# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1420 data_compound3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16.25 H25.50 Cl1.50 Mo O2 P2' _chemical_formula_weight 463.92 _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' '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' 'P' 'P' 0.1023 0.0942 '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 (no.2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.067(2) _cell_length_b 13.036(4) _cell_length_c 17.169(4) _cell_angle_alpha 67.90(2) _cell_angle_beta 87.66(2) _cell_angle_gamma 72.600(10) _cell_volume 1985.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method ? _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7673 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6974 _reflns_number_observed 5817 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 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^)+(0.0396P)^2^+1.2475P] 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 6971 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_all 0.0771 _refine_ls_wR_factor_obs 0.0741 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.109 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.109 _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 Mo1 Mo 0.13942(3) 0.14485(2) 0.12557(2) 0.03540(8) Uani 1 d . . P1 P 0.28189(8) -0.07230(6) 0.25862(5) 0.0388(2) Uani 1 d . . H1 H 0.2757(27) -0.1389(23) 0.2214(16) 0.029(7) Uiso 1 d . . P2 P 0.23379(9) 0.13108(7) 0.25767(5) 0.0402(2) Uani 1 d . . Cl1 Cl 0.24752(10) 0.30734(7) 0.05440(6) 0.0570(2) Uani 1 d . . O1 O -0.0924(3) 0.3543(3) 0.1373(2) 0.0886(10) Uani 1 d . . H1A H 0.4012(50) -0.2354(42) 0.3463(30) 0.100(17) Uiso 1 d . . O2 O 0.3581(3) -0.1662(2) 0.3463(2) 0.0609(7) Uani 1 d . . C1 C -0.0115(4) 0.2810(3) 0.1378(2) 0.0535(8) Uani 1 d . . C2 C 0.1833(4) 0.0226(3) 0.0471(2) 0.0554(9) Uani 1 d . . H2 H 0.2662(4) -0.0368(3) 0.0536(2) 0.066 Uiso 1 calc R . C3 C 0.0657(4) 0.0114(3) 0.0912(2) 0.0568(9) Uani 1 d . . H3A H 0.0573(4) -0.0568(3) 0.1325(2) 0.068 Uiso 1 calc R . C4 C -0.0389(4) 0.1211(3) 0.0628(2) 0.0573(9) Uani 1 d . . H4A H -0.1277(4) 0.1380(3) 0.0816(2) 0.069 Uiso 1 calc R . C5 C 0.0177(4) 0.2001(3) 0.0003(2) 0.0571(9) Uani 1 d . . H5 H -0.0274(4) 0.2787(3) -0.0297(2) 0.069 Uiso 1 calc R . C6 C 0.1554(4) 0.1378(3) -0.0082(2) 0.0577(9) Uani 1 d . . H6 H 0.2169(4) 0.1687(3) -0.0447(2) 0.069 Uiso 1 calc R . C7 C 0.3489(3) 0.0420(2) 0.2056(2) 0.0377(6) Uani 1 d . . C8 C 0.5012(3) 0.0336(3) 0.1847(2) 0.0502(8) Uani 1 d . . C9 C 0.5981(4) -0.0839(4) 0.2443(3) 0.0770(12) Uani 1 d . . H9A H 0.5724(22) -0.1457(4) 0.2379(15) 0.115 Uiso 1 calc R . H9B H 0.5896(25) -0.0894(12) 0.3015(3) 0.115 Uiso 1 calc R . H9C H 0.6929(5) -0.0902(12) 0.2307(14) 0.115 Uiso 1 calc R . C10 C 0.5417(4) 0.1317(4) 0.1961(3) 0.0710(11) Uani 1 d . . H10A H 0.4797(21) 0.2054(4) 0.1600(14) 0.106 Uiso 1 calc R . H10B H 0.6359(12) 0.1267(17) 0.1816(19) 0.106 Uiso 1 calc R . H10C H 0.5348(31) 0.1243(16) 0.2538(5) 0.106 Uiso 1 calc R . C11 C 0.5209(4) 0.0413(4) 0.0943(3) 0.0758(12) Uani 1 d . . H11A H 0.4973(32) -0.0210(17) 0.0873(6) 0.114 Uiso 1 calc R . H11B H 0.6165(9) 0.0352(28) 0.0829(7) 0.114 Uiso 1 calc R . H11C H 0.4612(25) 0.1144(12) 0.0560(3) 0.114 Uiso 1 calc R . C12 C 0.1306(3) 0.0331(3) 0.2633(2) 0.0412(7) Uani 1 d . . C13 C 0.0131(4) 0.0124(3) 0.3202(2) 0.0586(9) Uani 1 d . . C14 C 0.0720(6) -0.0482(5) 0.4123(3) 0.096(2) Uani 1 d . . H14A H -0.0010(11) -0.0660(31) 0.4476(3) 0.145 Uiso 1 calc R . H14B H 0.1089(37) 0.0021(14) 0.4276(7) 0.145 Uiso 1 calc R . H14C H 0.1451(28) -0.1189(18) 0.4195(6) 0.145 Uiso 1 calc R . C15 C -0.0505(5) -0.0692(4) 0.3004(3) 0.0810(13) Uani 1 d . . H15A H -0.1213(25) -0.0855(24) 0.3382(14) 0.121 Uiso 1 calc R . H15B H 0.0213(8) -0.1405(12) 0.3075(20) 0.121 Uiso 1 calc R . H15C H -0.0913(31) -0.0326(12) 0.2433(8) 0.121 Uiso 1 calc R . C16 C -0.1016(5) 0.1249(4) 0.3071(4) 0.109(2) Uani 1 d . . H16A H -0.1746(22) 0.1086(6) 0.3429(21) 0.163 Uiso 1 calc R . H16B H -0.1388(31) 0.1613(20) 0.2492(8) 0.163 Uiso 1 calc R . H16C H -0.0640(12) 0.1761(15) 0.3209(26) 0.163 Uiso 1 calc R . Mo2 Mo -0.33307(3) 0.50815(2) -0.34208(2) 0.04442(9) Uani 1 d . . P3 P -0.21401(9) 0.52272(7) -0.19925(5) 0.0417(2) Uani 1 d . . H3 H -0.2709(31) 0.6357(26) -0.2241(19) 0.046(8) Uiso 1 d . . P4 P -0.18724(8) 0.33972(6) -0.22763(5) 0.0376(2) Uani 1 d . . Cl3 Cl -0.50538(10) 0.39750(8) -0.33328(6) 0.0621(2) Uani 1 d . . O3 O -0.1906(4) 0.3694(3) -0.4500(2) 0.0824(9) Uani 1 d . . O4 O -0.1252(3) 0.4918(2) -0.11490(15) 0.0535(6) Uani 1 d . . H4 H -0.1495(41) 0.5425(34) -0.0988(25) 0.064(13) Uiso 1 d . . C17 C -0.2351(4) 0.4135(3) -0.4100(2) 0.0561(9) Uani 1 d . . C18 C -0.3400(6) 0.7018(3) -0.3892(2) 0.0748(13) Uani 1 d . . H18 H -0.2749(6) 0.7231(3) -0.3667(2) 0.090 Uiso 1 calc R . C19 C -0.4724(6) 0.7008(3) -0.3610(3) 0.0800(14) Uani 1 d . . H19 H -0.5112(6) 0.7228(3) -0.3174(3) 0.096 Uiso 1 calc R . C20 C -0.5359(6) 0.6610(3) -0.4096(3) 0.088(2) Uani 1 d . . H20 H -0.6240(6) 0.6511(3) -0.4039(3) 0.106 Uiso 1 calc R . C21 C -0.4431(7) 0.6385(4) -0.4689(3) 0.093(2) Uani 1 d . . H21 H -0.4590(7) 0.6106(4) -0.5091(3) 0.112 Uiso 1 calc R . C22 C -0.3223(6) 0.6654(3) -0.4570(3) 0.0848(15) Uani 1 d . . H22 H -0.2448(6) 0.6600(3) -0.4884(3) 0.102 Uiso 1 calc R . C23 C -0.3252(3) 0.4419(2) -0.1963(2) 0.0389(7) Uani 1 d . . C24 C -0.4351(3) 0.4151(3) -0.1331(2) 0.0486(8) Uani 1 d . . C25 C -0.3817(4) 0.4049(4) -0.0469(2) 0.0709(11) Uani 1 d . . H25A H -0.2925(15) 0.3461(18) -0.0292(9) 0.106 Uiso 1 calc R . H25B H -0.4469(16) 0.3841(25) -0.0061(5) 0.106 Uiso 1 calc R . H25C H -0.3725(29) 0.4782(8) -0.0516(5) 0.106 Uiso 1 calc R . C26 C -0.4559(5) 0.2986(3) -0.1205(3) 0.0725(12) Uani 1 d . . H26A H -0.3712(11) 0.2368(4) -0.0949(18) 0.109 Uiso 1 calc R . H26B H -0.4794(32) 0.2986(10) -0.1741(4) 0.109 Uiso 1 calc R . H26C H -0.5301(22) 0.2871(13) -0.0845(16) 0.109 Uiso 1 calc R . C27 C -0.5740(4) 0.5111(4) -0.1620(3) 0.0762(12) Uani 1 d . . H27A H -0.6401(10) 0.4932(14) -0.1212(10) 0.114 Uiso 1 calc R . H27B H -0.6082(17) 0.5172(19) -0.2155(10) 0.114 Uiso 1 calc R . H27C H -0.5613(8) 0.5837(6) -0.1677(19) 0.114 Uiso 1 calc R . C28 C -0.1256(3) 0.4685(3) -0.2719(2) 0.0422(7) Uani 1 d . . C29 C 0.0226(4) 0.4672(3) -0.2973(2) 0.0589(9) Uani 1 d . . C30 C 0.1272(4) 0.3947(4) -0.2198(3) 0.0806(13) Uani 1 d . . H30A H 0.2200(5) 0.3932(24) -0.2360(5) 0.121 Uiso 1 calc R . H30B H 0.1217(24) 0.3168(9) -0.1967(12) 0.121 Uiso 1 calc R . H30C H 0.1056(21) 0.4287(17) -0.1782(9) 0.121 Uiso 1 calc R . C31 C 0.0316(6) 0.5925(4) -0.3316(3) 0.096(2) Uani 1 d . . H31A H -0.0307(30) 0.6387(9) -0.3816(14) 0.144 Uiso 1 calc R . H31B H 0.1255(11) 0.5912(5) -0.3448(23) 0.144 Uiso 1 calc R . H31C H 0.0055(39) 0.6254(13) -0.2896(10) 0.144 Uiso 1 calc R . C32 C 0.0648(5) 0.4154(5) -0.3639(3) 0.0839(14) Uani 1 d . . H32A H 0.1599(12) 0.4115(28) -0.3752(16) 0.126 Uiso 1 calc R . H32B H 0.0051(24) 0.4633(17) -0.4147(7) 0.126 Uiso 1 calc R . H32C H 0.0559(35) 0.3385(12) -0.3436(9) 0.126 Uiso 1 calc R . C33 C 0.4620(12) -0.0199(6) 0.4656(5) 0.085(3) Uani 0.50 d P . Cl5 Cl 0.6335(2) -0.01283(15) 0.46431(13) 0.1425(7) 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 Mo1 0.03482(14) 0.03141(13) 0.03939(15) -0.01644(11) -0.00083(10) -0.00505(10) P1 0.0436(4) 0.0331(4) 0.0394(4) -0.0147(3) -0.0019(3) -0.0099(3) P2 0.0461(5) 0.0404(4) 0.0438(4) -0.0243(4) 0.0061(4) -0.0163(4) Cl1 0.0713(6) 0.0446(4) 0.0578(5) -0.0212(4) 0.0140(4) -0.0203(4) O1 0.071(2) 0.069(2) 0.130(3) -0.055(2) 0.013(2) -0.006(2) O2 0.081(2) 0.0434(14) 0.0456(13) -0.0087(11) -0.0123(12) -0.0097(13) C1 0.038(2) 0.058(2) 0.063(2) -0.022(2) 0.000(2) -0.013(2) C2 0.062(2) 0.056(2) 0.054(2) -0.035(2) -0.006(2) -0.007(2) C3 0.076(3) 0.046(2) 0.054(2) -0.023(2) -0.018(2) -0.019(2) C4 0.051(2) 0.062(2) 0.062(2) -0.029(2) -0.014(2) -0.013(2) C5 0.066(2) 0.046(2) 0.048(2) -0.015(2) -0.020(2) -0.003(2) C6 0.076(3) 0.056(2) 0.041(2) -0.021(2) -0.004(2) -0.015(2) C7 0.036(2) 0.037(2) 0.040(2) -0.0174(13) 0.0020(13) -0.0080(13) C8 0.034(2) 0.056(2) 0.063(2) -0.028(2) 0.0064(15) -0.0107(15) C9 0.038(2) 0.069(3) 0.115(4) -0.034(3) -0.009(2) -0.005(2) C10 0.048(2) 0.076(3) 0.103(3) -0.041(2) 0.012(2) -0.032(2) C11 0.054(2) 0.103(3) 0.083(3) -0.051(3) 0.030(2) -0.025(2) C12 0.042(2) 0.041(2) 0.047(2) -0.0219(14) 0.0090(14) -0.0156(14) C13 0.058(2) 0.066(2) 0.067(2) -0.035(2) 0.030(2) -0.033(2) C14 0.113(4) 0.141(5) 0.061(3) -0.047(3) 0.042(3) -0.070(4) C15 0.080(3) 0.098(3) 0.097(3) -0.050(3) 0.038(3) -0.060(3) C16 0.092(4) 0.086(3) 0.162(5) -0.061(4) 0.089(4) -0.039(3) Mo2 0.0648(2) 0.03072(14) 0.03427(15) -0.01054(11) -0.00805(13) -0.01063(13) P3 0.0568(5) 0.0309(4) 0.0384(4) -0.0147(3) -0.0022(4) -0.0120(4) P4 0.0455(4) 0.0287(4) 0.0379(4) -0.0131(3) 0.0028(3) -0.0097(3) Cl3 0.0616(6) 0.0570(5) 0.0714(6) -0.0311(5) -0.0088(5) -0.0130(4) O3 0.125(3) 0.074(2) 0.065(2) -0.037(2) 0.015(2) -0.041(2) O4 0.068(2) 0.0479(14) 0.0465(13) -0.0227(11) -0.0089(11) -0.0133(12) C17 0.072(3) 0.057(2) 0.036(2) -0.008(2) 0.006(2) -0.028(2) C18 0.130(4) 0.032(2) 0.052(2) -0.003(2) -0.025(2) -0.022(2) C19 0.116(4) 0.030(2) 0.070(3) -0.012(2) -0.020(3) 0.004(2) C20 0.094(3) 0.042(2) 0.100(4) -0.011(2) -0.044(3) 0.004(2) C21 0.162(5) 0.045(2) 0.052(2) -0.007(2) -0.049(3) -0.011(3) C22 0.144(5) 0.043(2) 0.046(2) 0.002(2) -0.001(3) -0.022(3) C23 0.046(2) 0.0335(15) 0.036(2) -0.0156(12) 0.0003(13) -0.0062(13) C24 0.046(2) 0.048(2) 0.051(2) -0.023(2) 0.0084(15) -0.0088(15) C25 0.065(3) 0.098(3) 0.050(2) -0.034(2) 0.016(2) -0.020(2) C26 0.088(3) 0.064(2) 0.076(3) -0.031(2) 0.037(2) -0.035(2) C27 0.052(2) 0.072(3) 0.093(3) -0.034(2) 0.008(2) 0.000(2) C28 0.056(2) 0.037(2) 0.036(2) -0.0134(13) 0.0040(14) -0.0193(14) C29 0.068(2) 0.064(2) 0.058(2) -0.026(2) 0.021(2) -0.037(2) C30 0.049(2) 0.115(4) 0.083(3) -0.039(3) 0.010(2) -0.030(2) C31 0.109(4) 0.085(3) 0.115(4) -0.034(3) 0.035(3) -0.066(3) C32 0.077(3) 0.117(4) 0.086(3) -0.058(3) 0.037(3) -0.048(3) C33 0.144(9) 0.040(4) 0.048(4) 0.002(3) -0.050(5) -0.014(5) Cl5 0.1370(15) 0.0976(11) 0.156(2) -0.0090(11) 0.0426(13) -0.0397(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 Mo1 C1 2.036(4) . ? Mo1 C5 2.273(3) . ? Mo1 C12 2.278(3) . ? Mo1 C4 2.285(3) . ? Mo1 C7 2.301(3) . ? Mo1 C6 2.330(3) . ? Mo1 C3 2.346(3) . ? Mo1 C2 2.387(3) . ? Mo1 P2 2.4179(10) . ? Mo1 Cl1 2.5468(11) . ? Mo1 P1 2.8745(13) . ? P1 O2 1.581(3) . ? P1 C7 1.742(3) . ? P1 C12 1.742(3) . ? P1 P2 2.5424(13) . ? P2 C7 1.839(3) . ? P2 C12 1.848(3) . ? O1 C1 1.051(4) . ? C2 C3 1.394(5) . ? C2 C6 1.390(5) . ? C3 C4 1.417(5) . ? C4 C5 1.416(5) . ? C5 C6 1.415(5) . ? C7 C8 1.541(4) . ? C8 C11 1.526(5) . ? C8 C9 1.534(5) . ? C8 C10 1.531(5) . ? C12 C13 1.525(4) . ? C13 C16 1.515(6) . ? C13 C14 1.527(6) . ? C13 C15 1.533(5) . ? Mo2 C17 2.028(4) . ? Mo2 C21 2.268(4) . ? Mo2 C22 2.276(4) . ? Mo2 C28 2.275(3) . ? Mo2 C23 2.316(3) . ? Mo2 C18 2.323(4) . ? Mo2 C20 2.347(4) . ? Mo2 C19 2.387(4) . ? Mo2 P4 2.4287(11) . ? Mo2 Cl3 2.5345(11) . ? Mo2 P3 2.8659(10) . ? P3 O4 1.584(2) . ? P3 C23 1.740(3) . ? P3 C28 1.744(3) . ? P3 P4 2.5457(12) . ? P4 C23 1.834(3) . ? P4 C28 1.846(3) . ? O3 C17 1.060(4) . ? C18 C19 1.402(7) . ? C18 C22 1.402(6) . ? C19 C20 1.395(6) . ? C20 C21 1.406(7) . ? C21 C22 1.405(7) . ? C23 C24 1.540(4) . ? C24 C27 1.520(5) . ? C24 C26 1.529(5) . ? C24 C25 1.541(5) . ? C28 C29 1.534(5) . ? C29 C32 1.521(5) . ? C29 C30 1.532(6) . ? C29 C31 1.543(5) . ? C33 Cl5 1.613(11) 2_656 ? C33 C33 1.74(2) 2_656 ? C33 Cl5 1.755(12) . ? Cl5 C33 1.613(11) 2_656 ? 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 C1 Mo1 C5 84.38(14) . . ? C1 Mo1 C12 90.28(13) . . ? C5 Mo1 C12 137.24(13) . . ? C1 Mo1 C4 84.50(14) . . ? C5 Mo1 C4 36.20(13) . . ? C12 Mo1 C4 101.09(13) . . ? C1 Mo1 C7 127.05(12) . . ? C5 Mo1 C7 146.40(12) . . ? C12 Mo1 C7 62.93(11) . . ? C4 Mo1 C7 141.90(12) . . ? C1 Mo1 C6 117.10(14) . . ? C5 Mo1 C6 35.77(13) . . ? C12 Mo1 C6 141.90(12) . . ? C4 Mo1 C6 59.33(14) . . ? C7 Mo1 C6 110.68(12) . . ? C1 Mo1 C3 117.28(14) . . ? C5 Mo1 C3 59.03(13) . . ? C12 Mo1 C3 86.97(12) . . ? C4 Mo1 C3 35.61(12) . . ? C7 Mo1 C3 106.53(11) . . ? C6 Mo1 C3 57.70(14) . . ? C1 Mo1 C2 140.77(13) . . ? C5 Mo1 C2 58.43(12) . . ? C12 Mo1 C2 108.04(12) . . ? C4 Mo1 C2 58.50(13) . . ? C7 Mo1 C2 92.08(11) . . ? C6 Mo1 C2 34.26(12) . . ? C3 Mo1 C2 34.25(13) . . ? C1 Mo1 P2 82.19(11) . . ? C5 Mo1 P2 166.21(9) . . ? C12 Mo1 P2 46.22(8) . . ? C4 Mo1 P2 144.28(10) . . ? C7 Mo1 P2 45.80(7) . . ? C6 Mo1 P2 154.19(10) . . ? C3 Mo1 P2 130.98(9) . . ? C2 Mo1 P2 135.35(9) . . ? C1 Mo1 Cl1 79.99(10) . . ? C5 Mo1 Cl1 88.03(10) . . ? C12 Mo1 Cl1 132.76(8) . . ? C4 Mo1 Cl1 123.42(10) . . ? C7 Mo1 Cl1 86.65(8) . . ? C6 Mo1 Cl1 80.69(10) . . ? C3 Mo1 Cl1 138.39(10) . . ? C2 Mo1 Cl1 108.32(10) . . ? P2 Mo1 Cl1 86.56(4) . . ? C1 Mo1 P1 126.77(11) . . ? C5 Mo1 P1 135.91(9) . . ? C12 Mo1 P1 37.30(8) . . ? C4 Mo1 P1 108.85(10) . . ? C7 Mo1 P1 37.30(8) . . ? C6 Mo1 P1 113.62(9) . . ? C3 Mo1 P1 77.80(9) . . ? C2 Mo1 P1 81.29(9) . . ? P2 Mo1 P1 56.63(3) . . ? Cl1 Mo1 P1 123.94(3) . . ? O2 P1 C7 118.31(15) . . ? O2 P1 C12 116.0(2) . . ? C7 P1 C12 86.65(14) . . ? O2 P1 P2 110.05(11) . . ? C7 P1 P2 46.33(10) . . ? C12 P1 P2 46.61(10) . . ? O2 P1 Mo1 162.53(11) . . ? C7 P1 Mo1 53.17(10) . . ? C12 P1 Mo1 52.43(10) . . ? P2 P1 Mo1 52.59(3) . . ? C7 P2 C12 80.83(13) . . ? C7 P2 Mo1 63.74(9) . . ? C12 P2 Mo1 62.91(10) . . ? C7 P2 P1 43.24(9) . . ? C12 P2 P1 43.25(10) . . ? Mo1 P2 P1 70.78(3) . . ? O1 C1 Mo1 173.9(4) . . ? C3 C2 C6 108.3(3) . . ? C3 C2 Mo1 71.3(2) . . ? C6 C2 Mo1 70.7(2) . . ? C2 C3 C4 108.7(3) . . ? C2 C3 Mo1 74.5(2) . . ? C4 C3 Mo1 69.8(2) . . ? C5 C4 C3 106.9(3) . . ? C5 C4 Mo1 71.5(2) . . ? C3 C4 Mo1 74.6(2) . . ? C6 C5 C4 107.6(3) . . ? C6 C5 Mo1 74.3(2) . . ? C4 C5 Mo1 72.3(2) . . ? C2 C6 C5 108.5(4) . . ? C2 C6 Mo1 75.1(2) . . ? C5 C6 Mo1 69.9(2) . . ? C8 C7 P1 127.3(2) . . ? C8 C7 P2 128.8(2) . . ? P1 C7 P2 90.42(14) . . ? C8 C7 Mo1 132.2(2) . . ? P1 C7 Mo1 89.53(12) . . ? P2 C7 Mo1 70.46(10) . . ? C11 C8 C9 108.2(3) . . ? C11 C8 C10 109.2(3) . . ? C9 C8 C10 109.2(3) . . ? C11 C8 C7 110.9(3) . . ? C9 C8 C7 109.2(3) . . ? C10 C8 C7 110.2(3) . . ? C13 C12 P1 126.5(2) . . ? C13 C12 P2 126.6(2) . . ? P1 C12 P2 90.14(14) . . ? C13 C12 Mo1 134.5(2) . . ? P1 C12 Mo1 90.27(13) . . ? P2 C12 Mo1 70.87(10) . . ? C16 C13 C12 111.6(3) . . ? C16 C13 C14 110.4(4) . . ? C12 C13 C14 109.7(3) . . ? C16 C13 C15 108.4(4) . . ? C12 C13 C15 109.4(3) . . ? C14 C13 C15 107.2(4) . . ? C17 Mo2 C21 83.9(2) . . ? C17 Mo2 C22 85.3(2) . . ? C21 Mo2 C22 36.0(2) . . ? C17 Mo2 C28 90.19(13) . . ? C21 Mo2 C28 134.7(2) . . ? C22 Mo2 C28 98.9(2) . . ? C17 Mo2 C23 125.72(12) . . ? C21 Mo2 C23 148.8(2) . . ? C22 Mo2 C23 141.15(14) . . ? C28 Mo2 C23 62.70(11) . . ? C17 Mo2 C18 118.3(2) . . ? C21 Mo2 C18 59.0(2) . . ? C22 Mo2 C18 35.48(15) . . ? C28 Mo2 C18 85.72(14) . . ? C23 Mo2 C18 106.20(12) . . ? C17 Mo2 C20 115.7(2) . . ? C21 Mo2 C20 35.4(2) . . ? C22 Mo2 C20 59.0(2) . . ? C28 Mo2 C20 141.94(14) . . ? C23 Mo2 C20 113.5(2) . . ? C18 Mo2 C20 58.0(2) . . ? C17 Mo2 C19 140.64(15) . . ? C21 Mo2 C19 58.2(2) . . ? C22 Mo2 C19 58.3(2) . . ? C28 Mo2 C19 108.54(14) . . ? C23 Mo2 C19 93.58(13) . . ? C18 Mo2 C19 34.6(2) . . ? C20 Mo2 C19 34.3(2) . . ? C17 Mo2 P4 81.39(10) . . ? C21 Mo2 P4 165.26(14) . . ? C22 Mo2 P4 142.0(2) . . ? C28 Mo2 P4 46.07(8) . . ? C23 Mo2 P4 45.39(7) . . ? C18 Mo2 P4 129.63(11) . . ? C20 Mo2 P4 156.8(2) . . ? C19 Mo2 P4 136.34(11) . . ? C17 Mo2 Cl3 81.51(11) . . ? C21 Mo2 Cl3 88.4(2) . . ? C22 Mo2 Cl3 123.99(15) . . ? C28 Mo2 Cl3 135.12(8) . . ? C23 Mo2 Cl3 86.90(8) . . ? C18 Mo2 Cl3 136.69(14) . . ? C20 Mo2 Cl3 78.83(13) . . ? C19 Mo2 Cl3 105.37(14) . . ? P4 Mo2 Cl3 89.05(4) . . ? C17 Mo2 P3 126.74(11) . . ? C21 Mo2 P3 135.12(12) . . ? C22 Mo2 P3 107.08(13) . . ? C28 Mo2 P3 37.49(8) . . ? C23 Mo2 P3 37.37(8) . . ? C18 Mo2 P3 76.62(10) . . ? C20 Mo2 P3 114.80(13) . . ? C19 Mo2 P3 81.94(11) . . ? P4 Mo2 P3 56.76(3) . . ? Cl3 Mo2 P3 124.22(3) . . ? O4 P3 C23 118.05(14) . . ? O4 P3 C28 116.0(2) . . ? C23 P3 C28 86.58(14) . . ? O4 P3 P4 110.34(10) . . ? C23 P3 P4 46.07(10) . . ? C28 P3 P4 46.47(10) . . ? O4 P3 Mo2 163.13(10) . . ? C23 P3 Mo2 53.90(10) . . ? C28 P3 Mo2 52.55(11) . . ? P4 P3 Mo2 52.93(3) . . ? C23 P4 C28 80.97(14) . . ? C23 P4 Mo2 64.05(9) . . ? C28 P4 Mo2 62.57(10) . . ? C23 P4 P3 43.11(10) . . ? C28 P4 P3 43.24(10) . . ? Mo2 P4 P3 70.31(3) . . ? O3 C17 Mo2 174.9(4) . . ? C19 C18 C22 108.4(4) . . ? C19 C18 Mo2 75.2(2) . . ? C22 C18 Mo2 70.4(2) . . ? C20 C19 C18 108.1(5) . . ? C20 C19 Mo2 71.3(2) . . ? C18 C19 Mo2 70.2(2) . . ? C19 C20 C21 107.9(5) . . ? C19 C20 Mo2 74.5(2) . . ? C21 C20 Mo2 69.2(2) . . ? C22 C21 C20 108.2(4) . . ? C22 C21 Mo2 72.3(2) . . ? C20 C21 Mo2 75.3(2) . . ? C18 C22 C21 107.4(5) . . ? C18 C22 Mo2 74.1(2) . . ? C21 C22 Mo2 71.7(2) . . ? C24 C23 P3 127.7(2) . . ? C24 C23 P4 128.2(2) . . ? P3 C23 P4 90.81(15) . . ? C24 C23 Mo2 132.6(2) . . ? P3 C23 Mo2 88.73(13) . . ? P4 C23 Mo2 70.55(10) . . ? C27 C24 C26 109.7(3) . . ? C27 C24 C23 111.0(3) . . ? C26 C24 C23 111.3(3) . . ? C27 C24 C25 109.1(3) . . ? C26 C24 C25 107.0(3) . . ? C23 C24 C25 108.6(3) . . ? C29 C28 P3 126.7(2) . . ? C29 C28 P4 125.6(2) . . ? P3 C28 P4 90.29(14) . . ? C29 C28 Mo2 135.1(2) . . ? P3 C28 Mo2 89.97(14) . . ? P4 C28 Mo2 71.36(11) . . ? C32 C29 C30 108.1(4) . . ? C32 C29 C28 112.2(3) . . ? C30 C29 C28 109.6(3) . . ? C32 C29 C31 109.2(3) . . ? C30 C29 C31 108.1(4) . . ? C28 C29 C31 109.5(3) . . ? Cl5 C33 C33 63.0(6) 2_656 2_656 ? Cl5 C33 Cl5 118.0(4) 2_656 . ? C33 C33 Cl5 55.0(6) 2_656 . ? C33 Cl5 C33 62.0(4) 2_656 . ? 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 C12 P2 C7 P1 -25.12(13) . . . . ? C23 P4 C28 P3 24.50(13) . . . . ? _refine_diff_density_max 0.681 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.060 #===END