.4589(2) 0.95859(19) 0.0424(10) Uani 0.25 1 d PRDU A -1 Cl2W Cl 0.0384(3) 0.2594(2) 0.85705(19) 0.0696(18) Uani 0.25 1 d PRDU A -1 C1Z C 0.0166(3) 0.1860(2) 0.90855(19) 0.035(3) Uani 0.25 1 d PRDU A -2 H1Z1 H -0.0145 0.1979 0.9848 0.042 Uiso 0.25 1 calc PR A -2 H1Z2 H 0.0406 0.1127 0.8969 0.042 Uiso 0.25 1 calc PR A -2 Cl1Z Cl -0.1267(3) 0.2225(2) 0.85865(19) 0.0433(11) Uani 0.25 1 d PRDU A -2 Cl2Z Cl 0.1521(3) 0.2408(2) 0.86085(19) 0.0495(12) Uani 0.25 1 d PRDU A -2 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 0.01151(7) 0.01868(8) 0.02006(8) -0.00353(5) -0.00547(5) -0.00061(5) Cl1 0.0131(4) 0.0227(4) 0.0249(4) -0.0058(3) -0.0039(3) -0.0009(3) N1 0.0198(15) 0.0248(15) 0.0222(15) -0.0065(12) -0.0076(12) 0.0021(12) Cl2 0.0188(4) 0.0321(5) 0.0270(4) -0.0059(4) -0.0115(3) 0.0028(3) N2 0.0143(14) 0.0219(14) 0.0204(14) -0.0025(11) -0.0060(11) -0.0004(11) Cl3 0.0161(4) 0.0227(4) 0.0363(5) -0.0042(3) -0.0090(4) -0.0044(3) N3 0.0128(13) 0.0196(14) 0.0192(14) -0.0025(11) -0.0033(11) -0.0027(10) C11 0.0216(18) 0.0245(18) 0.0221(18) -0.0072(14) -0.0076(14) 0.0051(14) C12 0.0224(18) 0.0263(18) 0.0271(19) -0.0083(15) -0.0073(15) 0.0012(14) C13 0.031(2) 0.0262(19) 0.0242(19) -0.0057(15) -0.0087(16) 0.0035(15) C14 0.026(2) 0.031(2) 0.0261(19) -0.0076(16) -0.0101(16) 0.0094(16) C15 0.0211(19) 0.035(2) 0.0220(18) -0.0093(15) -0.0064(15) 0.0059(15) C16 0.0223(19) 0.0294(19) 0.0234(18) -0.0059(15) -0.0073(15) 0.0022(15) C17 0.030(2) 0.037(2) 0.0241(19) -0.0104(16) -0.0122(16) 0.0086(17) C18 0.047(3) 0.043(3) 0.041(3) -0.017(2) -0.026(2) 0.001(2) C19 0.038(3) 0.051(3) 0.023(2) -0.0129(19) -0.0095(18) 0.016(2) C21 0.0196(18) 0.0243(18) 0.0251(19) -0.0010(14) -0.0011(15) 0.0001(14) C22 0.024(2) 0.037(2) 0.025(2) -0.0023(16) -0.0028(16) 0.0004(16) C23 0.039(3) 0.048(3) 0.026(2) 0.0023(19) 0.0008(19) 0.000(2) C24 0.026(2) 0.060(3) 0.036(3) 0.007(2) 0.0098(19) 0.004(2) C25 0.022(2) 0.053(3) 0.048(3) 0.013(2) 0.005(2) 0.001(2) C26 0.0191(19) 0.034(2) 0.038(2) 0.0082(18) -0.0032(17) -0.0007(16) C27 0.0173(17) 0.0209(17) 0.0264(18) -0.0023(14) -0.0057(14) -0.0019(13) C28 0.0238(19) 0.0244(18) 0.037(2) 0.0017(16) -0.0105(17) -0.0080(15) C29 0.026(2) 0.0247(18) 0.030(2) -0.0001(15) -0.0089(16) 0.0035(15) C31 0.0167(16) 0.0190(16) 0.0208(17) 0.0002(13) -0.0072(13) -0.0049(12) C32 0.0151(16) 0.0190(16) 0.0265(18) -0.0008(13) -0.0064(14) -0.0024(12) C33 0.0155(16) 0.0204(16) 0.0313(19) 0.0016(14) -0.0095(14) -0.0025(13) C34 0.0223(18) 0.0187(16) 0.036(2) 0.0016(15) -0.0170(16) -0.0056(13) C35 0.0231(18) 0.0177(16) 0.0270(18) -0.0013(13) -0.0118(15) -0.0016(13) C36 0.0147(16) 0.0202(16) 0.0248(18) -0.0025(13) -0.0072(13) -0.0004(12) C37 0.0181(16) 0.0204(16) 0.0229(17) -0.0004(13) -0.0061(14) -0.0048(13) C38 0.0263(19) 0.0217(17) 0.0285(19) 0.0032(14) -0.0117(16) -0.0044(14) C39 0.026(2) 0.0280(19) 0.0265(19) -0.0016(15) -0.0025(16) -0.0074(15) C131 0.039(2) 0.027(2) 0.043(3) 0.0010(18) -0.015(2) 0.0019(18) C151 0.022(2) 0.046(3) 0.032(2) -0.0065(19) -0.0076(17) 0.0039(17) C231 0.051(3) 0.085(4) 0.024(2) 0.003(3) -0.001(2) -0.003(3) C251 0.016(2) 0.113(6) 0.072(4) 0.037(4) 0.005(2) 0.002(3) C331 0.0171(18) 0.028(2) 0.052(3) -0.0020(18) -0.0130(18) -0.0021(15) C351 0.029(2) 0.0241(18) 0.034(2) -0.0079(16) -0.0159(17) -0.0018(15) C1W 0.002(4) 0.045(5) 0.006(4) -0.002(4) -0.002(4) -0.003(4) Cl1W 0.027(2) 0.057(3) 0.041(2) 0.006(2) -0.0093(18) -0.0014(19) Cl2W 0.085(5) 0.084(4) 0.031(3) -0.001(3) -0.010(3) 0.004(4) C1Z 0.058(6) 0.024(5) 0.018(5) -0.001(4) -0.013(5) 0.023(5) Cl1Z 0.049(3) 0.043(2) 0.031(2) -0.0107(18) -0.0080(19) 0.015(2) Cl2Z 0.066(3) 0.047(3) 0.043(3) -0.012(2) -0.032(3) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N1 1.950(3) . ? W1 N2 1.953(3) . ? W1 N3 1.953(3) . ? W1 Cl3 2.4371(9) . ? W1 Cl1 2.4371(8) . ? W1 Cl2 2.4482(9) . ? N1 C11 1.459(5) . ? N1 C17 1.517(5) . ? N2 C21 1.452(5) . ? N2 C27 1.520(5) . ? N3 C31 1.458(4) . ? N3 C37 1.509(5) . ? C11 C12 1.384(6) . ? C11 C16 1.396(5) . ? C12 C13 1.406(5) . ? C13 C14 1.382(6) . ? C13 C131 1.513(6) . ? C14 C15 1.396(6) . ? C15 C16 1.397(5) . ? C15 C151 1.516(6) . ? C17 C18 1.520(7) . ? C17 C19 1.522(6) . ? C21 C22 1.384(6) . ? C21 C26 1.395(6) . ? C22 C23 1.399(6) . ? C23 C24 1.393(7) . ? C23 C231 1.520(7) . ? C24 C25 1.397(8) . ? C25 C26 1.393(6) . ? C25 C251 1.506(7) . ? C27 C28 1.512(5) . ? C27 C29 1.527(5) . ? C31 C36 1.390(5) . ? C31 C32 1.390(5) . ? C32 C33 1.391(5) . ? C33 C34 1.388(5) . ? C33 C331 1.508(5) . ? C34 C35 1.393(5) . ? C35 C36 1.404(5) . ? C35 C351 1.504(5) . ? C37 C38 1.525(5) . ? C37 C39 1.530(5) . ? C1W Cl1W 1.4757 . ? C1W Cl2W 1.8145 . ? C1Z Cl2Z 1.6498 . ? C1Z Cl1Z 1.8817 . ? 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 97.55(13) . . ? N1 W1 N3 96.88(13) . . ? N2 W1 N3 96.81(12) . . ? N1 W1 Cl3 90.17(10) . . ? N2 W1 Cl3 169.69(9) . . ? N3 W1 Cl3 89.00(9) . . ? N1 W1 Cl1 169.24(10) . . ? N2 W1 Cl1 89.29(9) . . ? N3 W1 Cl1 90.50(9) . . ? Cl3 W1 Cl1 82.12(3) . . ? N1 W1 Cl2 89.32(10) . . ? N2 W1 Cl2 90.33(9) . . ? N3 W1 Cl2 169.83(9) . . ? Cl3 W1 Cl2 82.91(3) . . ? Cl1 W1 Cl2 82.33(3) . . ? C11 N1 C17 110.7(3) . . ? C11 N1 W1 121.1(2) . . ? C17 N1 W1 127.3(2) . . ? C21 N2 C27 110.5(3) . . ? C21 N2 W1 120.9(2) . . ? C27 N2 W1 127.8(2) . . ? C31 N3 C37 111.0(3) . . ? C31 N3 W1 120.5(2) . . ? C37 N3 W1 127.8(2) . . ? C12 C11 C16 121.0(4) . . ? C12 C11 N1 120.3(3) . . ? C16 C11 N1 118.6(4) . . ? C11 C12 C13 119.6(4) . . ? C14 C13 C12 119.0(4) . . ? C14 C13 C131 121.8(4) . . ? C12 C13 C131 119.2(4) . . ? C13 C14 C15 121.9(4) . . ? C14 C15 C16 118.8(4) . . ? C14 C15 C151 121.8(4) . . ? C16 C15 C151 119.4(4) . . ? C11 C16 C15 119.7(4) . . ? N1 C17 C18 110.8(4) . . ? N1 C17 C19 112.2(3) . . ? C18 C17 C19 111.4(4) . . ? C22 C21 C26 120.3(4) . . ? C22 C21 N2 120.4(3) . . ? C26 C21 N2 119.3(4) . . ? C21 C22 C23 120.1(4) . . ? C24 C23 C22 118.8(5) . . ? C24 C23 C231 120.6(4) . . ? C22 C23 C231 120.6(5) . . ? C23 C24 C25 121.8(4) . . ? C26 C25 C24 118.2(5) . . ? C26 C25 C251 119.5(5) . . ? C24 C25 C251 122.3(5) . . ? C25 C26 C21 120.7(4) . . ? C28 C27 N2 113.4(3) . . ? C28 C27 C29 111.1(3) . . ? N2 C27 C29 110.2(3) . . ? C36 C31 C32 120.6(3) . . ? C36 C31 N3 120.1(3) . . ? C32 C31 N3 119.2(3) . . ? C31 C32 C33 120.6(3) . . ? C34 C33 C32 118.6(3) . . ? C34 C33 C331 121.9(3) . . ? C32 C33 C331 119.5(3) . . ? C33 C34 C35 121.8(3) . . ? C34 C35 C36 118.9(3) . . ? C34 C35 C351 121.2(3) . . ? C36 C35 C351 119.9(3) . . ? C31 C36 C35 119.5(3) . . ? N3 C37 C38 112.9(3) . . ? N3 C37 C39 109.8(3) . . ? C38 C37 C39 111.3(3) . . ? Cl1W C1W Cl2W 128.2 . . ? Cl2Z C1Z Cl1Z 119.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.061 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.150