# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2226 data_ajn146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Mo Cl2 (N C6 H3 Me-2 -CH Me2-6)2 (dme)]' ; _chemical_name_common ? _chemical_formula_moiety '[Mo Cl2 (N C6 H3 Me-2 -CH Me2-6)2 (dme)]' _chemical_formula_sum 'C24 H36 Cl2 Mo N2 O2' _chemical_formula_weight 551.39 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.59800(10) _cell_length_b 10.0198(2) _cell_length_c 14.9081(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.1190(10) _cell_angle_gamma 90.00 _cell_volume 2595.50(8) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description 'platelike fragment' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorption_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.6885 _exptl_absorpt_correction_T_max 0.9172 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'area detector\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 7070 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3639 _reflns_number_gt 3347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART ' _computing_data_reduction 'Siemens SMART (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3' _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 w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.1783P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.29(10) _refine_ls_number_reflns 3639 _refine_ls_number_parameters 281 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.095 _refine_ls_shift/su_mean 0.019 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.75455(9) 0.181540(16) 0.60196(12) 0.01990(6) Uani 1 d . . . Cl1 Cl 0.82594(7) 0.1369(3) 0.47959(9) 0.0320(5) Uani 1 d . . . Cl2 Cl 0.68366(8) 0.1365(3) 0.72469(9) 0.0312(5) Uani 1 d . . . O1 O 0.6917(3) -0.0090(6) 0.5412(4) 0.0305(14) Uani 1 d . . . O2 O 0.8204(3) -0.0111(5) 0.6658(4) 0.0255(13) Uani 1 d . . . N1 N 0.6846(4) 0.2872(7) 0.5400(5) 0.0218(15) Uani 1 d . . . N2 N 0.8218(4) 0.2868(7) 0.6607(5) 0.0262(16) Uani 1 d . . . C1 C 0.7346(5) -0.1279(9) 0.5516(7) 0.037(2) Uani 1 d . . . H1A H 0.7721 -0.1292 0.5095 0.080 Uiso 1 calc R . . H1B H 0.7003 -0.2050 0.5384 0.080 Uiso 1 calc R . . C2 C 0.7752(5) -0.1341(9) 0.6480(7) 0.038(2) Uani 1 d . . . H2A H 0.7378 -0.1412 0.6898 0.080 Uiso 1 calc R . . H2B H 0.8092 -0.2121 0.6565 0.080 Uiso 1 calc R . . C3 C 0.6473(5) -0.0005(10) 0.4474(6) 0.041(2) Uani 1 d . . . H3A H 0.6177 0.0817 0.4410 0.080 Uiso 1 calc R . . H3B H 0.6126 -0.0760 0.4366 0.080 Uiso 1 calc R . . H3C H 0.6826 -0.0015 0.4036 0.080 Uiso 1 calc R . . C4 C 0.8609(6) -0.0071(9) 0.7542(6) 0.035(2) Uani 1 d . . . H4A H 0.8898 0.0756 0.7633 0.080 Uiso 1 calc R . . H4B H 0.8962 -0.0821 0.7636 0.080 Uiso 1 calc R . . H4C H 0.8250 -0.0120 0.7972 0.080 Uiso 1 calc R . . C5 C 0.6441(4) 0.3932(8) 0.4967(6) 0.0255(18) Uani 1 d . . . C6 C 0.6790(4) 0.4924(8) 0.4612(5) 0.0280(18) Uani 1 d . . . C7 C 0.6324(6) 0.5939(9) 0.4066(7) 0.037(2) Uani 1 d . . . H7 H 0.6551 0.6662 0.3806 0.080 Uiso 1 calc R . . C8 C 0.5564(7) 0.5782(9) 0.3960(7) 0.044(2) Uani 1 d . . . H8 H 0.5260 0.6349 0.3547 0.080 Uiso 1 calc R . . C9 C 0.5213(5) 0.4898(9) 0.4387(6) 0.040(2) Uani 1 d . . . H9 H 0.4675 0.4948 0.4352 0.080 Uiso 1 calc R . . C10 C 0.5626(5) 0.3852(8) 0.4909(5) 0.0258(18) Uani 1 d . . . C11 C 0.7681(4) 0.5064(8) 0.4705(5) 0.0389(19) Uani 1 d . . . H11A H 0.7806 0.5863 0.4391 0.080 Uiso 1 calc R . . H11B H 0.7890 0.4289 0.4439 0.080 Uiso 1 calc R . . H11C H 0.7902 0.5126 0.5342 0.080 Uiso 1 calc R . . C12 C 0.5234(5) 0.2758(9) 0.5437(7) 0.036(2) Uani 1 d . . . H12 H 0.5597 0.2008 0.5590 0.080 Uiso 1 calc R . . C13 C 0.5053(7) 0.3341(11) 0.6275(8) 0.055(3) Uani 1 d . . . H13A H 0.5522 0.3662 0.6642 0.080 Uiso 1 calc R . . H13B H 0.4818 0.2669 0.6611 0.080 Uiso 1 calc R . . H13C H 0.4698 0.4079 0.6130 0.080 Uiso 1 calc R . . C14 C 0.4505(6) 0.2239(11) 0.4855(8) 0.062(3) Uani 1 d . . . H14A H 0.4633 0.1857 0.4300 0.080 Uiso 1 calc R . . H14B H 0.4145 0.2969 0.4707 0.080 Uiso 1 calc R . . H14C H 0.4273 0.1560 0.5189 0.080 Uiso 1 calc R . . C15 C 0.8684(5) 0.3877(8) 0.7038(6) 0.0219(16) Uani 1 d . . . C16 C 0.8294(5) 0.4994(7) 0.7458(6) 0.0297(19) Uani 1 d . . . C17 C 0.8736(6) 0.5858(9) 0.7941(7) 0.037(2) Uani 1 d . . . H17 H 0.8499 0.6512 0.8255 0.080 Uiso 1 calc R . . C18 C 0.9570(6) 0.5880(9) 0.8027(7) 0.041(2) Uani 1 d . . . H18 H 0.9865 0.6560 0.8348 0.080 Uiso 1 calc R . . C19 C 0.9924(5) 0.4808(10) 0.7596(7) 0.0374(19) Uani 1 d . . . H19 H 1.0463 0.4777 0.7649 0.080 Uiso 1 calc R . . C20 C 0.9498(5) 0.3844(10) 0.7117(6) 0.033(2) Uani 1 d . . . C21 C 0.7447(5) 0.5068(6) 0.7264(5) 0.0359(19) Uani 1 d . . . H21A H 0.7249 0.4313 0.6891 0.080 Uiso 1 calc R . . H21B H 0.7294 0.5891 0.6943 0.080 Uiso 1 calc R . . H21C H 0.7242 0.5049 0.7830 0.080 Uiso 1 calc R . . C22 C 0.9871(5) 0.2841(9) 0.6643(7) 0.035(2) Uani 1 d . . . H22 H 0.9494 0.2112 0.6484 0.080 Uiso 1 calc R . . C23 C 1.0053(9) 0.3439(13) 0.5713(8) 0.062(3) Uani 1 d . . . H23A H 1.0302 0.2765 0.5394 0.080 Uiso 1 calc R . . H23B H 1.0391 0.4204 0.5838 0.080 Uiso 1 calc R . . H23C H 0.9577 0.3715 0.5340 0.080 Uiso 1 calc R . . C24 C 1.0602(6) 0.2203(11) 0.7196(9) 0.068(4) Uani 1 d . . . H24A H 1.0810 0.1544 0.6825 0.080 Uiso 1 calc R . . H24B H 1.0469 0.1775 0.7734 0.080 Uiso 1 calc R . . H24C H 1.0984 0.2891 0.7376 0.080 Uiso 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 Mo1 0.01666(9) 0.02178(9) 0.02132(9) -0.0004(4) 0.00321(6) -0.0001(4) Cl1 0.0284(12) 0.0414(13) 0.0280(12) -0.0046(11) 0.0104(10) 0.0004(10) Cl2 0.0329(13) 0.0340(12) 0.0298(13) 0.0012(11) 0.0147(10) -0.0013(10) O1 0.027(3) 0.040(3) 0.022(3) -0.001(2) -0.003(2) -0.001(2) O2 0.025(3) 0.017(2) 0.034(3) 0.008(2) 0.003(2) 0.0022(19) N1 0.009(3) 0.034(3) 0.022(3) -0.001(3) 0.003(2) -0.001(2) N2 0.034(4) 0.021(3) 0.026(4) -0.003(3) 0.010(3) -0.004(3) C1 0.036(4) 0.027(4) 0.044(4) -0.009(3) -0.008(3) -0.011(3) C2 0.044(4) 0.022(3) 0.050(4) 0.002(3) 0.014(4) -0.013(3) C3 0.029(4) 0.058(6) 0.031(4) -0.018(4) -0.013(3) -0.004(3) C4 0.040(4) 0.034(4) 0.031(4) 0.001(3) 0.006(3) 0.006(3) C5 0.020(3) 0.030(4) 0.024(3) 0.000(3) -0.003(3) 0.009(3) C6 0.030(4) 0.029(4) 0.022(3) 0.001(3) -0.001(3) 0.014(3) C7 0.059(5) 0.022(3) 0.029(4) 0.003(3) 0.003(3) 0.016(3) C8 0.059(5) 0.037(4) 0.030(3) 0.000(3) -0.009(3) 0.025(3) C9 0.035(4) 0.043(4) 0.039(4) -0.002(3) -0.007(3) 0.027(3) C10 0.030(4) 0.023(4) 0.024(4) 0.001(3) 0.004(3) 0.005(3) C11 0.029(3) 0.064(4) 0.024(2) -0.005(3) 0.005(2) -0.014(3) C12 0.025(4) 0.036(4) 0.050(5) 0.007(3) 0.011(3) -0.011(3) C13 0.056(5) 0.048(4) 0.066(7) 0.009(4) 0.025(5) -0.001(4) C14 0.040(5) 0.068(6) 0.073(6) 0.015(5) -0.007(5) -0.014(5) C15 0.030(4) 0.018(3) 0.020(3) 0.002(3) 0.010(3) 0.004(3) C16 0.044(4) 0.021(3) 0.026(3) 0.002(3) 0.014(3) 0.012(3) C17 0.055(5) 0.026(4) 0.031(4) -0.003(3) 0.009(4) 0.006(3) C18 0.044(4) 0.022(3) 0.055(5) -0.003(3) 0.000(3) -0.011(3) C19 0.029(3) 0.033(3) 0.048(4) 0.001(3) 0.001(3) 0.004(3) C20 0.020(4) 0.038(5) 0.040(5) 0.013(4) 0.000(3) -0.005(3) C21 0.045(4) 0.021(3) 0.048(4) -0.016(2) 0.024(3) -0.001(2) C22 0.022(4) 0.035(4) 0.048(5) 0.003(3) 0.004(3) -0.017(3) C23 0.088(7) 0.063(5) 0.047(5) 0.000(4) 0.045(5) -0.013(5) C24 0.027(5) 0.058(6) 0.118(9) 0.022(5) 0.008(5) 0.008(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 Mo1 N2 1.718(7) . ? Mo1 N1 1.769(7) . ? Mo1 O1 2.317(6) . ? Mo1 O2 2.372(5) . ? Mo1 Cl2 2.415(2) . ? Mo1 Cl1 2.415(2) . ? O1 C1 1.406(10) . ? O1 C3 1.492(9) . ? O2 C4 1.397(9) . ? O2 C2 1.467(10) . ? N1 C5 1.381(10) . ? N2 C15 1.393(10) . ? C1 C2 1.502(4) . ? C5 C6 1.322(12) . ? C5 C10 1.425(11) . ? C6 C7 1.469(11) . ? C6 C11 1.558(11) . ? C7 C8 1.330(16) . ? C8 C9 1.303(14) . ? C9 C10 1.434(10) . ? C10 C12 1.571(12) . ? C12 C13 1.460(15) . ? C12 C14 1.521(13) . ? C15 C20 1.420(11) . ? C15 C16 1.500(11) . ? C16 C17 1.302(12) . ? C16 C21 1.475(11) . ? C17 C18 1.453(15) . ? C18 C19 1.443(13) . ? C19 C20 1.354(12) . ? C20 C22 1.445(14) . ? C22 C24 1.551(14) . ? C22 C23 1.588(14) . ? 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 Mo1 N1 105.36(10) . . ? N2 Mo1 O1 162.3(3) . . ? N1 Mo1 O1 92.2(3) . . ? N2 Mo1 O2 92.4(3) . . ? N1 Mo1 O2 162.2(3) . . ? O1 Mo1 O2 70.06(6) . . ? N2 Mo1 Cl2 97.2(3) . . ? N1 Mo1 Cl2 96.2(2) . . ? O1 Mo1 Cl2 82.56(17) . . ? O2 Mo1 Cl2 79.74(16) . . ? N2 Mo1 Cl1 95.7(3) . . ? N1 Mo1 Cl1 96.8(3) . . ? O1 Mo1 Cl1 79.95(17) . . ? O2 Mo1 Cl1 82.71(16) . . ? Cl2 Mo1 Cl1 158.57(2) . . ? C1 O1 C3 110.1(7) . . ? C1 O1 Mo1 116.2(5) . . ? C3 O1 Mo1 117.8(5) . . ? C4 O2 C2 112.1(7) . . ? C4 O2 Mo1 120.0(5) . . ? C2 O2 Mo1 113.3(5) . . ? C5 N1 Mo1 165.8(6) . . ? C15 N2 Mo1 171.3(6) . . ? O1 C1 C2 107.8(7) . . ? O2 C2 C1 107.5(7) . . ? C6 C5 N1 121.8(7) . . ? C6 C5 C10 123.0(7) . . ? N1 C5 C10 115.2(8) . . ? C5 C6 C7 119.2(8) . . ? C5 C6 C11 123.9(6) . . ? C7 C6 C11 116.9(7) . . ? C8 C7 C6 116.6(9) . . ? C9 C8 C7 124.6(9) . . ? C8 C9 C10 121.5(9) . . ? C5 C10 C9 114.3(8) . . ? C5 C10 C12 121.8(8) . . ? C9 C10 C12 123.8(8) . . ? C13 C12 C14 110.3(9) . . ? C13 C12 C10 108.8(8) . . ? C14 C12 C10 110.6(8) . . ? N2 C15 C20 122.3(8) . . ? N2 C15 C16 117.4(7) . . ? C20 C15 C16 120.3(8) . . ? C17 C16 C21 124.8(7) . . ? C17 C16 C15 117.0(8) . . ? C21 C16 C15 118.1(7) . . ? C16 C17 C18 124.4(8) . . ? C19 C18 C17 116.8(9) . . ? C20 C19 C18 121.5(9) . . ? C19 C20 C15 119.6(9) . . ? C19 C20 C22 119.8(8) . . ? C15 C20 C22 120.5(8) . . ? C20 C22 C24 115.4(9) . . ? C20 C22 C23 109.5(8) . . ? C24 C22 C23 110.8(9) . . ? _diffrn_measured_fraction_theta_max 0.480 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.480 _refine_diff_density_max 0.336 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.048 data_ajn148 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Mo Cl2 (N C6 H4 CMe3-2)2(dme)]' ; _chemical_name_common ? _chemical_formula_moiety '[Mo Cl2 (N C6 H4 CMe3-2)2(dme)]' _chemical_formula_sum 'C24 H36 Cl2 Mo N2 O2' _chemical_formula_weight 551.39 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' 'Mo' 'Mo' -1.6832 0.6857 '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-bar)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.79290(10) _cell_length_b 16.87650(10) _cell_length_c 18.3315(2) _cell_angle_alpha 76.5050(10) _cell_angle_beta 88.2590(10) _cell_angle_gamma 86.3060(10) _cell_volume 2639.34(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description 'crystal fragment' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type 'multi-scans' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.7613 _exptl_absorpt_correction_T_max 0.9446 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemen's SMART diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 24570 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.43 _reflns_number_total 11281 _reflns_number_gt 9295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SMART (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _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 w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+2.4955P] 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 11281 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.84387(3) 0.193394(14) 0.283088(14) 0.02174(7) Uani 1 d . . . Cl1 Cl 1.07403(8) 0.19275(4) 0.20981(4) 0.03019(16) Uani 1 d . . . Cl2 Cl 0.61789(8) 0.14427(5) 0.35442(4) 0.03300(17) Uani 1 d . . . O1 O 0.9181(2) 0.05640(12) 0.32827(12) 0.0293(5) Uani 1 d . . . O2 O 0.7633(2) 0.11553(12) 0.19900(11) 0.0293(5) Uani 1 d . . . N1 N 0.9164(3) 0.22886(14) 0.35810(13) 0.0249(5) Uani 1 d . . . N2 N 0.7449(3) 0.27857(14) 0.22844(13) 0.0243(5) Uani 1 d . . . C1 C 0.9314(4) 0.0232(2) 0.40774(19) 0.0434(9) Uani 1 d . . . H1A H 0.9814 0.0611 0.4301 0.080 Uiso 1 calc R . . H1B H 0.9912 -0.0284 0.4165 0.080 Uiso 1 calc R . . H1C H 0.8307 0.0146 0.4301 0.080 Uiso 1 calc R . . C2 C 0.8432(4) 0.00018(19) 0.29397(19) 0.0355(7) Uani 1 d . . . H2A H 0.7391 -0.0069 0.3141 0.080 Uiso 1 calc R . . H2B H 0.8992 -0.0533 0.3047 0.080 Uiso 1 calc R . . C3 C 0.8402(4) 0.03575(19) 0.2109(2) 0.0387(8) Uani 1 d . . . H3A H 0.9443 0.0399 0.1903 0.080 Uiso 1 calc R . . H3B H 0.7858 0.0009 0.1858 0.080 Uiso 1 calc R . . C4 C 0.7583(4) 0.1554(2) 0.11981(18) 0.0389(8) Uani 1 d . . . H4A H 0.7060 0.2089 0.1135 0.080 Uiso 1 calc R . . H4B H 0.7041 0.1227 0.0933 0.080 Uiso 1 calc R . . H4C H 0.8613 0.1612 0.0997 0.080 Uiso 1 calc R . . C5 C 0.9030(3) 0.28779(17) 0.40074(15) 0.0241(6) Uani 1 d . . . C6 C 0.7567(3) 0.32528(19) 0.40543(16) 0.0295(6) Uani 1 d . . . H6A H 0.6768 0.3126 0.3780 0.080 Uiso 1 calc R . . C7 C 0.7290(4) 0.3808(2) 0.45019(18) 0.0364(7) Uani 1 d . . . H7A H 0.6303 0.4046 0.4541 0.080 Uiso 1 calc R . . C8 C 0.8473(4) 0.4008(2) 0.48888(19) 0.0403(8) Uani 1 d . . . H8A H 0.8295 0.4387 0.5189 0.080 Uiso 1 calc R . . C9 C 0.9926(4) 0.3650(2) 0.48347(18) 0.0366(7) Uani 1 d . . . H9A H 1.0716 0.3801 0.5099 0.080 Uiso 1 calc R . . C10 C 1.0266(3) 0.30786(18) 0.44074(16) 0.0270(6) Uani 1 d . . . C11 C 1.1897(4) 0.26985(19) 0.43652(18) 0.0324(7) Uani 1 d . . . C12 C 1.2454(4) 0.2855(2) 0.3539(2) 0.0396(8) Uani 1 d . . . H12A H 1.2420 0.3438 0.3322 0.080 Uiso 1 calc R . . H12B H 1.1800 0.2596 0.3259 0.080 Uiso 1 calc R . . H12C H 1.3493 0.2629 0.3517 0.080 Uiso 1 calc R . . C13 C 1.3027(4) 0.3068(2) 0.4799(2) 0.0450(9) Uani 1 d . . . H13A H 1.3024 0.3652 0.4596 0.080 Uiso 1 calc R . . H13B H 1.4043 0.2823 0.4750 0.080 Uiso 1 calc R . . H13C H 1.2726 0.2960 0.5325 0.080 Uiso 1 calc R . . C14 C 1.1936(5) 0.1775(2) 0.4716(3) 0.0614(12) Uani 1 d . . . H14A H 1.2966 0.1541 0.4686 0.080 Uiso 1 calc R . . H14B H 1.1258 0.1519 0.4445 0.080 Uiso 1 calc R . . H14C H 1.1607 0.1684 0.5237 0.080 Uiso 1 calc R . . C15 C 0.6374(3) 0.33729(17) 0.19031(16) 0.0240(6) Uani 1 d . . . C16 C 0.4871(3) 0.31202(19) 0.19498(17) 0.0297(7) Uani 1 d . . . H16A H 0.4665 0.2593 0.2223 0.080 Uiso 1 calc R . . C17 C 0.3696(4) 0.3641(2) 0.15980(19) 0.0367(7) Uani 1 d . . . H17A H 0.2692 0.3473 0.1639 0.080 Uiso 1 calc R . . C18 C 0.4011(4) 0.4406(2) 0.11876(19) 0.0379(8) Uani 1 d . . . H18A H 0.3220 0.4762 0.0945 0.080 Uiso 1 calc R . . C19 C 0.5505(4) 0.46569(19) 0.11297(17) 0.0320(7) Uani 1 d . . . H19A H 0.5690 0.5182 0.0844 0.080 Uiso 1 calc R . . C20 C 0.6736(3) 0.41593(17) 0.14784(16) 0.0251(6) Uani 1 d . . . C21 C 0.8377(4) 0.44384(18) 0.13705(17) 0.0292(6) Uani 1 d . . . C22 C 0.9277(4) 0.3920(2) 0.08944(19) 0.0374(8) Uani 1 d . . . H22A H 0.8775 0.3981 0.0419 0.080 Uiso 1 calc R . . H22B H 0.9318 0.3351 0.1161 0.080 Uiso 1 calc R . . H22C H 1.0304 0.4102 0.0804 0.080 Uiso 1 calc R . . C23 C 0.9154(4) 0.4346(2) 0.21266(19) 0.0390(8) Uani 1 d . . . H23A H 1.0184 0.4525 0.2041 0.080 Uiso 1 calc R . . H23B H 0.9186 0.3778 0.2397 0.080 Uiso 1 calc R . . H23C H 0.8583 0.4677 0.2420 0.080 Uiso 1 calc R . . C24 C 0.8419(4) 0.5342(2) 0.0951(2) 0.0459(9) Uani 1 d . . . H24A H 0.7936 0.5422 0.0469 0.080 Uiso 1 calc R . . H24B H 0.9470 0.5490 0.0875 0.080 Uiso 1 calc R . . H24C H 0.7880 0.5682 0.1246 0.080 Uiso 1 calc R . . Mo2 Mo 0.38863(3) 0.850773(14) 0.249992(14) 0.02296(7) Uani 1 d . . . Cl3 Cl 0.62044(8) 0.82950(4) 0.31939(4) 0.03075(16) Uani 1 d . . . Cl4 Cl 0.14557(9) 0.91091(5) 0.20126(5) 0.03587(18) Uani 1 d . . . O3 O 0.4243(2) 0.98795(12) 0.24125(12) 0.0318(5) Uani 1 d . . . O4 O 0.2930(2) 0.88960(13) 0.36354(12) 0.0325(5) Uani 1 d . . . N3 N 0.4648(3) 0.84631(15) 0.16025(14) 0.0276(5) Uani 1 d . . . N4 N 0.3137(3) 0.75567(14) 0.28158(14) 0.0261(5) Uani 1 d . . . C31 C 0.4154(4) 1.0445(2) 0.1682(2) 0.0439(9) Uani 1 d . . . H31A H 0.4710 1.0206 0.1314 0.080 Uiso 1 calc R . . H31B H 0.4597 1.0950 0.1707 0.080 Uiso 1 calc R . . H31C H 0.3095 1.0558 0.1539 0.080 Uiso 1 calc R . . C32 C 0.3417(4) 1.02309(19) 0.2967(2) 0.0362(7) Uani 1 d . . . H32A H 0.2340 1.0337 0.2834 0.080 Uiso 1 calc R . . H32B H 0.3837 1.0748 0.2989 0.080 Uiso 1 calc R . . C33 C 0.3574(4) 0.9633(2) 0.3712(2) 0.0383(8) Uani 1 d . . . H33A H 0.4649 0.9526 0.3847 0.080 Uiso 1 calc R . . H33B H 0.3027 0.9850 0.4104 0.080 Uiso 1 calc R . . C34 C 0.2915(5) 0.8282(2) 0.43375(19) 0.0462(9) Uani 1 d . . . H34A H 0.2474 0.7797 0.4260 0.080 Uiso 1 calc R . . H34B H 0.2311 0.8495 0.4709 0.080 Uiso 1 calc R . . H34C H 0.3949 0.8146 0.4513 0.080 Uiso 1 calc R . . C35 C 0.4611(4) 0.79969(18) 0.10611(16) 0.0281(6) Uani 1 d . . . C36 C 0.3220(4) 0.7648(2) 0.09930(18) 0.0350(7) Uani 1 d . . . H36A H 0.2366 0.7766 0.1278 0.080 Uiso 1 calc R . . C37 C 0.3099(4) 0.7135(2) 0.0511(2) 0.0414(8) Uani 1 d . . . H37A H 0.2169 0.6906 0.0469 0.080 Uiso 1 calc R . . C38 C 0.4355(4) 0.6963(2) 0.0096(2) 0.0444(9) Uani 1 d . . . H38A H 0.4292 0.6600 -0.0219 0.080 Uiso 1 calc R . . C39 C 0.5713(4) 0.7322(2) 0.01407(19) 0.0419(8) Uani 1 d . . . H39A H 0.6545 0.7202 -0.0157 0.080 Uiso 1 calc R . . C40 C 0.5903(4) 0.7856(2) 0.06095(17) 0.0330(7) Uani 1 d . . . C41 C 0.7437(4) 0.8230(2) 0.06550(18) 0.0392(8) Uani 1 d . . . C42 C 0.7234(5) 0.9167(3) 0.0492(2) 0.0567(11) Uani 1 d . . . H42A H 0.6496 0.9326 0.0844 0.080 Uiso 1 calc R . . H42B H 0.6874 0.9377 -0.0016 0.080 Uiso 1 calc R . . H42C H 0.8203 0.9391 0.0544 0.080 Uiso 1 calc R . . C43 C 0.8111(4) 0.7889(3) 0.1443(2) 0.0502(10) Uani 1 d . . . H43A H 0.7396 0.8012 0.1820 0.080 Uiso 1 calc R . . H43B H 0.9062 0.8138 0.1477 0.080 Uiso 1 calc R . . H43C H 0.8299 0.7302 0.1526 0.080 Uiso 1 calc R . . C44 C 0.8622(5) 0.8017(3) 0.0083(2) 0.0612(12) Uani 1 d . . . H44A H 0.8782 0.7429 0.0169 0.080 Uiso 1 calc R . . H44B H 0.9577 0.8252 0.0141 0.080 Uiso 1 calc R . . H44C H 0.8253 0.8237 -0.0422 0.080 Uiso 1 calc R . . C45 C 0.2188(3) 0.68999(18) 0.29849(16) 0.0249(6) Uani 1 d . . . C46 C 0.0625(4) 0.7124(2) 0.30462(18) 0.0324(7) Uani 1 d . . . H46A H 0.0305 0.7677 0.2986 0.080 Uiso 1 calc R . . C47 C -0.0447(4) 0.6535(2) 0.31942(18) 0.0364(7) Uani 1 d . . . H47A H -0.1490 0.6688 0.3224 0.080 Uiso 1 calc R . . C48 C 0.0037(4) 0.5721(2) 0.32974(19) 0.0378(8) Uani 1 d . . . H48A H -0.0677 0.5317 0.3406 0.080 Uiso 1 calc R . . C49 C 0.1586(4) 0.5500(2) 0.32403(18) 0.0342(7) Uani 1 d . . . H49A H 0.1885 0.4943 0.3308 0.080 Uiso 1 calc R . . C50 C 0.2717(3) 0.60668(17) 0.30867(16) 0.0261(6) Uani 1 d . . . C51 C 0.4419(4) 0.57930(17) 0.30855(17) 0.0284(6) Uani 1 d . . . C52 C 0.5155(4) 0.5974(2) 0.37756(19) 0.0354(7) Uani 1 d . . . H52A H 0.6231 0.5805 0.3781 0.080 Uiso 1 calc R . . H52B H 0.4662 0.5676 0.4229 0.080 Uiso 1 calc R . . H52C H 0.5036 0.6555 0.3752 0.080 Uiso 1 calc R . . C53 C 0.5267(4) 0.6231(2) 0.23679(19) 0.0374(8) Uani 1 d . . . H53A H 0.6333 0.6040 0.2393 0.080 Uiso 1 calc R . . H53B H 0.5186 0.6815 0.2329 0.080 Uiso 1 calc R . . H53C H 0.4816 0.6113 0.1932 0.080 Uiso 1 calc R . . C54 C 0.4648(4) 0.48736(18) 0.31224(19) 0.0371(8) Uani 1 d . . . H54A H 0.5730 0.4719 0.3121 0.080 Uiso 1 calc R . . H54B H 0.4182 0.4752 0.2691 0.080 Uiso 1 calc R . . H54C H 0.4176 0.4570 0.3579 0.080 Uiso 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 Mo1 0.02064(13) 0.02041(12) 0.02440(13) -0.00588(9) -0.00026(9) -0.00031(9) Cl1 0.0249(4) 0.0316(4) 0.0333(4) -0.0074(3) 0.0048(3) 0.0012(3) Cl2 0.0268(4) 0.0347(4) 0.0384(4) -0.0101(3) 0.0065(3) -0.0061(3) O1 0.0335(12) 0.0226(10) 0.0306(11) -0.0034(8) -0.0002(9) -0.0025(8) O2 0.0331(12) 0.0271(11) 0.0292(11) -0.0104(9) -0.0021(9) 0.0017(9) N1 0.0219(12) 0.0271(12) 0.0256(12) -0.0054(10) 0.0005(10) -0.0025(10) N2 0.0225(12) 0.0250(12) 0.0264(12) -0.0084(10) 0.0011(10) -0.0016(9) C1 0.058(2) 0.0336(18) 0.0339(18) 0.0042(14) -0.0085(16) -0.0053(16) C2 0.0396(19) 0.0240(15) 0.0446(19) -0.0119(14) -0.0009(15) -0.0006(13) C3 0.047(2) 0.0286(16) 0.044(2) -0.0167(15) -0.0026(16) 0.0043(14) C4 0.045(2) 0.045(2) 0.0280(17) -0.0100(15) -0.0019(14) -0.0045(16) C5 0.0285(15) 0.0245(14) 0.0183(13) -0.0029(11) 0.0016(11) -0.0025(11) C6 0.0281(16) 0.0361(17) 0.0241(15) -0.0072(13) -0.0012(12) 0.0001(13) C7 0.0363(18) 0.0420(19) 0.0326(17) -0.0142(14) 0.0030(14) 0.0034(14) C8 0.048(2) 0.045(2) 0.0329(18) -0.0195(15) 0.0047(15) -0.0033(16) C9 0.0420(19) 0.0425(19) 0.0299(17) -0.0149(14) -0.0014(14) -0.0121(15) C10 0.0275(15) 0.0300(15) 0.0209(14) 0.0006(12) 0.0002(11) -0.0065(12) C11 0.0279(16) 0.0299(16) 0.0358(17) 0.0010(13) -0.0069(13) -0.0030(12) C12 0.0238(16) 0.054(2) 0.046(2) -0.0214(17) 0.0026(14) -0.0035(14) C13 0.0350(19) 0.057(2) 0.040(2) -0.0031(17) -0.0108(15) -0.0121(16) C14 0.043(2) 0.039(2) 0.092(3) 0.008(2) -0.026(2) -0.0062(17) C15 0.0244(15) 0.0259(14) 0.0230(14) -0.0097(11) -0.0014(11) 0.0033(11) C16 0.0272(16) 0.0310(16) 0.0320(16) -0.0097(13) -0.0013(13) -0.0004(12) C17 0.0237(16) 0.050(2) 0.0376(18) -0.0138(16) -0.0042(13) 0.0020(14) C18 0.0312(17) 0.046(2) 0.0348(18) -0.0093(15) -0.0085(14) 0.0126(15) C19 0.0402(18) 0.0283(16) 0.0261(15) -0.0050(12) -0.0018(13) 0.0047(13) C20 0.0290(15) 0.0262(14) 0.0207(14) -0.0082(11) 0.0014(11) 0.0021(12) C21 0.0312(16) 0.0291(15) 0.0268(15) -0.0048(12) 0.0000(12) -0.0053(12) C22 0.0313(17) 0.046(2) 0.0338(17) -0.0100(15) 0.0086(14) -0.0007(14) C23 0.0409(19) 0.047(2) 0.0331(18) -0.0134(15) -0.0006(15) -0.0186(16) C24 0.049(2) 0.0334(18) 0.052(2) -0.0034(16) 0.0094(18) -0.0094(16) Mo2 0.02223(13) 0.02200(13) 0.02572(13) -0.00782(10) -0.00086(10) -0.00062(9) Cl3 0.0283(4) 0.0313(4) 0.0334(4) -0.0086(3) -0.0067(3) 0.0000(3) Cl4 0.0270(4) 0.0336(4) 0.0476(5) -0.0115(3) -0.0078(3) 0.0042(3) O3 0.0318(12) 0.0242(11) 0.0390(12) -0.0067(9) -0.0033(10) 0.0008(9) O4 0.0381(13) 0.0295(11) 0.0311(12) -0.0101(9) 0.0008(9) 0.0009(9) N3 0.0244(13) 0.0319(13) 0.0271(13) -0.0083(11) -0.0043(10) 0.0023(10) N4 0.0248(13) 0.0240(12) 0.0305(13) -0.0088(10) -0.0012(10) 0.0002(10) C31 0.045(2) 0.0307(18) 0.049(2) 0.0051(15) -0.0010(17) -0.0027(15) C32 0.0352(18) 0.0269(16) 0.051(2) -0.0177(15) -0.0047(15) -0.0002(13) C33 0.0409(19) 0.0378(18) 0.0432(19) -0.0240(15) -0.0010(15) -0.0006(15) C34 0.055(2) 0.048(2) 0.0322(18) -0.0044(16) 0.0061(16) 0.0004(17) C35 0.0326(16) 0.0298(15) 0.0213(14) -0.0052(12) -0.0052(12) 0.0021(12) C36 0.0348(18) 0.0389(18) 0.0319(17) -0.0092(14) -0.0062(14) 0.0005(14) C37 0.045(2) 0.044(2) 0.0395(19) -0.0168(16) -0.0163(16) -0.0014(16) C38 0.054(2) 0.048(2) 0.0359(19) -0.0201(16) -0.0152(17) 0.0113(17) C39 0.046(2) 0.051(2) 0.0301(17) -0.0158(15) -0.0058(15) 0.0149(17) C40 0.0338(17) 0.0404(18) 0.0230(15) -0.0055(13) -0.0041(13) 0.0061(14) C41 0.0334(18) 0.057(2) 0.0284(17) -0.0131(15) 0.0066(14) -0.0030(15) C42 0.057(3) 0.059(3) 0.055(3) -0.014(2) 0.015(2) -0.015(2) C43 0.0324(19) 0.085(3) 0.0343(19) -0.0143(19) -0.0039(15) -0.0060(19) C44 0.048(2) 0.093(3) 0.044(2) -0.022(2) 0.0141(18) 0.000(2) C45 0.0245(15) 0.0287(15) 0.0239(14) -0.0100(12) 0.0000(11) -0.0055(11) C46 0.0275(16) 0.0370(17) 0.0325(17) -0.0073(14) 0.0000(13) -0.0023(13) C47 0.0260(16) 0.051(2) 0.0323(17) -0.0094(15) -0.0023(13) -0.0069(14) C48 0.0359(18) 0.045(2) 0.0363(18) -0.0127(15) -0.0011(14) -0.0194(15) C49 0.0406(19) 0.0327(17) 0.0324(17) -0.0119(14) -0.0002(14) -0.0097(14) C50 0.0313(16) 0.0276(15) 0.0222(14) -0.0110(12) -0.0010(12) -0.0040(12) C51 0.0332(16) 0.0221(14) 0.0297(16) -0.0060(12) -0.0003(13) 0.0001(12) C52 0.0311(17) 0.0402(18) 0.0379(18) -0.0155(15) -0.0033(14) 0.0006(14) C53 0.0391(19) 0.0313(17) 0.0386(18) -0.0053(14) 0.0080(15) 0.0059(14) C54 0.048(2) 0.0253(16) 0.0365(18) -0.0058(13) -0.0004(15) 0.0013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.746(2) . ? Mo1 N1 1.773(2) . ? Mo1 O1 2.3242(19) . ? Mo1 O2 2.395(2) . ? Mo1 Cl1 2.3957(7) . ? Mo1 Cl2 2.4277(8) . ? O1 C1 1.439(4) . ? O1 C2 1.454(4) . ? O2 C3 1.439(4) . ? O2 C4 1.451(4) . ? N1 C5 1.399(4) . ? N2 C15 1.400(4) . ? C2 C3 1.502(5) . ? C5 C6 1.406(4) . ? C5 C10 1.430(4) . ? C6 C7 1.388(4) . ? C7 C8 1.379(5) . ? C8 C9 1.388(5) . ? C9 C10 1.391(4) . ? C10 C11 1.541(4) . ? C11 C13 1.538(5) . ? C11 C14 1.539(5) . ? C11 C12 1.546(5) . ? C15 C16 1.408(4) . ? C15 C20 1.423(4) . ? C16 C17 1.384(4) . ? C17 C18 1.375(5) . ? C18 C19 1.399(5) . ? C19 C20 1.400(4) . ? C20 C21 1.539(4) . ? C21 C23 1.535(4) . ? C21 C22 1.542(4) . ? C21 C24 1.541(4) . ? Mo2 N4 1.739(2) . ? Mo2 N3 1.773(2) . ? Mo2 O3 2.324(2) . ? Mo2 Cl3 2.3984(8) . ? Mo2 Cl4 2.4102(8) . ? Mo2 O4 2.435(2) . ? O3 C32 1.447(4) . ? O3 C31 1.452(4) . ? O4 C33 1.437(4) . ? O4 C34 1.452(4) . ? N3 C35 1.405(4) . ? N4 C45 1.401(4) . ? C32 C33 1.501(5) . ? C35 C36 1.412(4) . ? C35 C40 1.425(4) . ? C36 C37 1.384(5) . ? C37 C38 1.376(5) . ? C38 C39 1.387(5) . ? C39 C40 1.402(5) . ? C40 C41 1.539(5) . ? C41 C42 1.539(5) . ? C41 C44 1.541(5) . ? C41 C43 1.546(5) . ? C45 C46 1.410(4) . ? C45 C50 1.424(4) . ? C46 C47 1.389(5) . ? C47 C48 1.383(5) . ? C48 C49 1.396(5) . ? C49 C50 1.401(4) . ? C50 C51 1.537(4) . ? C51 C54 1.538(4) . ? C51 C52 1.539(4) . ? C51 C53 1.546(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 Mo1 N1 104.62(11) . . ? N2 Mo1 O1 157.73(9) . . ? N1 Mo1 O1 96.71(9) . . ? N2 Mo1 O2 88.19(9) . . ? N1 Mo1 O2 166.92(9) . . ? O1 Mo1 O2 70.28(7) . . ? N2 Mo1 Cl1 99.88(8) . . ? N1 Mo1 Cl1 98.36(8) . . ? O1 Mo1 Cl1 83.00(5) . . ? O2 Mo1 Cl1 81.68(5) . . ? N2 Mo1 Cl2 93.40(8) . . ? N1 Mo1 Cl2 92.89(8) . . ? O1 Mo1 Cl2 79.02(6) . . ? O2 Mo1 Cl2 83.59(5) . . ? Cl1 Mo1 Cl2 159.78(3) . . ? C1 O1 C2 110.1(2) . . ? C1 O1 Mo1 120.04(19) . . ? C2 O1 Mo1 114.99(17) . . ? C3 O2 C4 111.3(2) . . ? C3 O2 Mo1 112.89(18) . . ? C4 O2 Mo1 117.31(18) . . ? C5 N1 Mo1 146.6(2) . . ? C15 N2 Mo1 167.4(2) . . ? O1 C2 C3 107.7(3) . . ? O2 C3 C2 107.5(3) . . ? N1 C5 C6 116.1(3) . . ? N1 C5 C10 123.5(3) . . ? C6 C5 C10 120.3(3) . . ? C7 C6 C5 120.7(3) . . ? C8 C7 C6 119.5(3) . . ? C7 C8 C9 120.0(3) . . ? C8 C9 C10 123.0(3) . . ? C9 C10 C5 116.4(3) . . ? C9 C10 C11 121.1(3) . . ? C5 C10 C11 122.5(3) . . ? C13 C11 C14 107.2(3) . . ? C13 C11 C10 111.9(3) . . ? C14 C11 C10 110.0(3) . . ? C13 C11 C12 107.7(3) . . ? C14 C11 C12 110.1(3) . . ? C10 C11 C12 109.9(2) . . ? N2 C15 C16 114.7(3) . . ? N2 C15 C20 124.1(3) . . ? C16 C15 C20 121.2(3) . . ? C17 C16 C15 120.7(3) . . ? C18 C17 C16 119.3(3) . . ? C17 C18 C19 120.3(3) . . ? C18 C19 C20 122.8(3) . . ? C19 C20 C15 115.6(3) . . ? C19 C20 C21 121.5(3) . . ? C15 C20 C21 122.8(2) . . ? C23 C21 C20 111.4(2) . . ? C23 C21 C22 110.1(3) . . ? C20 C21 C22 108.3(2) . . ? C23 C21 C24 107.3(3) . . ? C20 C21 C24 111.7(3) . . ? C22 C21 C24 107.9(3) . . ? N4 Mo2 N3 102.89(12) . . ? N4 Mo2 O3 158.64(10) . . ? N3 Mo2 O3 97.07(10) . . ? N4 Mo2 Cl3 100.23(8) . . ? N3 Mo2 Cl3 99.30(8) . . ? O3 Mo2 Cl3 83.78(6) . . ? N4 Mo2 Cl4 91.47(8) . . ? N3 Mo2 Cl4 93.61(8) . . ? O3 Mo2 Cl4 79.66(6) . . ? Cl3 Mo2 Cl4 160.12(3) . . ? N4 Mo2 O4 89.74(10) . . ? N3 Mo2 O4 167.06(10) . . ? O3 Mo2 O4 70.05(7) . . ? Cl3 Mo2 O4 80.93(6) . . ? Cl4 Mo2 O4 83.13(6) . . ? C32 O3 C31 109.9(2) . . ? C32 O3 Mo2 115.09(18) . . ? C31 O3 Mo2 119.0(2) . . ? C33 O4 C34 112.3(3) . . ? C33 O4 Mo2 110.87(18) . . ? C34 O4 Mo2 119.26(19) . . ? C35 N3 Mo2 141.0(2) . . ? C45 N4 Mo2 165.1(2) . . ? O3 C32 C33 107.9(2) . . ? O4 C33 C32 106.8(3) . . ? N3 C35 C36 116.5(3) . . ? N3 C35 C40 123.0(3) . . ? C36 C35 C40 120.5(3) . . ? C37 C36 C35 120.9(3) . . ? C38 C37 C36 119.3(3) . . ? C37 C38 C39 120.3(3) . . ? C38 C39 C40 123.1(3) . . ? C39 C40 C35 115.8(3) . . ? C39 C40 C41 121.6(3) . . ? C35 C40 C41 122.5(3) . . ? C42 C41 C40 110.7(3) . . ? C42 C41 C44 107.1(3) . . ? C40 C41 C44 112.3(3) . . ? C42 C41 C43 110.2(3) . . ? C40 C41 C43 109.4(3) . . ? C44 C41 C43 107.0(3) . . ? N4 C45 C46 114.6(3) . . ? N4 C45 C50 124.1(3) . . ? C46 C45 C50 121.2(3) . . ? C47 C46 C45 120.7(3) . . ? C48 C47 C46 119.3(3) . . ? C47 C48 C49 120.0(3) . . ? C48 C49 C50 123.2(3) . . ? C49 C50 C45 115.6(3) . . ? C49 C50 C51 121.5(3) . . ? C45 C50 C51 122.8(3) . . ? C50 C51 C54 111.3(3) . . ? C50 C51 C52 108.6(2) . . ? C54 C51 C52 108.8(3) . . ? C50 C51 C53 112.5(2) . . ? C54 C51 C53 106.4(2) . . ? C52 C51 C53 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.405 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.089 data_mg14 _audit_creation_method SHELXL-97 _chemical_name_systematic '[W Cl3 (N C10 H7) (P Me3)2]' _chemical_name_common ? _chemical_formula_moiety '[W Cl3 (N C10 H7) (P Me3)2]' _chemical_formula_sum 'C16 H25 Cl3 N P2 W' _chemical_formula_weight 583.51 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'P' 'P' 0.1023 0.0942 '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 8.6183(14) _cell_length_b 27.756(4) _cell_length_c 9.486(2) _cell_angle_alpha 90.000(10) _cell_angle_beta 103.90(2) _cell_angle_gamma 90.000(10) _cell_volume 2202.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description 'blocks' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 5.752 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.2526 _exptl_absorpt_correction_T_max 0.6562 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 diffractometer' _diffrn_measurement_method 'omega/2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 4513 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.97 _reflns_number_total 4268 _reflns_number_gt 3106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction 'CAD4 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _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 w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+9.5481P] 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 4268 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.234 _refine_ls_shift/su_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.04207(5) 0.145736(16) 0.13456(5) 0.05471(19) Uani 1 d . . . Cl1 Cl -0.1382(6) 0.18287(18) -0.0771(5) 0.1111(14) Uani 1 d . . . Cl2 Cl 0.2056(6) 0.21465(16) 0.1160(5) 0.1032(14) Uani 1 d . . . Cl3 Cl -0.1515(6) 0.08335(16) 0.1135(6) 0.1079(14) Uani 1 d . . . P1 P 0.1676(5) 0.10234(13) -0.0450(4) 0.0723(9) Uani 0.55(4) d P A 1 C11 C 0.027(5) 0.0666(15) -0.179(4) 0.124(17) Uani 0.55(4) d P A 1 H11A H 0.0116 0.0359 -0.1378 0.100 Uiso 0.55(4) calc PR A 1 H11B H 0.0687 0.0620 -0.2631 0.100 Uiso 0.55(4) calc PR A 1 H11C H -0.0736 0.0832 -0.2064 0.100 Uiso 0.55(4) calc PR A 1 C12 C 0.224(11) 0.1445(14) -0.170(7) 0.25(5) Uani 0.55(4) d P A 1 H12A H 0.2616 0.1737 -0.1194 0.100 Uiso 0.55(4) calc PR A 1 H12B H 0.1322 0.1514 -0.2476 0.100 Uiso 0.55(4) calc PR A 1 H12C H 0.3065 0.1306 -0.2088 0.100 Uiso 0.55(4) calc PR A 1 C13 C 0.319(6) 0.061(2) 0.035(4) 0.127(19) Uani 0.55(4) d P A 1 H13A H 0.2778 0.0289 0.0203 0.100 Uiso 0.55(4) calc PR A 1 H13B H 0.3530 0.0675 0.1375 0.100 Uiso 0.55(4) calc PR A 1 H13C H 0.4078 0.0646 -0.0083 0.100 Uiso 0.55(4) calc PR A 1 P11 P 0.1676(5) 0.10234(13) -0.0450(4) 0.0723(9) Uani 0.45(4) d P A 2 C14 C 0.115(14) 0.0438(16) -0.072(14) 0.54(15) Uani 0.45(4) d P A 2 H14A H 0.0914 0.0368 -0.1743 0.100 Uiso 0.45(4) calc PR A 2 H14B H 0.0228 0.0376 -0.0355 0.100 Uiso 0.45(4) calc PR A 2 H14C H 0.2022 0.0238 -0.0223 0.100 Uiso 0.45(4) calc PR A 2 C15 C 0.160(16) 0.1222(17) -0.214(9) 0.35(10) Uani 0.45(4) d P A 2 H15A H 0.0780 0.1053 -0.2821 0.100 Uiso 0.45(4) calc PR A 2 H15B H 0.2615 0.1166 -0.2368 0.100 Uiso 0.45(4) calc PR A 2 H15C H 0.1373 0.1561 -0.2196 0.100 Uiso 0.45(4) calc PR A 2 C16 C 0.386(5) 0.107(3) 0.011(6) 0.14(2) Uani 0.45(4) d P A 2 H16A H 0.4220 0.0989 0.1121 0.100 Uiso 0.45(4) calc PR A 2 H16B H 0.4192 0.1386 -0.0058 0.100 Uiso 0.45(4) calc PR A 2 H16C H 0.4326 0.0842 -0.0448 0.100 Uiso 0.45(4) calc PR A 2 P2 P -0.1085(4) 0.19234(14) 0.2895(4) 0.0731(9) Uani 0.43(7) d P A 1 C21 C -0.331(8) 0.184(4) 0.232(6) 0.13(3) Uani 0.43(7) d P A 1 H21A H -0.3602 0.1724 0.1343 0.100 Uiso 0.43(7) calc PR A 1 H21B H -0.3827 0.2144 0.2381 0.100 Uiso 0.43(7) calc PR A 1 H21C H -0.3637 0.1613 0.2956 0.100 Uiso 0.43(7) calc PR A 1 C22 C -0.111(14) 0.258(3) 0.247(14) 0.29(9) Uani 0.43(7) d P A 1 H22A H -0.2165 0.2704 0.2406 0.100 Uiso 0.43(7) calc PR A 1 H22B H -0.0838 0.2624 0.1553 0.100 Uiso 0.43(7) calc PR A 1 H22C H -0.0356 0.2743 0.3217 0.100 Uiso 0.43(7) calc PR A 1 C23 C -0.078(4) 0.1716(14) 0.468(3) 0.226(16) Uani 1 d . A 1 H23A H 0.0312 0.1765 0.5186 0.100 Uiso 1 calc R A 1 H23B H -0.1032 0.1378 0.4676 0.100 Uiso 1 calc R A 1 H23C H -0.1466 0.1890 0.5169 0.100 Uiso 1 calc R A 1 P21 P -0.1085(4) 0.19234(14) 0.2895(4) 0.0731(9) Uani 0.57(7) d P A 2 C24 C -0.300(7) 0.206(4) 0.234(8) 0.22(6) Uani 0.57(7) d P A 2 H24A H -0.3542 0.1826 0.1667 0.100 Uiso 0.57(7) calc PR A 2 H24B H -0.3111 0.2374 0.1880 0.100 Uiso 0.57(7) calc PR A 2 H24C H -0.3473 0.2074 0.3165 0.100 Uiso 0.57(7) calc PR A 2 C25 C -0.024(8) 0.2471(18) 0.349(9) 0.21(5) Uani 0.57(7) d P A 2 H25A H -0.0032 0.2647 0.2681 0.100 Uiso 0.57(7) calc PR A 2 H25B H 0.0746 0.2420 0.4200 0.100 Uiso 0.57(7) calc PR A 2 H25C H -0.0960 0.2652 0.3914 0.100 Uiso 0.57(7) calc PR A 2 N N 0.1781(15) 0.1259(5) 0.2851(12) 0.084(3) Uani 1 d . . . C1 C 0.3055(19) 0.1199(6) 0.4168(18) 0.085(4) Uani 1 d . . . C2 C 0.4143(17) 0.1547(7) 0.4704(17) 0.090(5) Uani 1 d . . . H2 H 0.4057 0.1840 0.4213 0.100 Uiso 1 calc R . . C3 C 0.5375(18) 0.1494(7) 0.5937(18) 0.091(5) Uani 1 d . . . H3 H 0.6061 0.1750 0.6274 0.100 Uiso 1 calc R . . C4 C 0.5569(19) 0.1074(9) 0.6638(19) 0.107(6) Uani 1 d . . . H4 H 0.6413 0.1030 0.7447 0.100 Uiso 1 calc R . . C5 C 0.464(3) 0.0271(10) 0.684(2) 0.141(10) Uani 1 d . . . H5 H 0.5476 0.0223 0.7656 0.100 Uiso 1 calc R . . C6 C 0.349(3) -0.0077(9) 0.629(2) 0.119(7) Uani 1 d . . . H6 H 0.3598 -0.0367 0.6797 0.100 Uiso 1 calc R . . C7 C 0.224(2) -0.0049(6) 0.5110(18) 0.090(4) Uani 1 d . . . H7 H 0.1554 -0.0311 0.4852 0.100 Uiso 1 calc R . . C8 C 0.199(2) 0.0365(6) 0.430(2) 0.104(6) Uani 1 d . . . H8 H 0.1155 0.0402 0.3482 0.100 Uiso 1 calc R . . C9 C 0.3230(13) 0.0767(4) 0.4871(11) 0.055(3) Uani 1 d . . . C10 C 0.4415(19) 0.0674(7) 0.6105(14) 0.088(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.0586(3) 0.0601(3) 0.0474(3) 0.0019(2) 0.01686(19) 0.0005(2) Cl1 0.120(3) 0.121(3) 0.081(2) 0.025(2) 0.001(2) 0.038(3) Cl2 0.119(3) 0.091(3) 0.120(3) -0.024(2) 0.068(3) -0.036(2) Cl3 0.110(3) 0.088(3) 0.140(4) -0.018(2) 0.058(3) -0.037(2) P1 0.087(2) 0.076(2) 0.0616(18) -0.0026(16) 0.0342(17) 0.0052(18) C11 0.14(3) 0.13(3) 0.11(3) -0.09(3) 0.04(2) -0.02(2) C12 0.58(13) 0.04(2) 0.24(6) -0.02(3) 0.34(8) -0.03(4) C13 0.14(4) 0.16(4) 0.09(2) 0.02(2) 0.05(2) 0.08(3) P11 0.087(2) 0.076(2) 0.0616(18) -0.0026(16) 0.0342(17) 0.0052(18) C14 0.8(2) 0.04(3) 1.2(3) -0.14(8) 0.9(3) -0.09(6) C15 0.9(3) 0.04(3) 0.28(10) 0.04(4) 0.47(16) 0.06(7) C16 0.11(4) 0.19(6) 0.12(4) -0.05(4) 0.04(3) 0.02(4) P2 0.0643(19) 0.081(2) 0.082(2) -0.0067(18) 0.0326(18) 0.0043(16) C21 0.04(2) 0.27(10) 0.07(3) 0.03(4) 0.001(19) 0.00(4) C22 0.38(18) 0.11(5) 0.5(2) 0.03(9) 0.25(17) 0.10(8) C23 0.22(3) 0.38(5) 0.11(2) -0.05(3) 0.10(2) -0.02(3) P21 0.0643(19) 0.081(2) 0.082(2) -0.0067(18) 0.0326(18) 0.0043(16) C24 0.07(4) 0.37(13) 0.20(6) -0.16(7) 0.00(3) 0.07(6) C25 0.24(6) 0.13(4) 0.37(10) -0.17(6) 0.26(8) -0.10(4) N 0.081(8) 0.118(9) 0.064(7) -0.002(6) 0.040(6) 0.016(7) C1 0.093(10) 0.083(10) 0.097(11) -0.009(8) 0.059(9) -0.011(8) C2 0.059(8) 0.139(15) 0.074(9) -0.023(9) 0.018(7) -0.007(8) C3 0.071(9) 0.124(15) 0.078(10) -0.010(9) 0.019(8) -0.016(9) C4 0.065(9) 0.17(2) 0.085(11) -0.032(12) 0.022(8) 0.019(11) C5 0.147(19) 0.22(3) 0.067(10) 0.042(14) 0.042(12) 0.100(19) C6 0.134(17) 0.133(18) 0.099(15) -0.017(13) 0.046(13) -0.011(14) C7 0.120(13) 0.068(9) 0.087(10) 0.015(7) 0.037(10) 0.017(8) C8 0.142(15) 0.080(10) 0.112(13) 0.006(9) 0.073(12) 0.037(10) C9 0.060(6) 0.067(7) 0.045(5) 0.002(5) 0.028(5) 0.008(5) C10 0.093(10) 0.127(13) 0.052(7) 0.014(8) 0.034(7) 0.048(10) _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 W N 1.707(13) . ? W Cl3 2.379(4) . ? W Cl2 2.407(4) . ? W Cl1 2.451(4) . ? W P1 2.531(3) . ? W P2 2.536(3) . ? P1 C13 1.76(3) . ? P1 C12 1.81(4) . ? P1 C11 1.82(3) . ? P2 C23 1.75(3) . ? P2 C22 1.86(8) . ? P2 C21 1.88(7) . ? N C1 1.46(2) . ? C1 C2 1.36(2) . ? C1 C9 1.365(19) . ? C2 C3 1.39(2) . ? C3 C4 1.33(3) . ? C4 C10 1.49(3) . ? C5 C10 1.31(3) . ? C5 C6 1.39(3) . ? C6 C7 1.36(3) . ? C7 C8 1.37(2) . ? C8 C9 1.55(2) . ? C9 C10 1.380(18) . ? 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 N W Cl3 99.3(5) . . ? N W Cl2 91.2(5) . . ? Cl3 W Cl2 169.44(18) . . ? N W Cl1 173.7(5) . . ? Cl3 W Cl1 86.77(19) . . ? Cl2 W Cl1 82.69(18) . . ? N W P1 95.2(4) . . ? Cl3 W P1 90.08(14) . . ? Cl2 W P1 88.65(13) . . ? Cl1 W P1 86.45(15) . . ? N W P2 91.4(4) . . ? Cl3 W P2 88.51(14) . . ? Cl2 W P2 91.56(13) . . ? Cl1 W P2 87.04(15) . . ? P1 W P2 173.41(12) . . ? C13 P1 C12 115(3) . . ? C13 P1 C11 104(2) . . ? C12 P1 C11 98(3) . . ? C13 P1 W 114.1(11) . . ? C12 P1 W 110.9(12) . . ? C11 P1 W 114.1(12) . . ? C23 P2 C22 122(4) . . ? C23 P2 C21 98(2) . . ? C22 P2 C21 96(5) . . ? C23 P2 W 114.6(11) . . ? C22 P2 W 111(3) . . ? C21 P2 W 114(3) . . ? C1 N W 167.4(12) . . ? C2 C1 C9 117.3(17) . . ? C2 C1 N 123.3(15) . . ? C9 C1 N 119.3(13) . . ? C1 C2 C3 124.1(19) . . ? C4 C3 C2 119.6(17) . . ? C3 C4 C10 119.2(16) . . ? C10 C5 C6 113(2) . . ? C7 C6 C5 129(2) . . ? C6 C7 C8 120(2) . . ? C7 C8 C9 114.0(17) . . ? C1 C9 C10 123.4(14) . . ? C1 C9 C8 118.5(13) . . ? C10 C9 C8 118.0(13) . . ? C5 C10 C9 127(2) . . ? C5 C10 C4 117(2) . . ? C9 C10 C4 116.4(15) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.290 _refine_diff_density_min -2.505 _refine_diff_density_rms 0.196 data_mg188 _audit_creation_method SHELXL-97 _chemical_name_systematic '[W Cl2 (N C6H4 CMe3-2)(P Me3)3]' _chemical_name_common ? _chemical_formula_moiety '[W Cl2 (N C6H4 CMe3-2)(P Me3)3]' _chemical_formula_sum 'C22.50 H43.50 Cl2 N P3 W' _chemical_formula_weight 675.74 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' '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 'Triclinic' _symmetry_space_group_name_H-M 'P(1-bar)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.688 _cell_length_b 9.43090(10) _cell_length_c 19.9949(3) _cell_angle_alpha 90.39 _cell_angle_beta 94.6940(10) _cell_angle_gamma 116.93 _cell_volume 1453.94(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description 'needle' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 677 _exptl_absorpt_coefficient_mu 4.332 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.2303 _exptl_absorpt_correction_T_max 0.5822 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'area detector\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 6288 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.44 _reflns_number_total 6288 _reflns_number_gt 6046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SMART (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _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 w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+3.6560P] 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 6288 _refine_ls_number_parameters 263 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.078 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.581684(17) 0.679488(15) 0.689010(6) 0.01818(5) Uani 1 d . . . Cl1 Cl 0.60630(13) 0.51262(11) 0.59699(5) 0.03016(19) Uani 1 d . . . Cl2 Cl 0.89145(12) 0.74184(12) 0.72224(5) 0.03068(19) Uani 1 d . . . P1 P 0.69929(13) 0.89347(11) 0.60682(5) 0.02538(19) Uani 1 d . . . P2 P 0.50286(13) 0.42790(12) 0.74994(5) 0.0262(2) Uani 1 d . . . P3 P 0.27793(12) 0.58865(12) 0.64009(5) 0.02418(19) Uani 1 d . . . N N 0.5541(4) 0.7933(4) 0.75344(14) 0.0203(6) Uani 1 d . . . C1 C 0.5102(5) 0.8754(4) 0.80155(17) 0.0209(7) Uani 1 d . . . C2 C 0.3403(5) 0.8592(5) 0.7922(2) 0.0274(8) Uani 1 d . . . H2 H 0.2668 0.7991 0.7545 0.033 Uiso 1 calc R . . C3 C 0.2785(5) 0.9296(5) 0.8371(2) 0.0326(9) Uani 1 d . . . H3 H 0.1648 0.9174 0.8298 0.039 Uiso 1 calc R . . C4 C 0.3860(6) 1.0179(5) 0.8927(2) 0.0325(9) Uani 1 d . . . H4 H 0.3452 1.0646 0.9239 0.039 Uiso 1 calc R . . C5 C 0.5540(6) 1.0369(5) 0.90201(19) 0.0294(8) Uani 1 d . . . H5 H 0.6251 1.0982 0.9399 0.035 Uiso 1 calc R . . C6 C 0.6241(5) 0.9699(4) 0.85816(17) 0.0220(7) Uani 1 d . . . C7 C 0.8119(5) 0.9985(4) 0.87191(18) 0.0243(7) Uani 1 d . . . C8 C 0.9138(5) 1.0789(5) 0.8114(2) 0.0296(8) Uani 1 d . . . H8C H 0.8642 1.0079 0.7716 0.044 Uiso 1 calc R . . H8B H 1.0343 1.1019 0.8210 0.044 Uiso 1 calc R . . H8A H 0.9068 1.1773 0.8035 0.044 Uiso 1 calc R . . C9 C 0.8144(5) 0.8387(5) 0.8855(2) 0.0287(8) Uani 1 d . . . H9C H 0.7491 0.7917 0.9234 0.043 Uiso 1 calc R . . H9B H 0.9332 0.8570 0.8955 0.043 Uiso 1 calc R . . H9A H 0.7624 0.7670 0.8460 0.043 Uiso 1 calc R . . C10 C 0.9075(6) 1.1118(6) 0.9341(2) 0.0386(10) Uani 1 d . . . H10C H 0.8462 1.0676 0.9733 0.058 Uiso 1 calc R . . H10B H 0.9115 1.2149 0.9267 0.058 Uiso 1 calc R . . H10A H 1.0246 1.1239 0.9415 0.058 Uiso 1 calc R . . C11 C 0.9305(6) 0.9723(7) 0.5962(3) 0.0503(13) Uani 1 d . . . H11C H 0.9649 1.0608 0.5668 0.076 Uiso 1 calc R . . H11B H 0.9518 0.8893 0.5765 0.076 Uiso 1 calc R . . H11A H 0.9972 1.0085 0.6396 0.076 Uiso 1 calc R . . C12 C 0.6102(6) 0.8491(5) 0.5191(2) 0.0364(9) Uani 1 d . . . H12C H 0.6764 0.9388 0.4927 0.055 Uiso 1 calc R . . H12B H 0.4900 0.8294 0.5155 0.055 Uiso 1 calc R . . H12A H 0.6166 0.7553 0.5023 0.055 Uiso 1 calc R . . C13 C 0.6797(7) 1.0722(5) 0.6290(2) 0.0443(11) Uani 1 d . . . H13C H 0.7284 1.1505 0.5956 0.066 Uiso 1 calc R . . H13B H 0.7421 1.1160 0.6727 0.066 Uiso 1 calc R . . H13A H 0.5583 1.0453 0.6306 0.066 Uiso 1 calc R . . C14 C 0.3459(7) 0.2401(5) 0.7067(2) 0.0416(10) Uani 1 d . . . H14C H 0.3411 0.1519 0.7326 0.062 Uiso 1 calc R . . H14B H 0.3811 0.2321 0.6625 0.062 Uiso 1 calc R . . H14A H 0.2323 0.2368 0.7019 0.062 Uiso 1 calc R . . C15 C 0.4116(6) 0.4257(6) 0.8292(2) 0.0388(10) Uani 1 d . . . H15C H 0.3851 0.3257 0.8501 0.058 Uiso 1 calc R . . H15B H 0.3062 0.4369 0.8207 0.058 Uiso 1 calc R . . H15A H 0.4950 0.5132 0.8590 0.058 Uiso 1 calc R . . C16 C 0.6803(7) 0.3788(6) 0.7746(3) 0.0460(11) Uani 1 d . . . H16C H 0.6362 0.2817 0.7990 0.069 Uiso 1 calc R . . H16B H 0.7696 0.4651 0.8032 0.069 Uiso 1 calc R . . H16A H 0.7288 0.3637 0.7348 0.069 Uiso 1 calc R . . C17 C 0.2119(6) 0.7382(6) 0.6093(2) 0.0390(10) Uani 1 d . . . H17C H 0.0867 0.6890 0.6000 0.059 Uiso 1 calc R . . H17B H 0.2656 0.7803 0.5685 0.059 Uiso 1 calc R . . H17A H 0.2485 0.8241 0.6432 0.059 Uiso 1 calc R . . C18 C 0.1018(5) 0.4801(5) 0.6937(2) 0.0358(9) Uani 1 d . . . H18C H -0.0068 0.4700 0.6718 0.054 Uiso 1 calc R . . H18B H 0.1270 0.5382 0.7366 0.054 Uiso 1 calc R . . H18A H 0.0927 0.3750 0.7007 0.054 Uiso 1 calc R . . C19 C 0.2039(6) 0.4501(6) 0.5663(2) 0.0419(11) Uani 1 d . . . H19C H 0.0816 0.4166 0.5539 0.063 Uiso 1 calc R . . H19B H 0.2214 0.3578 0.5766 0.063 Uiso 1 calc R . . H19A H 0.2696 0.5027 0.5291 0.063 Uiso 1 calc R . . C20 C 0.8417(14) 1.4473(13) 1.0159(5) 0.114(3) Uiso 1 d D . . C21 C 0.8804(12) 1.5138(11) 0.9563(4) 0.092(2) Uiso 1 d D . . H21 H 0.7936 1.5205 0.9272 0.110 Uiso 1 calc R . . C22 C 1.0322(12) 1.5669(12) 0.9393(5) 0.101(3) Uiso 1 d D . . H22 H 1.0608 1.6147 0.8981 0.122 Uiso 1 calc R . . C23 C 0.6831(19) 1.391(2) 1.0346(8) 0.083(4) Uiso 0.50 d PD . . H23D H 0.6798 1.3470 1.0785 0.125 Uiso 0.50 calc PR . . H23A H 0.6029 1.3079 1.0023 0.125 Uiso 0.50 calc PR . . H23B H 0.6501 1.4761 1.0367 0.125 Uiso 0.50 calc PR . . 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 W 0.01794(8) 0.01889(8) 0.01947(8) -0.00137(5) 0.00218(5) 0.00987(6) Cl1 0.0365(5) 0.0307(5) 0.0264(4) -0.0063(3) 0.0055(4) 0.0177(4) Cl2 0.0216(4) 0.0393(5) 0.0353(5) -0.0042(4) -0.0002(3) 0.0180(4) P1 0.0268(5) 0.0216(4) 0.0258(5) 0.0014(4) 0.0022(4) 0.0093(4) P2 0.0304(5) 0.0244(5) 0.0269(5) 0.0035(4) 0.0049(4) 0.0147(4) P3 0.0197(4) 0.0271(5) 0.0251(4) -0.0015(4) 0.0009(3) 0.0103(4) N 0.0195(14) 0.0224(14) 0.0208(14) -0.0009(11) 0.0008(11) 0.0113(12) C1 0.0210(17) 0.0219(16) 0.0235(16) 0.0008(13) 0.0047(13) 0.0126(14) C2 0.0227(18) 0.033(2) 0.0302(19) -0.0039(15) 0.0024(14) 0.0157(16) C3 0.029(2) 0.040(2) 0.039(2) 0.0016(17) 0.0102(16) 0.0230(18) C4 0.037(2) 0.037(2) 0.034(2) -0.0018(17) 0.0115(17) 0.0257(19) C5 0.037(2) 0.0307(19) 0.0232(18) -0.0046(15) 0.0028(15) 0.0175(17) C6 0.0281(18) 0.0196(16) 0.0208(16) 0.0003(13) 0.0034(13) 0.0129(14) C7 0.0246(18) 0.0236(17) 0.0247(17) -0.0034(14) -0.0003(14) 0.0115(15) C8 0.0233(18) 0.0268(19) 0.037(2) 0.0020(16) 0.0044(15) 0.0096(15) C9 0.030(2) 0.0306(19) 0.0300(19) 0.0021(15) 0.0017(15) 0.0178(17) C10 0.036(2) 0.040(2) 0.038(2) -0.0132(19) -0.0099(18) 0.018(2) C11 0.030(2) 0.051(3) 0.061(3) 0.022(2) 0.011(2) 0.009(2) C12 0.044(2) 0.036(2) 0.0252(19) 0.0032(16) 0.0032(17) 0.0145(19) C13 0.063(3) 0.030(2) 0.041(2) 0.0003(18) 0.002(2) 0.023(2) C14 0.052(3) 0.0214(19) 0.047(3) 0.0026(18) 0.006(2) 0.0132(19) C15 0.045(3) 0.037(2) 0.034(2) 0.0066(18) 0.0120(19) 0.017(2) C16 0.049(3) 0.048(3) 0.055(3) 0.020(2) 0.010(2) 0.034(2) C17 0.036(2) 0.053(3) 0.039(2) 0.010(2) 0.0029(18) 0.030(2) C18 0.0239(19) 0.036(2) 0.046(2) 0.0023(18) 0.0091(17) 0.0116(17) C19 0.031(2) 0.053(3) 0.036(2) -0.018(2) -0.0067(17) 0.016(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 W N 1.770(3) . ? W P3 2.4845(10) . ? W Cl1 2.4974(9) . ? W P1 2.5039(10) . ? W P2 2.5074(10) . ? W Cl2 2.5096(9) . ? P1 C12 1.824(4) . ? P1 C13 1.825(5) . ? P1 C11 1.831(5) . ? P2 C15 1.826(4) . ? P2 C14 1.828(5) . ? P2 C16 1.833(5) . ? P3 C19 1.832(4) . ? P3 C17 1.840(4) . ? P3 C18 1.844(4) . ? N C1 1.409(4) . ? C1 C2 1.410(5) . ? C1 C6 1.435(5) . ? C2 C3 1.389(5) . ? C3 C4 1.384(6) . ? C4 C5 1.384(6) . ? C5 C6 1.403(5) . ? C6 C7 1.528(5) . ? C7 C9 1.542(5) . ? C7 C10 1.546(5) . ? C7 C8 1.551(5) . ? C20 C23 1.321(14) . ? C20 C21 1.347(11) . ? C20 C22 1.412(10) 2_787 ? C21 C22 1.257(10) . ? C22 C20 1.412(10) 2_787 ? 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 N W P3 91.09(10) . . ? N W Cl1 177.45(10) . . ? P3 W Cl1 86.45(3) . . ? N W P1 98.03(10) . . ? P3 W P1 92.57(3) . . ? Cl1 W P1 82.75(3) . . ? N W P2 98.16(10) . . ? P3 W P2 92.33(3) . . ? Cl1 W P2 81.31(3) . . ? P1 W P2 162.99(3) . . ? N W Cl2 98.85(10) . . ? P3 W Cl2 170.07(3) . . ? Cl1 W Cl2 83.62(3) . . ? P1 W Cl2 86.20(3) . . ? P2 W Cl2 86.17(3) . . ? C12 P1 C13 103.4(2) . . ? C12 P1 C11 99.8(2) . . ? C13 P1 C11 102.7(3) . . ? C12 P1 W 118.95(15) . . ? C13 P1 W 113.57(17) . . ? C11 P1 W 116.16(17) . . ? C15 P2 C14 103.2(2) . . ? C15 P2 C16 102.8(2) . . ? C14 P2 C16 100.2(2) . . ? C15 P2 W 113.97(15) . . ? C14 P2 W 118.03(16) . . ? C16 P2 W 116.40(17) . . ? C19 P3 C17 100.0(2) . . ? C19 P3 C18 100.1(2) . . ? C17 P3 C18 99.4(2) . . ? C19 P3 W 116.93(15) . . ? C17 P3 W 118.75(16) . . ? C18 P3 W 118.10(15) . . ? C1 N W 172.9(3) . . ? N C1 C2 115.9(3) . . ? N C1 C6 124.8(3) . . ? C2 C1 C6 119.3(3) . . ? C3 C2 C1 121.8(4) . . ? C4 C3 C2 119.3(4) . . ? C3 C4 C5 119.6(3) . . ? C4 C5 C6 123.7(4) . . ? C5 C6 C1 116.3(3) . . ? C5 C6 C7 120.3(3) . . ? C1 C6 C7 123.5(3) . . ? C6 C7 C9 109.3(3) . . ? C6 C7 C10 112.5(3) . . ? C9 C7 C10 107.3(3) . . ? C6 C7 C8 109.5(3) . . ? C9 C7 C8 111.7(3) . . ? C10 C7 C8 106.5(3) . . ? C23 C20 C21 121.2(12) . . ? C23 C20 C22 117.2(12) . 2_787 ? C21 C20 C22 121.6(10) . 2_787 ? C22 C21 C20 120.3(10) . . ? C21 C22 C20 118.1(10) . 2_787 ? 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 N W P1 C11 107.7(2) . . . . ? N W P1 C12 -133.1(2) . . . . ? N W P1 C13 -11.1(2) . . . . ? N W P2 C14 131.0(2) . . . . ? N W P2 C15 9.6(2) . . . . ? N W P2 C16 -109.9(2) . . . . ? N W P3 C17 61.5(2) . . . . ? N W P3 C18 -58.76(19) . . . . ? N W P3 C19 -178.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 2.059 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.114 data_mg2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[W Cl2 (N C6 H4 Ph-2) (P Me3)3]' ; _chemical_name_common '[W Cl2 (N C6 H4 Ph-2) (P Me3)3]' _chemical_formula_moiety ? _chemical_formula_sum 'C21 H36 Cl2 N P3 W' _chemical_formula_weight 650.17 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' '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 'Orthorhombic' _symmetry_space_group_name_H-M 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.10570(10) _cell_length_b 15.04740(10) _cell_length_c 19.80710(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2713.91(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description 'tablet' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 4.638 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process-details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.2584 _exptl_absorpt_correction_T_max 0.7079 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemen's SMART diffractometer' _diffrn_measurement_method 'area detector\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6009 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6009 _reflns_number_gt 5817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SMART (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(4) _refine_ls_number_reflns 6009 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.114 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.346283(13) 1.035522(7) 0.708089(6) 0.02101(4) Uani 1 d . . . Cl1 Cl 0.16130(10) 0.98678(5) 0.79361(5) 0.03542(18) Uani 1 d . . . Cl2 Cl 0.42600(9) 0.87715(5) 0.71094(5) 0.03548(19) Uani 1 d . . . P2 P 0.52673(10) 1.04627(5) 0.80385(5) 0.02802(18) Uani 1 d . . . P1 P 0.17525(10) 0.98722(6) 0.61636(5) 0.0312(2) Uani 1 d . . . P3 P 0.21199(10) 1.17522(5) 0.72616(5) 0.02677(19) Uani 1 d . . . N N 0.4757(3) 1.08483(17) 0.65341(14) 0.0243(6) Uani 1 d . . . C1 C 0.5814(3) 1.1333(2) 0.61814(18) 0.0252(7) Uani 1 d . . . C2 C 0.6306(4) 1.2146(2) 0.6456(2) 0.0313(8) Uani 1 d . . . H2 H 0.5935 1.2341 0.6873 0.038 Uiso 1 calc R . . C3 C 0.7328(4) 1.2661(2) 0.6115(2) 0.0384(9) Uani 1 d . . . H3 H 0.7653 1.3199 0.6304 0.046 Uiso 1 calc R . . C4 C 0.7871(4) 1.2384(2) 0.5498(2) 0.0435(10) Uani 1 d . . . H4 H 0.8555 1.2736 0.5264 0.052 Uiso 1 calc R . . C5 C 0.7398(4) 1.1581(2) 0.5226(2) 0.0394(9) Uani 1 d . . . H5 H 0.7759 1.1402 0.4803 0.047 Uiso 1 calc R . . C6 C 0.6403(4) 1.1036(2) 0.55637(17) 0.0275(7) Uani 1 d . . . C7 C 0.6066(3) 1.0144(2) 0.52698(19) 0.0273(7) Uani 1 d . . . C8 C 0.5614(4) 1.0061(2) 0.4598(2) 0.0368(9) Uani 1 d . . . H8 H 0.5441 1.0574 0.4339 0.044 Uiso 1 calc R . . C9 C 0.5420(5) 0.9229(3) 0.4312(2) 0.0429(10) Uani 1 d . . . H9 H 0.5091 0.9178 0.3864 0.052 Uiso 1 calc R . . C10 C 0.5712(4) 0.8474(3) 0.4687(2) 0.0417(9) Uani 1 d . . . H10 H 0.5609 0.7909 0.4489 0.050 Uiso 1 calc R . . C11 C 0.6150(4) 0.8548(2) 0.5348(2) 0.0383(9) Uani 1 d . . . H11 H 0.6347 0.8032 0.5600 0.046 Uiso 1 calc R . . C12 C 0.6306(4) 0.9374(2) 0.56464(19) 0.0308(8) Uani 1 d . . . H12 H 0.6574 0.9417 0.6104 0.037 Uiso 1 calc R . . C16 C 0.5757(6) 1.1476(3) 0.8493(3) 0.0586(14) Uani 1 d . . . H16A H 0.6581 1.1357 0.8789 0.088 Uiso 1 calc R . . H16B H 0.4924 1.1675 0.8758 0.088 Uiso 1 calc R . . H16C H 0.6025 1.1935 0.8172 0.088 Uiso 1 calc R . . C17 C 0.4954(4) 0.9710(3) 0.8735(2) 0.0449(9) Uani 1 d . . . H17A H 0.5763 0.9751 0.9052 0.067 Uiso 1 calc R . . H17B H 0.4884 0.9106 0.8565 0.067 Uiso 1 calc R . . H17C H 0.4046 0.9867 0.8961 0.067 Uiso 1 calc R . . C18 C 0.7054(4) 1.0116(3) 0.7724(2) 0.0433(10) Uani 1 d . . . H18A H 0.7756 1.0114 0.8093 0.065 Uiso 1 calc R . . H18B H 0.7379 1.0526 0.7377 0.065 Uiso 1 calc R . . H18C H 0.6979 0.9523 0.7536 0.065 Uiso 1 calc R . . C13 C 0.2377(5) 0.8969(3) 0.5629(3) 0.0619(14) Uani 1 d . . . H13A H 0.1638 0.8843 0.5289 0.093 Uiso 1 calc R . . H13B H 0.2540 0.8443 0.5902 0.093 Uiso 1 calc R . . H13C H 0.3287 0.9137 0.5409 0.093 Uiso 1 calc R . . C14 C -0.0122(8) 0.9634(6) 0.6370(4) 0.0388(17) Uiso 0.50 d P A 1 H14A H -0.0567 0.9296 0.6007 0.058 Uiso 0.50 calc PR A 1 H14B H -0.0654 1.0186 0.6432 0.058 Uiso 0.50 calc PR A 1 H14C H -0.0159 0.9290 0.6784 0.058 Uiso 0.50 calc PR A 1 C15 C 0.1632(11) 1.0701(6) 0.5488(5) 0.045(2) Uiso 0.50 d P A 1 H15A H 0.1121 1.0447 0.5104 0.067 Uiso 0.50 calc PR A 1 H15B H 0.2613 1.0878 0.5353 0.067 Uiso 0.50 calc PR A 1 H15C H 0.1097 1.1216 0.5650 0.067 Uiso 0.50 calc PR A 1 C19 C 0.2509(5) 1.2627(2) 0.6654(3) 0.0504(12) Uani 1 d . . . H19A H 0.1811 1.3108 0.6712 0.076 Uiso 1 calc R . . H19B H 0.2428 1.2391 0.6200 0.076 Uiso 1 calc R . . H19C H 0.3497 1.2849 0.6726 0.076 Uiso 1 calc R . . C20 C 0.2356(4) 1.2339(3) 0.8063(2) 0.0456(11) Uani 1 d . . . H20A H 0.1663 1.2828 0.8088 0.068 Uiso 1 calc R . . H20B H 0.3349 1.2569 0.8092 0.068 Uiso 1 calc R . . H20C H 0.2180 1.1932 0.8434 0.068 Uiso 1 calc R . . C21 C 0.0110(4) 1.1724(3) 0.7234(2) 0.0398(9) Uani 1 d . . . H21A H -0.0273 1.2316 0.7317 0.060 Uiso 1 calc R . . H21B H -0.0252 1.1321 0.7578 0.060 Uiso 1 calc R . . H21C H -0.0209 1.1520 0.6793 0.060 Uiso 1 calc R . . C22 C 0.0112(10) 0.9255(6) 0.6472(5) 0.046(2) Uiso 0.50 d P A 2 H22A H -0.0377 0.8973 0.6094 0.068 Uiso 0.50 calc PR A 2 H22B H -0.0559 0.9666 0.6689 0.068 Uiso 0.50 calc PR A 2 H22C H 0.0417 0.8806 0.6794 0.068 Uiso 0.50 calc PR A 2 C23 C 0.0972(13) 1.0664(7) 0.5578(6) 0.061(3) Uiso 0.50 d P A 2 H23A H 0.0328 1.0357 0.5266 0.092 Uiso 0.50 calc PR A 2 H23B H 0.1755 1.0953 0.5329 0.092 Uiso 0.50 calc PR A 2 H23C H 0.0415 1.1106 0.5826 0.092 Uiso 0.50 calc PR 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 W 0.02412(6) 0.01830(5) 0.02060(6) 0.00021(5) 0.00203(5) -0.00059(5) Cl1 0.0364(4) 0.0349(4) 0.0350(5) 0.0065(4) 0.0119(5) -0.0003(3) Cl2 0.0469(5) 0.0201(3) 0.0394(5) 0.0002(4) 0.0054(5) 0.0038(3) P2 0.0327(4) 0.0234(4) 0.0279(5) 0.0020(4) -0.0043(3) 0.0013(3) P1 0.0292(5) 0.0351(5) 0.0294(5) -0.0049(4) -0.0014(4) -0.0047(3) P3 0.0263(4) 0.0232(4) 0.0308(5) 0.0003(3) 0.0017(3) 0.0023(3) N 0.0257(14) 0.0269(13) 0.0202(14) -0.0014(11) 0.0018(11) -0.0009(11) C1 0.0234(15) 0.0239(14) 0.0282(18) 0.0044(14) -0.0013(13) 0.0010(12) C2 0.0313(19) 0.0263(15) 0.036(2) 0.0002(15) 0.0009(15) -0.0003(13) C3 0.035(2) 0.0246(16) 0.056(3) 0.0036(18) -0.0059(18) -0.0026(14) C4 0.037(2) 0.0312(18) 0.062(3) 0.0127(19) 0.013(2) -0.0057(16) C5 0.041(2) 0.0388(19) 0.039(2) 0.0076(18) 0.0134(17) 0.0019(17) C6 0.0287(17) 0.0263(14) 0.0277(17) 0.0040(14) 0.0015(15) 0.0019(15) C7 0.0262(16) 0.0288(17) 0.0270(18) 0.0013(14) 0.0043(13) 0.0033(12) C8 0.043(2) 0.0365(18) 0.031(2) 0.0073(17) 0.0002(17) 0.0081(16) C9 0.046(2) 0.055(2) 0.028(2) -0.0093(19) -0.0039(17) 0.0059(19) C10 0.049(2) 0.0359(19) 0.040(2) -0.0094(18) 0.0003(18) 0.0045(17) C11 0.046(2) 0.0318(17) 0.037(2) 0.0046(17) -0.0010(17) 0.0052(15) C12 0.033(2) 0.0321(16) 0.0272(18) 0.0002(14) -0.0005(14) 0.0034(14) C16 0.076(3) 0.036(2) 0.064(3) -0.015(2) -0.042(3) 0.010(2) C17 0.050(2) 0.051(2) 0.034(2) 0.014(2) -0.0010(17) 0.004(2) C18 0.0296(18) 0.053(2) 0.047(2) 0.0064(19) -0.0026(16) -0.0014(16) C13 0.050(3) 0.068(3) 0.068(3) -0.043(3) -0.013(2) -0.001(2) C19 0.058(3) 0.0296(18) 0.063(3) 0.019(2) 0.012(2) 0.0093(18) C20 0.041(2) 0.042(2) 0.054(3) -0.022(2) -0.0014(19) 0.0099(17) C21 0.0289(18) 0.0398(19) 0.051(3) -0.0035(19) -0.0041(16) 0.0074(15) _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 W N 1.764(3) . ? W P3 2.4581(8) . ? W Cl2 2.4918(7) . ? W Cl1 2.4989(8) . ? W P1 2.5010(10) . ? W P2 2.5148(9) . ? P2 C17 1.808(4) . ? P2 C18 1.818(4) . ? P2 C16 1.826(4) . ? P1 C14 1.791(8) . ? P1 C23 1.808(11) . ? P1 C13 1.815(4) . ? P1 C15 1.832(9) . ? P1 C22 1.862(9) . ? P3 C19 1.818(4) . ? P3 C20 1.829(4) . ? P3 C21 1.831(4) . ? N C1 1.394(4) . ? C1 C6 1.408(5) . ? C1 C2 1.412(5) . ? C2 C3 1.386(5) . ? C3 C4 1.383(6) . ? C4 C5 1.391(5) . ? C5 C6 1.393(5) . ? C6 C7 1.495(5) . ? C7 C12 1.395(5) . ? C7 C8 1.398(5) . ? C8 C9 1.386(5) . ? C9 C10 1.384(6) . ? C10 C11 1.373(6) . ? C11 C12 1.384(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 N W P3 93.57(9) . . ? N W Cl2 102.79(9) . . ? P3 W Cl2 163.63(3) . . ? N W Cl1 171.84(9) . . ? P3 W Cl1 79.45(3) . . ? Cl2 W Cl1 84.28(3) . . ? N W P1 95.29(9) . . ? P3 W P1 92.55(3) . . ? Cl2 W P1 85.41(3) . . ? Cl1 W P1 89.28(3) . . ? N W P2 89.97(9) . . ? P3 W P2 99.22(3) . . ? Cl2 W P2 81.61(3) . . ? Cl1 W P2 87.02(3) . . ? P1 W P2 166.79(3) . . ? C17 P2 C18 102.85(19) . . ? C17 P2 C16 100.7(2) . . ? C18 P2 C16 101.0(2) . . ? C17 P2 W 115.59(14) . . ? C18 P2 W 107.93(14) . . ? C16 P2 W 125.79(14) . . ? C14 P1 C23 84.5(5) . . ? C14 P1 C13 106.4(3) . . ? C23 P1 C13 104.0(5) . . ? C14 P1 C15 104.2(4) . . ? C23 P1 C15 19.9(4) . . ? C13 P1 C15 95.9(3) . . ? C14 P1 C22 20.1(3) . . ? C23 P1 C22 102.9(5) . . ? C13 P1 C22 94.0(3) . . ? C15 P1 C22 122.1(4) . . ? C14 P1 W 119.0(3) . . ? C23 P1 W 121.3(4) . . ? C13 P1 W 116.53(15) . . ? C15 P1 W 111.7(3) . . ? C22 P1 W 114.0(3) . . ? C19 P3 C20 101.7(2) . . ? C19 P3 C21 101.1(2) . . ? C20 P3 C21 98.86(19) . . ? C19 P3 W 115.19(14) . . ? C20 P3 W 118.74(13) . . ? C21 P3 W 118.23(13) . . ? C1 N W 171.2(2) . . ? N C1 C6 122.2(3) . . ? N C1 C2 118.6(3) . . ? C6 C1 C2 119.2(3) . . ? C3 C2 C1 120.7(4) . . ? C4 C3 C2 120.1(3) . . ? C3 C4 C5 119.5(4) . . ? C4 C5 C6 121.8(4) . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C7 118.4(3) . . ? C1 C6 C7 123.0(3) . . ? C12 C7 C8 118.8(3) . . ? C12 C7 C6 120.4(3) . . ? C8 C7 C6 120.7(3) . . ? C9 C8 C7 120.5(3) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 120.0(4) . . ? C10 C11 C12 120.7(4) . . ? C11 C12 C7 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.701 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.096 data_mg448 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Ta Cl4 (N C6 H4 CMe3-2)(py)].pyH.C H2 Cl2' ; _chemical_name_common ? _chemical_formula_moiety '[Ta Cl4 (N C6 H4 CMe3-2)(py)].pyH.C H2 Cl2' _chemical_formula_sum 'C21 H26 Cl6 N3 Ta' _chemical_formula_weight 714.10 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' 'Ta' 'Ta' -0.7052 6.5227 '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-bar)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.34720(10) _cell_length_b 10.0506(2) _cell_length_c 16.8679(2) _cell_angle_alpha 100.66 _cell_angle_beta 93.2530(10) _cell_angle_gamma 93.4750(10) _cell_volume 1384.82(4) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description 'tablet' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 4.562 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.3616 _exptl_absorpt_correction_T_max 0.7714 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'area detector\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 6022 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6022 _reflns_number_gt 5279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SMART (Siemens 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _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 w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+3.2773P] 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 6022 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta 0.71483(3) 0.81613(2) 0.634168(14) 0.02823(10) Uani 1 d . . . Cl1 Cl 0.98851(18) 0.81420(17) 0.68392(10) 0.0383(3) Uani 1 d . . . Cl2 Cl 0.7814(2) 1.00856(16) 0.57151(10) 0.0397(3) Uani 1 d . . . Cl3 Cl 0.6519(2) 0.59362(16) 0.66479(10) 0.0395(3) Uani 1 d . . . Cl4 Cl 0.46214(18) 0.78730(17) 0.55009(9) 0.0377(3) Uani 1 d . . . N1 N 0.6373(6) 0.9045(6) 0.7236(3) 0.0327(11) Uani 1 d . . . N2 N 0.8140(6) 0.6853(5) 0.5128(3) 0.0292(10) Uani 1 d . . . C1 C 0.5442(7) 0.9475(7) 0.7886(4) 0.0329(13) Uani 1 d . . . C2 C 0.3974(8) 0.8696(8) 0.7890(4) 0.0419(16) Uani 1 d . . . H2A H 0.3696 0.7948 0.7471 0.050 Uiso 1 calc R . . C3 C 0.2945(8) 0.9008(10) 0.8494(4) 0.053(2) Uani 1 d . . . H3A H 0.1983 0.8471 0.8494 0.064 Uiso 1 calc R . . C4 C 0.3342(9) 1.0112(10) 0.9095(4) 0.058(2) Uani 1 d . . . H4A H 0.2629 1.0357 0.9500 0.069 Uiso 1 calc R . . C5 C 0.4780(9) 1.0868(9) 0.9111(4) 0.051(2) Uani 1 d . . . H5A H 0.5026 1.1606 0.9540 0.061 Uiso 1 calc R . . C6 C 0.5894(7) 1.0598(8) 0.8525(4) 0.0382(15) Uani 1 d . . . C7 C 0.7513(8) 1.1422(7) 0.8596(4) 0.0392(15) Uani 1 d . . . C8 C 0.8857(8) 1.0484(8) 0.8699(4) 0.0447(17) Uani 1 d . . . H8A H 0.8770 0.9724 0.8247 0.067 Uiso 1 calc R . . H8B H 0.8759 1.0150 0.9199 0.067 Uiso 1 calc R . . H8C H 0.9893 1.0984 0.8716 0.067 Uiso 1 calc R . . C9 C 0.7675(10) 1.2600(9) 0.9337(5) 0.057(2) Uani 1 d . . . H9A H 0.7575 1.2234 0.9827 0.085 Uiso 1 calc R . . H9B H 0.6833 1.3210 0.9289 0.085 Uiso 1 calc R . . H9C H 0.8718 1.3092 0.9361 0.085 Uiso 1 calc R . . C10 C 0.7741(10) 1.2055(8) 0.7844(5) 0.0517(18) Uani 1 d . . . H10A H 0.7633 1.1346 0.7365 0.077 Uiso 1 calc R . . H10B H 0.8803 1.2523 0.7889 0.077 Uiso 1 calc R . . H10C H 0.6931 1.2697 0.7804 0.077 Uiso 1 calc R . . C11 C 0.7497(7) 0.5618(7) 0.4771(4) 0.0343(13) Uani 1 d . . . H11A H 0.6567 0.5270 0.4975 0.041 Uiso 1 calc R . . C12 C 0.8135(8) 0.4828(7) 0.4118(4) 0.0396(15) Uani 1 d . . . H12A H 0.7650 0.3964 0.3888 0.048 Uiso 1 calc R . . C13 C 0.9498(8) 0.5334(7) 0.3810(4) 0.0396(15) Uani 1 d . . . H13A H 0.9960 0.4819 0.3370 0.048 Uiso 1 calc R . . C14 C 1.0161(8) 0.6607(7) 0.4163(4) 0.0389(15) Uani 1 d . . . H14A H 1.1077 0.6983 0.3962 0.047 Uiso 1 calc R . . C15 C 0.9460(8) 0.7323(7) 0.4815(4) 0.0351(13) Uani 1 d . . . H15A H 0.9931 0.8188 0.5054 0.042 Uiso 1 calc R . . N3 N 0.6141(8) 0.8613(7) 0.3806(4) 0.0546(17) Uani 1 d . . . H3B H 0.5764 0.9011 0.4252 0.066 Uiso 1 calc R . . C16 C 0.7243(10) 0.9304(8) 0.3474(5) 0.0503(18) Uani 1 d . . . H16A H 0.7599 1.0200 0.3717 0.060 Uiso 1 calc R . . C17 C 0.7851(10) 0.8694(8) 0.2773(5) 0.0527(19) Uani 1 d . . . H17A H 0.8634 0.9163 0.2529 0.063 Uiso 1 calc R . . C18 C 0.7310(10) 0.7400(9) 0.2434(5) 0.058(2) Uani 1 d . . . H18A H 0.7707 0.6974 0.1948 0.069 Uiso 1 calc R . . C19 C 0.6176(10) 0.6709(9) 0.2802(5) 0.056(2) Uani 1 d . . . H19A H 0.5819 0.5807 0.2575 0.067 Uiso 1 calc R . . C20 C 0.5583(9) 0.7344(9) 0.3492(5) 0.0508(19) Uani 1 d . . . H20A H 0.4792 0.6898 0.3744 0.061 Uiso 1 calc R . . Cl5 Cl 0.1527(9) 0.3200(6) 0.0590(4) 0.207(3) Uani 1 d . . . Cl6 Cl 0.4756(7) 0.4118(5) 0.0932(3) 0.1381(16) Uani 1 d . . . C21 C 0.314(2) 0.3127(18) 0.1133(13) 0.146(7) Uani 1 d . . . H21A H 0.3424 0.2182 0.1052 0.176 Uiso 1 calc R . . H21B H 0.2929 0.3404 0.1703 0.176 Uiso 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 Ta 0.02540(13) 0.02987(15) 0.02915(14) 0.00391(9) 0.00775(9) -0.00048(9) Cl1 0.0273(7) 0.0403(8) 0.0437(8) -0.0011(7) 0.0022(6) 0.0018(6) Cl2 0.0474(9) 0.0312(8) 0.0421(8) 0.0087(6) 0.0155(7) -0.0008(6) Cl3 0.0436(8) 0.0351(8) 0.0409(8) 0.0101(6) 0.0112(7) -0.0049(6) Cl4 0.0282(7) 0.0478(9) 0.0362(8) 0.0056(7) 0.0040(6) 0.0011(6) N1 0.026(2) 0.041(3) 0.033(3) 0.009(2) 0.005(2) 0.004(2) N2 0.029(2) 0.031(3) 0.029(2) 0.007(2) 0.0070(19) 0.0028(19) C1 0.025(3) 0.051(4) 0.026(3) 0.011(3) 0.008(2) 0.008(3) C2 0.027(3) 0.063(5) 0.036(3) 0.011(3) 0.004(3) -0.002(3) C3 0.029(3) 0.093(6) 0.042(4) 0.020(4) 0.012(3) 0.004(4) C4 0.037(4) 0.105(7) 0.031(4) 0.009(4) 0.009(3) 0.017(4) C5 0.037(4) 0.081(6) 0.031(3) -0.003(3) 0.007(3) 0.016(4) C6 0.026(3) 0.054(4) 0.033(3) 0.003(3) 0.006(2) 0.012(3) C7 0.037(3) 0.041(4) 0.036(3) -0.005(3) 0.002(3) 0.005(3) C8 0.030(3) 0.058(5) 0.042(4) 0.000(3) -0.003(3) 0.003(3) C9 0.056(5) 0.060(5) 0.044(4) -0.013(4) -0.004(4) 0.002(4) C10 0.056(5) 0.050(4) 0.046(4) 0.004(3) -0.001(3) -0.005(3) C11 0.027(3) 0.036(3) 0.039(3) 0.003(3) 0.006(2) -0.002(2) C12 0.038(3) 0.036(4) 0.043(4) 0.001(3) 0.005(3) 0.000(3) C13 0.045(4) 0.032(3) 0.042(4) 0.004(3) 0.017(3) 0.008(3) C14 0.033(3) 0.041(4) 0.043(4) 0.006(3) 0.017(3) 0.001(3) C15 0.032(3) 0.031(3) 0.043(3) 0.007(3) 0.010(3) -0.001(2) N3 0.056(4) 0.067(5) 0.038(3) 0.000(3) 0.019(3) 0.000(3) C16 0.059(5) 0.038(4) 0.053(4) 0.007(3) 0.018(4) -0.004(3) C17 0.059(5) 0.047(4) 0.057(5) 0.015(4) 0.026(4) 0.002(4) C18 0.056(5) 0.056(5) 0.059(5) -0.001(4) 0.022(4) 0.001(4) C19 0.056(5) 0.048(5) 0.060(5) 0.004(4) 0.001(4) -0.007(4) C20 0.047(4) 0.062(5) 0.044(4) 0.017(4) 0.004(3) -0.015(4) Cl5 0.233(7) 0.148(5) 0.225(6) 0.034(4) -0.129(6) 0.023(4) Cl6 0.199(5) 0.112(3) 0.104(3) 0.007(2) 0.031(3) 0.039(3) C21 0.148(16) 0.111(13) 0.172(17) 0.024(12) -0.017(14) -0.028(11) _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 Ta N1 1.779(5) . ? Ta Cl1 2.3910(15) . ? Ta Cl2 2.4204(16) . ? Ta Cl3 2.4205(16) . ? Ta N2 2.437(5) . ? Ta Cl4 2.4451(15) . ? N1 C1 1.399(7) . ? N2 C11 1.341(8) . ? N2 C15 1.346(8) . ? C1 C2 1.415(9) . ? C1 C6 1.425(9) . ? C2 C3 1.374(9) . ? C3 C4 1.368(12) . ? C4 C5 1.378(12) . ? C5 C6 1.397(9) . ? C6 C7 1.528(10) . ? C7 C8 1.531(9) . ? C7 C10 1.537(10) . ? C7 C9 1.548(9) . ? C11 C12 1.387(9) . ? C12 C13 1.385(10) . ? C13 C14 1.376(10) . ? C14 C15 1.378(9) . ? N3 C16 1.330(10) . ? N3 C20 1.332(10) . ? C16 C17 1.366(11) . ? C17 C18 1.359(11) . ? C18 C19 1.382(12) . ? C19 C20 1.355(12) . ? Cl5 C21 1.598(19) . ? Cl6 C21 1.714(18) . ? 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 Ta Cl1 98.79(16) . . ? N1 Ta Cl2 98.56(18) . . ? Cl1 Ta Cl2 91.15(6) . . ? N1 Ta Cl3 94.33(18) . . ? Cl1 Ta Cl3 91.06(6) . . ? Cl2 Ta Cl3 166.44(6) . . ? N1 Ta N2 177.3(2) . . ? Cl1 Ta N2 82.07(12) . . ? Cl2 Ta N2 83.98(12) . . ? Cl3 Ta N2 83.07(12) . . ? N1 Ta Cl4 96.43(16) . . ? Cl1 Ta Cl4 164.77(5) . . ? Cl2 Ta Cl4 86.20(6) . . ? Cl3 Ta Cl4 88.18(6) . . ? N2 Ta Cl4 82.74(12) . . ? C1 N1 Ta 165.1(5) . . ? C11 N2 C15 116.7(5) . . ? C11 N2 Ta 123.2(4) . . ? C15 N2 Ta 120.0(4) . . ? N1 C1 C2 115.5(6) . . ? N1 C1 C6 124.5(6) . . ? C2 C1 C6 120.0(6) . . ? C3 C2 C1 121.5(7) . . ? C4 C3 C2 119.0(7) . . ? C3 C4 C5 120.4(7) . . ? C4 C5 C6 123.7(7) . . ? C5 C6 C1 115.4(6) . . ? C5 C6 C7 121.5(6) . . ? C1 C6 C7 123.0(5) . . ? C6 C7 C8 108.7(6) . . ? C6 C7 C10 111.1(6) . . ? C8 C7 C10 109.9(6) . . ? C6 C7 C9 112.2(6) . . ? C8 C7 C9 107.7(6) . . ? C10 C7 C9 107.1(7) . . ? N2 C11 C12 123.3(6) . . ? C13 C12 C11 118.9(6) . . ? C14 C13 C12 118.6(6) . . ? C13 C14 C15 119.0(6) . . ? N2 C15 C14 123.6(6) . . ? C16 N3 C20 123.5(7) . . ? N3 C16 C17 119.0(7) . . ? C18 C17 C16 119.2(7) . . ? C17 C18 C19 120.1(8) . . ? C20 C19 C18 119.4(8) . . ? N3 C20 C19 118.7(7) . . ? Cl5 C21 Cl6 114.6(12) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 3.214 _refine_diff_density_min -2.118 _refine_diff_density_rms 0.176