# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1540 data_VG9713 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H49 N2 O F5 Mo' _chemical_formula_weight 860.83 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -0.0483 2.7339 '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 11.809(3) _cell_length_b 11.9047(14) _cell_length_c 16.348(3) _cell_angle_alpha 87.302(12) _cell_angle_beta 81.012(15) _cell_angle_gamma 66.879(11) _cell_volume 2087.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.39 _exptl_crystal_description Prismatic_plates _exptl_crystal_colour Orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method ? _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 3.074 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2891 _exptl_absorpt_correction_T_max 0.8012 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.74 _diffrn_reflns_number 6898 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 61.99 _reflns_number_total 6537 _reflns_number_observed 6227 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+1.9378P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6536 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_obs 0.0408 _refine_ls_wR_factor_all 0.2221 _refine_ls_wR_factor_obs 0.1100 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.028 _refine_ls_restrained_S_all 2.058 _refine_ls_restrained_S_obs 1.028 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.86557(2) 0.88210(2) 0.207465(13) 0.02900(12) Uani 1 d . . O O 0.8309(2) 0.8815(2) 0.09091(14) 0.0417(5) Uani 1 d . . N1 N 0.8965(2) 0.8755(2) 0.30897(15) 0.0316(5) Uani 1 d . . N2 N 0.9273(2) 0.8593(2) 0.3850(2) 0.0373(6) Uani 1 d . . C1 C 0.7004(3) 0.8458(3) 0.2447(2) 0.0372(7) Uani 1 d . . H1A H 0.6675(3) 0.8763(3) 0.3018(2) 0.045 Uiso 1 calc R . H1B H 0.6386(3) 0.8954(3) 0.2102(2) 0.045 Uiso 1 calc R . C2 C 1.0392(3) 0.7342(3) 0.1669(2) 0.0360(7) Uani 1 d . . H2A H 1.0625(3) 0.6837(3) 0.2155(2) 0.043 Uiso 1 calc R . H2B H 1.0221(3) 0.6844(3) 0.1282(2) 0.043 Uiso 1 calc R . C3 C 0.8509(3) 1.0639(3) 0.1834(2) 0.0367(7) Uani 1 d . . H3A H 0.9295(3) 1.0548(3) 0.1484(2) 0.044 Uiso 1 calc R . H3B H 0.7867(3) 1.0965(3) 0.1474(2) 0.044 Uiso 1 calc R . C4 C 0.7168(2) 0.9820(2) 0.45054(9) 0.0411(7) Uani 1 d G . H4A H 0.6944(2) 1.0103(2) 0.39840(9) 0.049 Uiso 1 calc R . C5 C 0.62921(14) 1.0215(2) 0.52152(12) 0.0484(8) Uani 1 d G . H5A H 0.5476(2) 1.0765(3) 0.5174(2) 0.058 Uiso 1 calc R . C6 C 0.6623(2) 0.9795(2) 0.59862(10) 0.0528(9) Uani 1 d G . H6A H 0.6031(2) 1.0062(3) 0.64662(12) 0.063 Uiso 1 calc R . C7 C 0.7830(2) 0.8981(2) 0.60472(9) 0.0485(8) Uani 1 d G . H7A H 0.8054(3) 0.8697(3) 0.65686(10) 0.058 Uiso 1 calc R . C8 C 0.87064(15) 0.8586(2) 0.53374(11) 0.0408(7) Uani 1 d G . H8A H 0.9523(2) 0.8035(2) 0.5379(2) 0.049 Uiso 1 calc R . C9 C 0.8375(2) 0.9005(2) 0.45665(9) 0.0344(6) Uani 1 d G . C10 C 1.1340(2) 0.82812(15) 0.41534(15) 0.0461(8) Uani 1 d G . H10A H 1.1043(2) 0.91051(15) 0.43190(15) 0.055 Uiso 1 calc R . C11 C 1.2583(2) 0.7526(2) 0.4160(2) 0.0604(10) Uani 1 d G . H11A H 1.3128(2) 0.7840(3) 0.4329(2) 0.073 Uiso 1 calc R . C12 C 1.30218(14) 0.6308(2) 0.3915(2) 0.0590(10) Uani 1 d G . H12A H 1.3863(2) 0.5797(3) 0.3919(2) 0.071 Uiso 1 calc R . C13 C 1.2217(2) 0.58446(14) 0.36636(15) 0.0504(9) Uani 1 d G . H13A H 1.2513(3) 0.5021(2) 0.3498(2) 0.060 Uiso 1 calc R . C14 C 1.0973(2) 0.6600(2) 0.36575(13) 0.0383(7) Uani 1 d G . H14A H 1.0428(2) 0.6286(2) 0.3488(2) 0.046 Uiso 1 calc R . C15 C 1.05345(14) 0.7818(2) 0.39023(13) 0.0352(6) Uani 1 d G . C16 C 0.8351(3) 0.8006(4) -0.0394(2) 0.0485(8) Uani 1 d . . F16 F 0.9352(2) 0.6990(2) -0.02769(14) 0.0664(6) Uani 1 d . . C17 C 0.7855(4) 0.8121(5) -0.1117(2) 0.0672(12) Uani 1 d . . F17 F 0.8399(3) 0.7225(3) -0.1695(2) 0.1029(11) Uani 1 d . . C18 C 0.6831(4) 0.9127(5) -0.1246(2) 0.0695(13) Uani 1 d . . F18 F 0.6366(3) 0.9248(4) -0.1958(2) 0.1119(13) Uani 1 d . . C19 C 0.6296(4) 1.0017(4) -0.0648(2) 0.0584(10) Uani 1 d . . F19 F 0.5295(2) 1.1026(3) -0.0768(2) 0.0831(8) Uani 1 d . . C20 C 0.6783(3) 0.9905(3) 0.0072(2) 0.0432(8) Uani 1 d . . F20 F 0.6218(2) 1.0788(2) 0.06568(14) 0.0567(5) Uani 1 d . . C21 C 0.7839(3) 0.8900(3) 0.0229(2) 0.0383(7) Uani 1 d . . C22 C 0.7067(3) 0.7137(3) 0.2418(2) 0.0399(7) Uani 1 d . . C23 C 0.5740(3) 0.7191(4) 0.2711(3) 0.0582(10) Uani 1 d . . H23A H 0.5463(3) 0.7507(4) 0.3275(3) 0.087 Uiso 1 calc R . H23B H 0.5744(3) 0.6376(4) 0.2689(3) 0.087 Uiso 1 calc R . H23C H 0.5179(3) 0.7722(4) 0.2352(3) 0.087 Uiso 1 calc R . C24 C 0.7455(4) 0.6633(3) 0.1529(2) 0.0504(9) Uani 1 d . . H24A H 0.8289(4) 0.6587(3) 0.1324(2) 0.076 Uiso 1 calc R . H24B H 0.6879(4) 0.7170(3) 0.1180(2) 0.076 Uiso 1 calc R . H24C H 0.7443(4) 0.5824(3) 0.1518(2) 0.076 Uiso 1 calc R . C25 C 0.7618(2) 0.6587(2) 0.38603(12) 0.0456(8) Uani 1 d G . H25A H 0.6940(2) 0.7309(2) 0.40496(12) 0.055 Uiso 1 calc R . C26 C 0.8305(2) 0.5802(2) 0.44224(9) 0.0521(9) Uani 1 d G . H26A H 0.8091(3) 0.5994(3) 0.49918(9) 0.062 Uiso 1 calc R . C27 C 0.9308(2) 0.4734(2) 0.41425(12) 0.0498(8) Uani 1 d G . H27A H 0.9773(3) 0.4204(2) 0.45226(15) 0.060 Uiso 1 calc R . C28 C 0.9625(2) 0.44513(15) 0.33004(13) 0.0466(8) Uani 1 d G . H28A H 1.0303(2) 0.3729(2) 0.3111(2) 0.056 Uiso 1 calc R . C29 C 0.8938(2) 0.5236(2) 0.27383(9) 0.0409(7) Uani 1 d G . H29A H 0.9152(3) 0.5045(2) 0.21689(10) 0.049 Uiso 1 calc R . C30 C 0.7935(2) 0.6304(2) 0.30183(11) 0.0368(7) Uani 1 d G . C31 C 1.1570(3) 0.7539(3) 0.1251(2) 0.0371(7) Uani 1 d . . C32 C 1.1912(3) 0.8316(3) 0.1808(2) 0.0455(8) Uani 1 d . . H32A H 1.2041(3) 0.7924(3) 0.2339(2) 0.068 Uiso 1 calc R . H32B H 1.1242(3) 0.9118(3) 0.1892(2) 0.068 Uiso 1 calc R . H32C H 1.2671(3) 0.8400(3) 0.1548(2) 0.068 Uiso 1 calc R . C33 C 1.1372(3) 0.8172(3) 0.0420(2) 0.0488(8) Uani 1 d . . H33A H 1.1153(3) 0.7687(3) 0.0060(2) 0.073 Uiso 1 calc R . H33B H 1.2132(3) 0.8256(3) 0.0164(2) 0.073 Uiso 1 calc R . H33C H 1.0703(3) 0.8974(3) 0.0508(2) 0.073 Uiso 1 calc R . C34 C 1.3614(2) 0.5857(2) 0.1554(2) 0.0637(11) Uani 1 d G . H34A H 1.3667(2) 0.6390(2) 0.1939(2) 0.076 Uiso 1 calc R . C35 C 1.4531(2) 0.4685(3) 0.1428(2) 0.089(2) Uani 1 d G . H35A H 1.5206(3) 0.4426(4) 0.1728(3) 0.107 Uiso 1 calc R . C36 C 1.4452(3) 0.3897(2) 0.0860(2) 0.092(2) Uani 1 d G . H36A H 1.5073(4) 0.3105(2) 0.0775(3) 0.110 Uiso 1 calc R . C37 C 1.3455(3) 0.4280(2) 0.0417(2) 0.088(2) Uani 1 d G . H37A H 1.3401(4) 0.3747(3) 0.0032(3) 0.105 Uiso 1 calc R . C38 C 1.2537(2) 0.5452(2) 0.0542(2) 0.0664(11) Uani 1 d G . H38A H 1.1863(3) 0.5711(3) 0.0243(2) 0.080 Uiso 1 calc R . C39 C 1.2617(2) 0.6240(2) 0.11111(15) 0.0419(7) Uani 1 d G . C40 C 0.8248(3) 1.1702(3) 0.2433(2) 0.0391(7) Uani 1 d . . C41 C 0.9295(4) 1.1365(3) 0.2965(3) 0.0548(9) Uani 1 d . . H41A H 0.9124(4) 1.2038(3) 0.3341(3) 0.082 Uiso 1 calc R . H41B H 1.0082(4) 1.1201(3) 0.2609(3) 0.082 Uiso 1 calc R . H41C H 0.9340(4) 1.0643(3) 0.3282(3) 0.082 Uiso 1 calc R . C42 C 0.8253(4) 1.2807(3) 0.1896(2) 0.0527(9) Uani 1 d . . H42A H 0.7597(4) 1.3034(3) 0.1554(2) 0.079 Uiso 1 calc R . H42B H 0.9052(4) 1.2587(3) 0.1543(2) 0.079 Uiso 1 calc R . H42C H 0.8114(4) 1.3491(3) 0.2252(2) 0.079 Uiso 1 calc R . C43 C 0.6701(3) 1.2785(2) 0.3679(2) 0.0726(13) Uani 1 d G . H43A H 0.7325(3) 1.2989(2) 0.3843(2) 0.087 Uiso 1 calc R . C44 C 0.5528(3) 1.3171(3) 0.41545(14) 0.094(2) Uani 1 d G . H44A H 0.5358(4) 1.3637(4) 0.4641(2) 0.113 Uiso 1 calc R . C45 C 0.4605(2) 1.2869(3) 0.3911(2) 0.091(2) Uani 1 d G . H45A H 0.3812(3) 1.3130(4) 0.4233(2) 0.110 Uiso 1 calc R . C46 C 0.4855(2) 1.2180(3) 0.3193(2) 0.0734(13) Uani 1 d G . H46A H 0.4231(2) 1.1976(4) 0.3028(3) 0.088 Uiso 1 calc R . C47 C 0.6028(2) 1.1794(2) 0.27168(14) 0.0505(8) Uani 1 d G . H47A H 0.6197(3) 1.1329(3) 0.2231(2) 0.061 Uiso 1 calc R . C48 C 0.6951(2) 1.2096(2) 0.29599(13) 0.0433(8) Uani 1 d G . 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 Mo 0.0303(2) 0.0280(2) 0.0288(2) 0.00079(9) -0.00552(10) -0.01100(11) O 0.0494(13) 0.0407(12) 0.0359(12) 0.0005(9) -0.0131(10) -0.0161(10) N1 0.0329(13) 0.0286(12) 0.0319(13) -0.0006(10) -0.0048(10) -0.0104(10) N2 0.0370(14) 0.0406(14) 0.0312(13) 0.0011(11) -0.0100(11) -0.0100(11) C1 0.033(2) 0.035(2) 0.044(2) 0.0034(13) -0.0096(13) -0.0126(13) C2 0.039(2) 0.0284(14) 0.038(2) -0.0004(12) -0.0041(13) -0.0101(13) C3 0.038(2) 0.034(2) 0.038(2) 0.0045(12) -0.0043(13) -0.0147(13) C4 0.044(2) 0.039(2) 0.036(2) -0.0002(13) -0.0062(13) -0.0114(14) C5 0.044(2) 0.042(2) 0.048(2) -0.0059(15) -0.0006(15) -0.0064(15) C6 0.056(2) 0.054(2) 0.041(2) -0.004(2) 0.006(2) -0.019(2) C7 0.059(2) 0.050(2) 0.033(2) 0.0033(14) -0.0048(15) -0.018(2) C8 0.046(2) 0.035(2) 0.038(2) 0.0011(13) -0.0069(14) -0.0118(14) C9 0.040(2) 0.0308(15) 0.0314(15) -0.0010(11) -0.0038(12) -0.0135(13) C10 0.050(2) 0.045(2) 0.050(2) 0.0029(15) -0.017(2) -0.022(2) C11 0.049(2) 0.077(3) 0.069(3) 0.014(2) -0.025(2) -0.034(2) C12 0.038(2) 0.067(3) 0.065(2) 0.014(2) -0.013(2) -0.013(2) C13 0.049(2) 0.041(2) 0.049(2) 0.0073(15) -0.006(2) -0.006(2) C14 0.042(2) 0.037(2) 0.038(2) 0.0069(13) -0.0069(13) -0.0181(14) C15 0.036(2) 0.037(2) 0.0324(15) 0.0046(12) -0.0065(12) -0.0136(13) C16 0.050(2) 0.064(2) 0.036(2) -0.006(2) -0.0002(15) -0.029(2) F16 0.0618(14) 0.0650(14) 0.0642(14) -0.0226(11) 0.0030(11) -0.0182(12) C17 0.074(3) 0.109(4) 0.035(2) -0.020(2) 0.007(2) -0.056(3) F17 0.104(2) 0.160(3) 0.055(2) -0.056(2) 0.0122(14) -0.065(2) C18 0.070(3) 0.127(4) 0.035(2) 0.014(2) -0.016(2) -0.062(3) F18 0.108(2) 0.219(4) 0.0400(13) 0.016(2) -0.0325(14) -0.091(3) C19 0.051(2) 0.087(3) 0.052(2) 0.030(2) -0.020(2) -0.041(2) F19 0.0629(15) 0.109(2) 0.087(2) 0.051(2) -0.0387(13) -0.0400(15) C20 0.046(2) 0.052(2) 0.040(2) 0.0099(15) -0.0105(14) -0.028(2) F20 0.0549(12) 0.0439(11) 0.0677(14) 0.0017(10) -0.0146(10) -0.0135(9) C21 0.046(2) 0.047(2) 0.031(2) 0.0053(13) -0.0089(13) -0.027(2) C22 0.041(2) 0.039(2) 0.046(2) 0.0052(13) -0.0098(14) -0.0209(14) C23 0.046(2) 0.061(2) 0.079(3) 0.012(2) -0.016(2) -0.031(2) C24 0.067(2) 0.048(2) 0.047(2) 0.003(2) -0.021(2) -0.030(2) C25 0.042(2) 0.045(2) 0.044(2) -0.0008(14) 0.0000(14) -0.0127(15) C26 0.056(2) 0.057(2) 0.041(2) 0.007(2) -0.003(2) -0.022(2) C27 0.059(2) 0.041(2) 0.052(2) 0.012(2) -0.014(2) -0.022(2) C28 0.052(2) 0.030(2) 0.060(2) -0.0018(14) -0.013(2) -0.0168(15) C29 0.048(2) 0.037(2) 0.043(2) -0.0043(13) -0.0039(14) -0.0221(15) C30 0.040(2) 0.037(2) 0.039(2) 0.0028(13) -0.0034(13) -0.0215(14) C31 0.033(2) 0.039(2) 0.035(2) -0.0014(13) 0.0014(12) -0.0119(13) C32 0.041(2) 0.040(2) 0.055(2) -0.0039(15) -0.0014(15) -0.0175(15) C33 0.049(2) 0.051(2) 0.042(2) 0.008(2) -0.0008(15) -0.019(2) C34 0.048(2) 0.058(2) 0.074(3) -0.006(2) -0.013(2) -0.007(2) C35 0.057(3) 0.073(3) 0.110(4) -0.002(3) -0.026(3) 0.009(2) C36 0.079(3) 0.055(3) 0.107(4) -0.015(3) 0.001(3) 0.007(2) C37 0.097(4) 0.059(3) 0.084(3) -0.030(2) -0.005(3) -0.006(3) C38 0.069(3) 0.054(2) 0.063(3) -0.018(2) -0.010(2) -0.009(2) C39 0.036(2) 0.041(2) 0.041(2) -0.0015(14) 0.0020(13) -0.0101(14) C40 0.047(2) 0.0274(15) 0.045(2) 0.0005(13) -0.0124(14) -0.0149(13) C41 0.060(2) 0.039(2) 0.073(3) -0.002(2) -0.028(2) -0.020(2) C42 0.065(2) 0.037(2) 0.060(2) 0.005(2) -0.010(2) -0.026(2) C43 0.083(3) 0.055(2) 0.056(2) -0.013(2) -0.021(2) 0.004(2) C44 0.097(4) 0.077(3) 0.048(2) -0.010(2) -0.004(2) 0.029(3) C45 0.065(3) 0.082(3) 0.068(3) 0.021(3) 0.015(2) 0.023(3) C46 0.047(2) 0.072(3) 0.082(3) 0.021(2) 0.000(2) -0.009(2) C47 0.044(2) 0.042(2) 0.058(2) 0.009(2) -0.005(2) -0.010(2) C48 0.053(2) 0.030(2) 0.037(2) 0.0026(12) -0.0075(14) -0.0057(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 Mo N1 1.746(2) . ? Mo O 2.011(2) . ? Mo C3 2.126(3) . ? Mo C2 2.144(3) . ? Mo C1 2.152(3) . ? O C21 1.300(4) . ? N1 N2 1.333(4) . ? N2 C9 1.412(3) . ? N2 C15 1.425(3) . ? C1 C22 1.547(4) . ? C2 C31 1.549(4) . ? C3 C40 1.539(4) . ? C4 C5 1.39 . ? C4 C9 1.39 . ? C5 C6 1.39 . ? C6 C7 1.39 . ? C7 C8 1.39 . ? C8 C9 1.39 . ? C10 C11 1.39 . ? C10 C15 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C16 F16 1.350(4) . ? C16 C17 1.377(5) . ? C16 C21 1.393(5) . ? C17 F17 1.345(5) . ? C17 C18 1.365(7) . ? C18 F18 1.341(4) . ? C18 C19 1.363(7) . ? C19 F19 1.347(5) . ? C19 C20 1.368(5) . ? C20 F20 1.345(4) . ? C20 C21 1.397(5) . ? C22 C24 1.531(5) . ? C22 C23 1.542(5) . ? C22 C30 1.555(3) . ? C25 C26 1.39 . ? C25 C30 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C28 C29 1.39 . ? C29 C30 1.39 . ? C31 C33 1.528(4) . ? C31 C32 1.529(5) . ? C31 C39 1.555(3) . ? C34 C35 1.39 . ? C34 C39 1.39 . ? C35 C36 1.39 . ? C36 C37 1.39 . ? C37 C38 1.39 . ? C38 C39 1.39 . ? C40 C41 1.536(5) . ? C40 C48 1.539(4) . ? C40 C42 1.549(4) . ? C43 C44 1.39 . ? C43 C48 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? 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 Mo O 177.31(9) . . ? N1 Mo C3 97.23(11) . . ? O Mo C3 85.45(11) . . ? N1 Mo C2 92.62(12) . . ? O Mo C2 85.94(11) . . ? C3 Mo C2 118.68(12) . . ? N1 Mo C1 92.68(12) . . ? O Mo C1 86.07(11) . . ? C3 Mo C1 120.11(12) . . ? C2 Mo C1 119.64(12) . . ? C21 O Mo 167.8(2) . . ? N2 N1 Mo 174.5(2) . . ? N1 N2 C9 122.2(2) . . ? N1 N2 C15 115.6(2) . . ? C9 N2 C15 121.5(2) . . ? C22 C1 Mo 120.2(2) . . ? C31 C2 Mo 122.9(2) . . ? C40 C3 Mo 130.5(2) . . ? C5 C4 C9 120.0 . . ? C4 C5 C6 120.0 . . ? C7 C6 C5 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 N2 119.4(2) . . ? C4 C9 N2 120.6(2) . . ? C11 C10 C15 120.0 . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 N2 119.1(2) . . ? C10 C15 N2 120.8(2) . . ? F16 C16 C17 119.3(3) . . ? F16 C16 C21 118.7(3) . . ? C17 C16 C21 122.0(4) . . ? F17 C17 C18 120.4(4) . . ? F17 C17 C16 118.9(5) . . ? C18 C17 C16 120.6(4) . . ? F18 C18 C19 120.4(5) . . ? F18 C18 C17 120.5(5) . . ? C19 C18 C17 119.2(4) . . ? F19 C19 C18 120.2(4) . . ? F19 C19 C20 119.5(4) . . ? C18 C19 C20 120.4(4) . . ? F20 C20 C19 118.9(3) . . ? F20 C20 C21 118.5(3) . . ? C19 C20 C21 122.6(4) . . ? O C21 C16 122.7(3) . . ? O C21 C20 122.1(3) . . ? C16 C21 C20 115.2(3) . . ? C24 C22 C23 107.2(3) . . ? C24 C22 C1 110.6(3) . . ? C23 C22 C1 107.3(3) . . ? C24 C22 C30 112.3(3) . . ? C23 C22 C30 108.1(3) . . ? C1 C22 C30 111.0(2) . . ? C26 C25 C30 120.0 . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 C22 121.3(2) . . ? C25 C30 C22 118.4(2) . . ? C33 C31 C32 108.6(3) . . ? C33 C31 C2 111.3(3) . . ? C32 C31 C2 110.6(2) . . ? C33 C31 C39 109.7(2) . . ? C32 C31 C39 111.0(2) . . ? C2 C31 C39 105.6(2) . . ? C35 C34 C39 120.0 . . ? C34 C35 C36 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 C31 119.1(2) . . ? C34 C39 C31 120.9(2) . . ? C41 C40 C3 109.9(3) . . ? C41 C40 C48 112.4(3) . . ? C3 C40 C48 112.1(2) . . ? C41 C40 C42 108.2(3) . . ? C3 C40 C42 107.0(3) . . ? C48 C40 C42 106.9(3) . . ? C44 C43 C48 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 C40 120.9(2) . . ? C43 C48 C40 119.1(2) . . ? _refine_diff_density_max 0.908 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.070 data_VG9759 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H43 N2 O F5 Si3 W' _chemical_formula_weight 810.78 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -5.4734 5.5774 '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 9.9973(12) _cell_length_b 10.6644(8) _cell_length_c 18.1009(13) _cell_angle_alpha 90.841(7) _cell_angle_beta 90.338(8) _cell_angle_gamma 110.944(8) _cell_volume 1802.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 10.72 _cell_measurement_theta_max 28.00 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method ? _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 7.334 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.0477 _exptl_absorpt_correction_T_max 0.1596 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5686 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 59.99 _reflns_number_total 5327 _reflns_number_observed 4795 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.4424P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00111(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5325 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_obs 0.0458 _refine_ls_wR_factor_all 0.1261 _refine_ls_wR_factor_obs 0.1173 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.098 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W W 0.20753(3) 0.19719(3) 0.24279(2) 0.0507(2) Uani 1 d . . Si1 Si 0.1904(3) -0.0567(2) 0.11403(13) 0.0820(7) Uani 1 d . . Si2 Si -0.0490(2) 0.3363(2) 0.20569(12) 0.0638(5) Uani 1 d . . Si3 Si 0.4450(2) 0.3399(2) 0.38166(11) 0.0628(5) Uani 1 d . . O O 0.3275(6) 0.3610(5) 0.1879(3) 0.0750(14) Uani 1 d . . N1 N 0.1070(6) 0.0593(6) 0.2942(3) 0.0567(13) Uani 1 d . . N2 N 0.0243(7) -0.0393(6) 0.3365(4) 0.070(2) Uani 1 d . . C1 C 0.1522(9) 0.0964(8) 0.1406(4) 0.068(2) Uani 1 d . . H1A H 0.0496(9) 0.0729(8) 0.1347(4) 0.082 Uiso 1 calc R . H1B H 0.1963(9) 0.1624(8) 0.1033(4) 0.082 Uiso 1 calc R . C2 C 0.0877(8) 0.3154(7) 0.2722(4) 0.065(2) Uani 1 d . . H2A H 0.0379(8) 0.2792(7) 0.3173(4) 0.078 Uiso 1 calc R . H2B H 0.1552(8) 0.4045(7) 0.2844(4) 0.078 Uiso 1 calc R . C3 C 0.4019(8) 0.2236(7) 0.2995(4) 0.064(2) Uani 1 d . . H3A H 0.3991(8) 0.1363(7) 0.3155(4) 0.077 Uiso 1 calc R . H3B H 0.4796(8) 0.2566(7) 0.2647(4) 0.077 Uiso 1 calc R . C4 C -0.2320(6) -0.1028(6) 0.3117(3) 0.088(2) Uani 1 d G . H4A H -0.2235(6) -0.1519(6) 0.2702(3) 0.105 Uiso 1 calc R . C5 C -0.3647(5) -0.0978(6) 0.3304(4) 0.100(3) Uani 1 d G . H5A H -0.4450(6) -0.1437(9) 0.3015(5) 0.120 Uiso 1 calc R . C6 C -0.3773(5) -0.0244(7) 0.3923(4) 0.098(3) Uani 1 d G . H6A H -0.4661(6) -0.0211(10) 0.4048(5) 0.117 Uiso 1 calc R . C7 C -0.2572(7) 0.0441(6) 0.4355(3) 0.093(3) Uani 1 d G . H7A H -0.2656(9) 0.0932(9) 0.4770(4) 0.112 Uiso 1 calc R . C8 C -0.1245(5) 0.0392(5) 0.4168(3) 0.079(2) Uani 1 d G . H8A H -0.0442(7) 0.0850(8) 0.4457(4) 0.094 Uiso 1 calc R . C9 C -0.1119(4) -0.0343(5) 0.3549(3) 0.062(2) Uani 1 d G . C10 C -0.0264(4) -0.2428(5) 0.4057(3) 0.070(2) Uani 1 d G . H10A H -0.1137(4) -0.2376(5) 0.4197(3) 0.084 Uiso 1 calc R . C11 C 0.0124(5) -0.3485(5) 0.4295(3) 0.082(2) Uani 1 d G . H11A H -0.0489(7) -0.4140(6) 0.4594(4) 0.099 Uiso 1 calc R . C12 C 0.1428(6) -0.3563(5) 0.4086(3) 0.079(2) Uani 1 d G . H12A H 0.1688(8) -0.4270(6) 0.4245(5) 0.095 Uiso 1 calc R . C13 C 0.2344(5) -0.2584(5) 0.3639(4) 0.084(3) Uani 1 d G . H13A H 0.3216(6) -0.2636(8) 0.3500(5) 0.101 Uiso 1 calc R . C14 C 0.1956(5) -0.1527(5) 0.3402(3) 0.073(2) Uani 1 d G . H14A H 0.2568(6) -0.0872(6) 0.3103(4) 0.088 Uiso 1 calc R . C15 C 0.0651(5) -0.1449(4) 0.3611(3) 0.0553(15) Uani 1 d G . C16 C 0.4337(8) 0.4362(8) 0.1502(4) 0.064(2) Uani 1 d . . C17 C 0.4709(9) 0.5745(8) 0.1504(5) 0.072(2) Uani 1 d . . F17 F 0.3969(6) 0.6303(5) 0.1924(3) 0.098(2) Uani 1 d . . C18 C 0.5822(11) 0.6569(9) 0.1103(6) 0.089(3) Uani 1 d . . F18 F 0.6156(8) 0.7897(6) 0.1140(5) 0.138(3) Uani 1 d . . C19 C 0.6620(9) 0.6028(11) 0.0657(5) 0.085(3) Uani 1 d . . F19 F 0.7662(7) 0.6855(8) 0.0245(4) 0.131(2) Uani 1 d . . C20 C 0.6277(9) 0.4687(11) 0.0639(5) 0.082(2) Uani 1 d . . F20 F 0.7026(7) 0.4142(8) 0.0207(4) 0.124(2) Uani 1 d . . C21 C 0.5159(9) 0.3869(9) 0.1053(5) 0.076(2) Uani 1 d . . F21 F 0.4868(7) 0.2546(6) 0.1012(4) 0.115(2) Uani 1 d . . C22 C 0.0442(14) -0.2035(10) 0.1516(7) 0.122(4) Uani 1 d . . H22A H 0.0607(14) -0.2844(10) 0.1388(7) 0.183 Uiso 1 calc R . H22B H -0.0460(14) -0.2075(10) 0.1310(7) 0.183 Uiso 1 calc R . H22C H 0.0423(14) -0.1945(10) 0.2044(7) 0.183 Uiso 1 calc R . C23 C 0.3684(13) -0.0526(12) 0.1486(7) 0.112(4) Uani 1 d . . H23A H 0.4427(13) 0.0236(12) 0.1287(7) 0.168 Uiso 1 calc R . H23B H 0.3826(13) -0.1334(12) 0.1332(7) 0.168 Uiso 1 calc R . H23C H 0.3713(13) -0.0460(12) 0.2016(7) 0.168 Uiso 1 calc R . C24 C 0.1894(18) -0.0689(14) 0.0111(6) 0.141(5) Uani 1 d . . H24A H 0.2651(18) 0.0072(14) -0.0079(6) 0.211 Uiso 1 calc R . H24B H 0.0991(18) -0.0702(14) -0.0079(6) 0.211 Uiso 1 calc R . H24C H 0.2037(18) -0.1499(14) -0.0039(6) 0.211 Uiso 1 calc R . C25 C -0.2013(10) 0.1752(11) 0.1901(6) 0.093(3) Uani 1 d . . H25A H -0.2433(10) 0.1413(11) 0.2366(6) 0.140 Uiso 1 calc R . H25B H -0.1672(10) 0.1111(11) 0.1668(6) 0.140 Uiso 1 calc R . H25C H -0.2719(10) 0.1901(11) 0.1588(6) 0.140 Uiso 1 calc R . C26 C 0.0361(11) 0.4061(10) 0.1173(5) 0.088(3) Uani 1 d . . H26A H 0.1142(11) 0.4890(10) 0.1269(5) 0.132 Uiso 1 calc R . H26B H -0.0332(11) 0.4222(10) 0.0857(5) 0.132 Uiso 1 calc R . H26C H 0.0715(11) 0.3433(10) 0.0936(5) 0.132 Uiso 1 calc R . C27 C -0.1224(11) 0.4583(11) 0.2495(6) 0.095(3) Uani 1 d . . H27A H -0.1668(11) 0.4232(11) 0.2953(6) 0.142 Uiso 1 calc R . H27B H -0.1921(11) 0.4716(11) 0.2169(6) 0.142 Uiso 1 calc R . H27C H -0.0458(11) 0.5425(11) 0.2586(6) 0.142 Uiso 1 calc R . C28 C 0.2918(10) 0.2971(11) 0.4459(5) 0.092(3) Uani 1 d . . H28A H 0.2663(10) 0.2055(11) 0.4607(5) 0.138 Uiso 1 calc R . H28B H 0.2114(10) 0.3084(11) 0.4216(5) 0.138 Uiso 1 calc R . H28C H 0.3184(10) 0.3553(11) 0.4888(5) 0.138 Uiso 1 calc R . C29 C 0.4918(11) 0.5163(9) 0.3541(6) 0.090(3) Uani 1 d . . H29A H 0.4128(11) 0.5259(9) 0.3274(6) 0.135 Uiso 1 calc R . H29B H 0.5745(11) 0.5414(9) 0.3231(6) 0.135 Uiso 1 calc R . H29C H 0.5123(11) 0.5734(9) 0.3974(6) 0.135 Uiso 1 calc R . C30 C 0.5986(11) 0.3236(11) 0.4330(6) 0.098(3) Uani 1 d . . H30A H 0.5753(11) 0.2321(11) 0.4476(6) 0.146 Uiso 1 calc R . H30B H 0.6189(11) 0.3810(11) 0.4762(6) 0.146 Uiso 1 calc R . H30C H 0.6811(11) 0.3491(11) 0.4019(6) 0.146 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 W 0.0553(2) 0.0458(2) 0.0528(2) 0.00473(12) 0.00296(12) 0.02008(14) Si1 0.119(2) 0.0630(13) 0.0692(13) -0.0062(10) -0.0018(13) 0.0398(13) Si2 0.0656(12) 0.0672(12) 0.0660(11) 0.0079(9) 0.0037(9) 0.0324(10) Si3 0.0650(12) 0.0607(11) 0.0628(11) -0.0006(9) -0.0044(9) 0.0228(9) O 0.068(3) 0.061(3) 0.093(4) 0.024(3) 0.023(3) 0.018(3) N1 0.058(3) 0.053(3) 0.061(3) 0.006(3) -0.001(3) 0.023(3) N2 0.060(4) 0.064(4) 0.091(5) 0.030(3) 0.022(3) 0.028(3) C1 0.085(5) 0.065(4) 0.058(4) 0.005(3) -0.001(4) 0.032(4) C2 0.069(4) 0.059(4) 0.072(4) 0.002(3) -0.006(4) 0.029(4) C3 0.063(4) 0.061(4) 0.069(4) -0.003(3) 0.005(3) 0.025(3) C4 0.082(6) 0.084(6) 0.090(6) -0.005(5) 0.001(5) 0.022(5) C5 0.067(6) 0.107(8) 0.124(9) 0.013(7) -0.001(5) 0.028(5) C6 0.067(6) 0.094(7) 0.140(9) 0.022(6) 0.025(6) 0.038(5) C7 0.095(7) 0.092(7) 0.104(7) 0.004(5) 0.012(6) 0.046(6) C8 0.076(5) 0.077(5) 0.093(6) 0.002(4) -0.001(4) 0.040(4) C9 0.057(4) 0.052(4) 0.078(5) 0.020(3) 0.007(3) 0.016(3) C10 0.076(5) 0.069(5) 0.074(5) 0.019(4) 0.015(4) 0.036(4) C11 0.094(6) 0.081(5) 0.076(5) 0.026(4) 0.011(4) 0.036(5) C12 0.090(6) 0.067(5) 0.088(6) 0.019(4) -0.009(5) 0.035(4) C13 0.066(5) 0.078(5) 0.119(7) 0.019(5) 0.002(5) 0.037(4) C14 0.070(5) 0.066(5) 0.087(5) 0.022(4) 0.012(4) 0.027(4) C15 0.065(4) 0.051(4) 0.052(3) 0.007(3) 0.001(3) 0.024(3) C16 0.064(4) 0.067(4) 0.063(4) 0.010(3) 0.002(3) 0.024(4) C17 0.073(5) 0.064(5) 0.080(5) 0.016(4) 0.003(4) 0.025(4) F17 0.116(4) 0.071(3) 0.114(4) 0.014(3) 0.023(3) 0.041(3) C18 0.087(6) 0.070(5) 0.094(6) 0.031(5) 0.002(5) 0.009(5) F18 0.142(6) 0.070(4) 0.187(8) 0.040(4) 0.035(5) 0.018(4) C19 0.062(5) 0.101(7) 0.082(6) 0.031(5) 0.007(4) 0.014(5) F19 0.094(4) 0.156(6) 0.117(5) 0.054(5) 0.031(4) 0.011(4) C20 0.066(5) 0.121(8) 0.069(5) 0.015(5) 0.010(4) 0.045(5) F20 0.103(4) 0.173(6) 0.108(4) -0.002(4) 0.031(4) 0.065(4) C21 0.076(5) 0.075(5) 0.079(5) 0.001(4) -0.004(4) 0.031(4) F21 0.125(5) 0.084(4) 0.144(5) 0.003(4) 0.035(4) 0.047(3) C22 0.151(11) 0.069(6) 0.123(10) -0.006(6) -0.024(8) 0.013(6) C23 0.123(9) 0.110(8) 0.133(9) 0.015(7) 0.013(7) 0.078(7) C24 0.234(17) 0.130(10) 0.081(7) -0.029(7) -0.009(9) 0.094(11) C25 0.078(6) 0.110(7) 0.083(6) 0.011(5) -0.009(5) 0.023(5) C26 0.104(7) 0.094(6) 0.076(5) 0.013(5) 0.008(5) 0.046(6) C27 0.104(7) 0.112(8) 0.090(6) 0.000(6) -0.006(5) 0.064(6) C28 0.078(6) 0.118(8) 0.077(5) -0.003(5) 0.006(4) 0.033(5) C29 0.102(7) 0.064(5) 0.099(7) 0.000(5) -0.006(5) 0.023(5) C30 0.093(7) 0.111(8) 0.093(7) -0.004(6) -0.020(5) 0.043(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W N1 1.741(6) . ? W O 2.011(5) . ? W C2 2.091(7) . ? W C1 2.095(8) . ? W C3 2.117(7) . ? Si1 C22 1.860(12) . ? Si1 C1 1.861(8) . ? Si1 C24 1.866(11) . ? Si1 C23 1.868(11) . ? Si2 C26 1.854(9) . ? Si2 C25 1.859(10) . ? Si2 C27 1.876(9) . ? Si2 C2 1.891(7) . ? Si3 C29 1.846(9) . ? Si3 C30 1.852(9) . ? Si3 C28 1.856(9) . ? Si3 C3 1.869(7) . ? O C16 1.285(9) . ? N1 N2 1.337(8) . ? N2 C15 1.405(7) . ? N2 C9 1.423(7) . ? C4 C5 1.39 . ? C4 C9 1.39 . ? C5 C6 1.39 . ? C6 C7 1.39 . ? C7 C8 1.39 . ? C8 C9 1.39 . ? C10 C11 1.39 . ? C10 C15 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C16 C21 1.385(11) . ? C16 C17 1.387(11) . ? C17 F17 1.337(10) . ? C17 C18 1.365(12) . ? C18 F18 1.334(11) . ? C18 C19 1.396(14) . ? C19 F19 1.338(10) . ? C19 C20 1.346(14) . ? C20 F20 1.347(10) . ? C20 C21 1.379(12) . ? C21 F21 1.335(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 W O 177.3(3) . . ? N1 W C2 95.2(3) . . ? O W C2 84.0(3) . . ? N1 W C1 94.6(3) . . ? O W C1 88.0(3) . . ? C2 W C1 115.1(3) . . ? N1 W C3 94.3(3) . . ? O W C3 83.9(3) . . ? C2 W C3 119.8(3) . . ? C1 W C3 123.2(3) . . ? C22 Si1 C1 107.4(5) . . ? C22 Si1 C24 109.9(6) . . ? C1 Si1 C24 108.0(5) . . ? C22 Si1 C23 110.4(6) . . ? C1 Si1 C23 113.0(5) . . ? C24 Si1 C23 108.1(6) . . ? C26 Si2 C25 111.2(5) . . ? C26 Si2 C27 108.6(4) . . ? C25 Si2 C27 107.6(5) . . ? C26 Si2 C2 110.6(4) . . ? C25 Si2 C2 111.3(4) . . ? C27 Si2 C2 107.3(4) . . ? C29 Si3 C30 108.8(5) . . ? C29 Si3 C28 108.6(5) . . ? C30 Si3 C28 107.4(5) . . ? C29 Si3 C3 111.4(4) . . ? C30 Si3 C3 109.3(4) . . ? C28 Si3 C3 111.2(4) . . ? C16 O W 157.3(5) . . ? N2 N1 W 174.8(5) . . ? N1 N2 C15 123.2(5) . . ? N1 N2 C9 116.2(5) . . ? C15 N2 C9 120.6(5) . . ? Si1 C1 W 124.5(4) . . ? Si2 C2 W 120.5(4) . . ? Si3 C3 W 116.5(3) . . ? C5 C4 C9 120.0 . . ? C4 C5 C6 120.0 . . ? C7 C6 C5 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 N2 119.5(5) . . ? C4 C9 N2 120.5(5) . . ? C11 C10 C15 120.0 . . ? C12 C11 C10 120.0 . . ? C13 C12 C11 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 N2 120.3(4) . . ? C10 C15 N2 119.7(4) . . ? O C16 C21 123.5(8) . . ? O C16 C17 121.3(7) . . ? C21 C16 C17 115.2(7) . . ? F17 C17 C18 118.4(8) . . ? F17 C17 C16 119.0(7) . . ? C18 C17 C16 122.6(9) . . ? F18 C18 C17 120.1(10) . . ? F18 C18 C19 119.7(9) . . ? C17 C18 C19 120.2(9) . . ? F19 C19 C20 122.7(10) . . ? F19 C19 C18 118.8(10) . . ? C20 C19 C18 118.5(8) . . ? C19 C20 F20 119.4(9) . . ? C19 C20 C21 120.6(8) . . ? F20 C20 C21 119.9(10) . . ? F21 C21 C20 117.9(8) . . ? F21 C21 C16 119.2(8) . . ? C20 C21 C16 122.9(8) . . ? _refine_diff_density_max 1.704 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.105 data_VG9760 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H18 N2 O3 F10 Cl2 W' _chemical_formula_weight 875.19 _chemical_melting_point ? _chemical_compound_source ? 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 C2/c 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' '-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 10.908(2) _cell_length_b 13.007(2) _cell_length_c 21.660(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.29(2) _cell_angle_gamma 90.00 _cell_volume 3041.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.38 _cell_measurement_theta_max 12.54 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method ? _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 4.070 _exptl_absorpt_correction_type Lamina _exptl_absorpt_correction_T_min 0.3887 _exptl_absorpt_correction_T_max 0.8154 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.13 _diffrn_reflns_number 2551 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2412 _reflns_number_observed 2050 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2412 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all 0.0858 _refine_ls_wR_factor_obs 0.0803 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.040 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.040 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W W 0.5000 0.42919(3) -0.2500 0.03973(13) Uani 1 d S . Cl Cl 0.2883(2) 0.44369(14) -0.23951(11) 0.0619(5) Uani 1 d . . N1 N 0.5000 0.2956(5) -0.2500 0.039(2) Uani 1 d S . N2 N 0.5000 0.1943(5) -0.2500 0.049(2) Uani 1 d S . O1 O 0.4605(5) 0.4528(3) -0.3388(3) 0.0538(12) Uani 1 d . . O2 O 0.5000 0.5995(5) -0.2500 0.054(2) Uani 1 d S . C1 C 0.4765(5) 0.0588(4) -0.3277(3) 0.062(2) Uani 1 d G . H1A H 0.4071(5) 0.0350(4) -0.3117(3) 0.075 Uiso 1 calc R . C2 C 0.5156(6) 0.0093(3) -0.3783(3) 0.072(3) Uani 1 d G . H2A H 0.4724(8) -0.0475(5) -0.3961(4) 0.087 Uiso 1 calc R . C3 C 0.6193(6) 0.0448(4) -0.4023(3) 0.078(3) Uani 1 d G . H3A H 0.6455(9) 0.0118(6) -0.4362(3) 0.094 Uiso 1 calc R . C4 C 0.6838(5) 0.1298(4) -0.3757(3) 0.075(3) Uani 1 d G . H4A H 0.7532(7) 0.1536(6) -0.3918(4) 0.090 Uiso 1 calc R . C5 C 0.6447(5) 0.1792(3) -0.3251(3) 0.058(2) Uani 1 d G . H5A H 0.6879(6) 0.2361(5) -0.3073(4) 0.070 Uiso 1 calc R . C6 C 0.5410(5) 0.1437(3) -0.3011(2) 0.046(2) Uani 1 d G . C7 C 0.4685(9) 0.3943(5) -0.3880(4) 0.057(2) Uani 1 d . . C8 C 0.3923(11) 0.3092(6) -0.4032(5) 0.075(3) Uani 1 d . . F8 F 0.3079(6) 0.2839(4) -0.3672(4) 0.097(2) Uani 1 d . . C9 C 0.4016(16) 0.2502(8) -0.4558(6) 0.108(5) Uani 1 d . . F9 F 0.3296(10) 0.1684(5) -0.4694(4) 0.150(4) Uani 1 d . . C10 C 0.4860(20) 0.2722(10) -0.4942(6) 0.129(7) Uani 1 d . . F10 F 0.4971(14) 0.2171(7) -0.5444(4) 0.199(6) Uani 1 d . . C11 C 0.5598(17) 0.3562(11) -0.4800(6) 0.120(6) Uani 1 d . . F11 F 0.6437(13) 0.3845(9) -0.5178(4) 0.193(5) Uani 1 d . . C12 C 0.5532(12) 0.4171(8) -0.4287(5) 0.086(3) Uani 1 d . . F12 F 0.6249(8) 0.4999(5) -0.4165(4) 0.111(2) Uani 1 d . . C13 C 0.5509(10) 0.6628(6) -0.2950(5) 0.073(3) Uani 1 d . . H13A H 0.5208(10) 0.6406(6) -0.3372(5) 0.088 Uiso 1 calc R . H13B H 0.6407(10) 0.6597(6) -0.2885(5) 0.088 Uiso 1 calc R . C14 C 0.5066(10) 0.7703(6) -0.2838(5) 0.079(3) Uani 1 d . . H14A H 0.5667(10) 0.8212(6) -0.2927(5) 0.095 Uiso 1 calc R . H14B H 0.4279(10) 0.7843(6) -0.3094(5) 0.095 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 W 0.0484(2) 0.0305(2) 0.0435(2) 0.000 0.0174(2) 0.000 Cl 0.0530(10) 0.0522(10) 0.0848(14) 0.0016(9) 0.0248(10) 0.0059(8) N1 0.044(4) 0.035(3) 0.041(4) 0.000 0.016(4) 0.000 N2 0.064(5) 0.032(4) 0.056(5) 0.000 0.029(5) 0.000 O1 0.071(3) 0.045(3) 0.047(3) 0.001(2) 0.014(3) -0.007(2) O2 0.077(5) 0.032(3) 0.056(4) 0.000 0.016(4) 0.000 C1 0.088(6) 0.043(4) 0.060(5) 0.001(4) 0.028(4) -0.009(4) C2 0.108(8) 0.045(4) 0.066(6) -0.012(4) 0.020(6) -0.002(4) C3 0.109(8) 0.073(6) 0.061(5) -0.006(4) 0.041(6) 0.017(5) C4 0.076(6) 0.079(6) 0.079(6) -0.006(5) 0.043(6) 0.013(5) C5 0.060(5) 0.052(4) 0.067(5) 0.002(4) 0.028(4) -0.004(4) C6 0.060(4) 0.039(3) 0.041(4) 0.002(3) 0.014(3) 0.009(3) C7 0.081(6) 0.047(3) 0.043(4) -0.001(3) 0.009(4) 0.008(4) C8 0.106(8) 0.050(4) 0.059(5) -0.001(4) -0.022(5) 0.006(5) F8 0.085(4) 0.071(3) 0.128(6) 0.001(4) -0.008(4) -0.019(3) C9 0.169(14) 0.064(6) 0.074(8) -0.022(6) -0.035(9) 0.025(7) F9 0.203(9) 0.075(4) 0.141(7) -0.046(4) -0.079(7) 0.021(5) C10 0.235(20) 0.084(8) 0.057(6) -0.025(6) -0.015(10) 0.052(10) F10 0.370(17) 0.150(7) 0.074(5) -0.056(5) 0.019(8) 0.079(9) C11 0.196(16) 0.116(10) 0.062(7) 0.012(7) 0.064(9) 0.049(11) F11 0.302(15) 0.196(9) 0.111(7) 0.003(7) 0.132(9) 0.041(10) C12 0.123(9) 0.076(6) 0.065(6) 0.008(5) 0.035(6) 0.005(6) F12 0.150(6) 0.100(4) 0.097(5) 0.008(4) 0.071(5) -0.026(4) C13 0.099(7) 0.043(4) 0.082(7) 0.012(4) 0.030(6) -0.015(4) C14 0.077(6) 0.039(4) 0.116(9) 0.019(4) -0.004(7) -0.007(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 W N1 1.738(7) . ? W O1 1.934(5) 2_654 ? W O1 1.934(5) . ? W O2 2.215(6) . ? W Cl 2.360(2) . ? W Cl 2.360(2) 2_654 ? N1 N2 1.317(10) . ? N2 C6 1.415(6) 2_654 ? N2 C6 1.415(5) . ? O1 C7 1.323(9) . ? O2 C13 1.447(8) 2_654 ? O2 C13 1.447(8) . ? C1 C2 1.39 . ? C1 C6 1.39 . ? C2 C3 1.39 . ? C3 C4 1.39 . ? C4 C5 1.39 . ? C5 C6 1.39 . ? C7 C8 1.395(12) . ? C7 C12 1.396(13) . ? C8 F8 1.331(13) . ? C8 C9 1.389(15) . ? C9 F9 1.330(15) . ? C9 C10 1.36(2) . ? C10 F10 1.322(13) . ? C10 C11 1.36(2) . ? C11 F11 1.36(2) . ? C11 C12 1.38(2) . ? C12 F12 1.336(13) . ? C13 C14 1.510(11) . ? C14 C14 1.49(2) 2_654 ? 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 W O1 99.12(13) . 2_654 ? N1 W O1 99.12(13) . . ? O1 W O1 161.8(3) 2_654 . ? N1 W O2 180.0 . . ? O1 W O2 80.88(13) 2_654 . ? O1 W O2 80.88(13) . . ? N1 W Cl 94.58(4) . . ? O1 W Cl 88.4(2) 2_654 . ? O1 W Cl 90.1(2) . . ? O2 W Cl 85.42(4) . . ? N1 W Cl 94.58(4) . 2_654 ? O1 W Cl 90.1(2) 2_654 2_654 ? O1 W Cl 88.4(2) . 2_654 ? O2 W Cl 85.42(4) . 2_654 ? Cl W Cl 170.84(9) . 2_654 ? N2 N1 W 180.0 . . ? N1 N2 C6 117.7(5) . 2_654 ? N1 N2 C6 117.7(3) . . ? C6 N2 C6 124.6(8) 2_654 . ? C7 O1 W 132.8(5) . . ? C13 O2 C13 110.6(8) 2_654 . ? C13 O2 W 124.7(4) 2_654 . ? C13 O2 W 124.7(4) . . ? C2 C1 C6 120.0 . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 N2 120.3(4) . . ? C1 C6 N2 119.7(4) . . ? O1 C7 C8 122.7(8) . . ? O1 C7 C12 120.8(8) . . ? C8 C7 C12 116.4(9) . . ? F8 C8 C9 118.9(11) . . ? F8 C8 C7 119.8(8) . . ? C9 C8 C7 121.4(12) . . ? F9 C9 C10 117.7(12) . . ? F9 C9 C8 120.8(16) . . ? C10 C9 C8 121.5(13) . . ? F10 C10 C9 122.7(17) . . ? F10 C10 C11 119.9(18) . . ? C9 C10 C11 117.5(11) . . ? F11 C11 C10 120.4(14) . . ? F11 C11 C12 116.6(15) . . ? C10 C11 C12 123.0(14) . . ? F12 C12 C11 121.8(11) . . ? F12 C12 C7 117.9(9) . . ? C11 C12 C7 120.3(12) . . ? O2 C13 C14 104.8(7) . . ? C14 C14 C13 103.7(6) 2_654 . ? _refine_diff_density_max 0.567 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.105