# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1290 data_global _publ_contact_author m.g.b.drew _publ_contact_author_email m.g.b.drew@reading.ac.uk _publ_contact_author_fax '44 118 931 6331' _publ_contact_author_phone '44 118 931 8789' loop_ _publ_contact_letter ;Dr M.G.B.Drew Department of Chemistry University of Reading, Whiteknights, Reading RG6 6AD ; data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H33 Cl I O11 P3 W4 ' _chemical_formula_weight 1674.32 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' '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' 'I' 'I' -0.4742 1.8119 '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' _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 11.759(14) _cell_length_b 14.428(16) _cell_length_c 14.855(16) _cell_angle_alpha 78.131(10) _cell_angle_beta 88.426(10) _cell_angle_gamma 86.037(10) _cell_volume 2460(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 10.151 _exptl_absorpt_correction_type 'DIFABS (Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6165 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.11 _reflns_number_total 6165 _reflns_number_gt 3689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.0048(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6165 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1637 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2638 _refine_ls_wR_factor_gt 0.2219 _refine_ls_goodness_of_fit_ref 1.300 _refine_ls_restrained_S_all 1.300 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.002 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 W1 W 0.18206(11) 0.21452(10) 0.06252(10) 0.0545(5) Uani 1 d . . . I5 I 0.0009(2) 0.36030(18) 0.0379(2) 0.0711(8) Uani 1 d . . . P1 P 0.1942(8) 0.2634(7) -0.1129(7) 0.062(2) Uani 1 d . . . C11 C 0.259(3) 0.178(2) -0.170(2) 0.057(8) Uiso 1 d . . . C12 C 0.353(3) 0.189(3) -0.234(3) 0.073(10) Uiso 1 d . . . H12 H 0.3849 0.2475 -0.2493 0.088 Uiso 1 calc R . . C13 C 0.398(4) 0.112(3) -0.274(3) 0.089(13) Uiso 1 d . . . H13 H 0.4548 0.1257 -0.3186 0.107 Uiso 1 calc R . . C14 C 0.367(3) 0.023(3) -0.253(3) 0.068(10) Uiso 1 d . . . H14 H 0.4055 -0.0248 -0.2778 0.082 Uiso 1 calc R . . C15 C 0.268(4) 0.003(3) -0.190(3) 0.084(12) Uiso 1 d . . . H15 H 0.2413 -0.0569 -0.1746 0.101 Uiso 1 calc R . . C16 C 0.212(4) 0.085(4) -0.149(4) 0.102(15) Uiso 1 d . . . H16 H 0.1485 0.0746 -0.1114 0.123 Uiso 1 calc R . . C21 C 0.068(3) 0.309(2) -0.182(2) 0.055(8) Uiso 1 d . . . C22 C -0.045(5) 0.263(4) -0.152(4) 0.107(16) Uiso 1 d . . . H22 H -0.0512 0.2191 -0.0967 0.128 Uiso 1 calc R . . C23 C -0.126(4) 0.286(3) -0.202(3) 0.085(12) Uiso 1 d . . . H23 H -0.1865 0.2468 -0.1913 0.102 Uiso 1 calc R . . C24 C -0.140(5) 0.370(4) -0.281(4) 0.106(16) Uiso 1 d . . . H24 H -0.2093 0.3923 -0.3077 0.127 Uiso 1 calc R . . C25 C -0.037(3) 0.410(3) -0.309(3) 0.075(11) Uiso 1 d . . . H25 H -0.0362 0.4588 -0.3602 0.091 Uiso 1 calc R . . C26 C 0.068(4) 0.380(3) -0.262(3) 0.080(11) Uiso 1 d . . . H26 H 0.1356 0.4072 -0.2838 0.096 Uiso 1 calc R . . C2 C 0.293(4) 0.363(3) -0.141(3) 0.093(13) Uiso 1 d . . . H2A H 0.3716 0.3369 -0.1419 0.112 Uiso 1 calc R . . H2B H 0.2767 0.4005 -0.2022 0.112 Uiso 1 calc R . . C3 C 0.280(4) 0.431(3) -0.068(3) 0.077(11) Uiso 1 d . . . H3A H 0.2047 0.4631 -0.0714 0.092 Uiso 1 calc R . . H3B H 0.3359 0.4788 -0.0808 0.092 Uiso 1 calc R . . P4 P 0.3021(8) 0.3594(6) 0.0459(7) 0.057(2) Uani 1 d . . . C31 C 0.457(3) 0.334(2) 0.073(3) 0.062(9) Uiso 1 d . . . C32 C 0.487(4) 0.289(3) 0.161(3) 0.077(11) Uiso 1 d . . . H32 H 0.4350 0.2741 0.2091 0.092 Uiso 1 calc R . . C33 C 0.601(5) 0.271(4) 0.171(4) 0.112(17) Uiso 1 d . . . H33 H 0.6228 0.2409 0.2298 0.135 Uiso 1 calc R . . C34 C 0.692(3) 0.288(3) 0.108(3) 0.072(10) Uiso 1 d . . . H34 H 0.7678 0.2678 0.1232 0.086 Uiso 1 calc R . . C35 C 0.659(4) 0.337(3) 0.021(3) 0.081(12) Uiso 1 d . . . H35 H 0.7153 0.3564 -0.0224 0.098 Uiso 1 calc R . . C36 C 0.544(4) 0.361(3) -0.005(3) 0.080(11) Uiso 1 d . . . H36 H 0.5236 0.3902 -0.0645 0.095 Uiso 1 calc R . . C5 C 0.252(3) 0.433(2) 0.131(2) 0.054(8) Uiso 1 d . . . H5A H 0.3140 0.4694 0.1438 0.065 Uiso 1 calc R . . H5B H 0.1901 0.4771 0.1054 0.065 Uiso 1 calc R . . C6 C 0.211(4) 0.371(3) 0.223(3) 0.077(11) Uiso 1 d . . . H6A H 0.1493 0.4068 0.2470 0.092 Uiso 1 calc R . . H6B H 0.2734 0.3630 0.2660 0.092 Uiso 1 calc R . . P7 P 0.1624(8) 0.2510(7) 0.2229(7) 0.057(2) Uani 1 d . . . C41 C 0.021(3) 0.244(3) 0.276(2) 0.062(10) Uani 1 d . . . C42 C -0.045(4) 0.323(4) 0.293(3) 0.097(14) Uiso 1 d . . . H42 H -0.0150 0.3823 0.2740 0.116 Uiso 1 calc R . . C43 C -0.173(5) 0.319(4) 0.343(4) 0.119(18) Uiso 1 d . . . H43 H -0.2145 0.3705 0.3581 0.143 Uiso 1 calc R . . C44 C -0.202(5) 0.242(4) 0.357(4) 0.113(17) Uiso 1 d . . . H44 H -0.2727 0.2353 0.3868 0.136 Uiso 1 calc R . . C45 C -0.148(5) 0.154(4) 0.336(4) 0.106(16) Uiso 1 d . . . H45 H -0.1867 0.0983 0.3451 0.127 Uiso 1 calc R . . C46 C -0.029(4) 0.156(4) 0.300(4) 0.098(14) Uiso 1 d . . . H46 H 0.0116 0.1006 0.2930 0.117 Uiso 1 calc R . . C51 C 0.251(3) 0.173(2) 0.308(3) 0.057(8) Uiso 1 d . . . C52 C 0.279(4) 0.077(3) 0.310(3) 0.085(12) Uiso 1 d . . . H52 H 0.2663 0.0549 0.2568 0.102 Uiso 1 calc R . . C53 C 0.324(4) 0.009(4) 0.387(4) 0.101(15) Uiso 1 d . . . H53 H 0.3315 -0.0565 0.3893 0.121 Uiso 1 calc R . . C54 C 0.355(6) 0.051(5) 0.454(5) 0.14(2) Uiso 1 d . . . H54 H 0.4020 0.0135 0.4985 0.166 Uiso 1 calc R . . C55 C 0.327(8) 0.138(7) 0.467(7) 0.20(4) Uiso 1 d . . . H55 H 0.3408 0.1529 0.5233 0.243 Uiso 1 calc R . . C56 C 0.282(6) 0.203(6) 0.402(5) 0.15(3) Uiso 1 d . . . H56 H 0.2672 0.2651 0.4093 0.185 Uiso 1 calc R . . C61 C 0.232(5) -0.031(4) 0.095(4) 0.126(19) Uiso 1 d . . . H61A H 0.3025 -0.0643 0.1158 0.151 Uiso 1 calc R . . H61B H 0.2106 -0.0471 0.0386 0.151 Uiso 1 calc R . . H61C H 0.1733 -0.0476 0.1409 0.151 Uiso 1 calc R . . C62 C 0.245(3) 0.076(2) 0.079(2) 0.054(8) Uiso 1 d . . . C63 C 0.329(3) 0.139(3) 0.063(3) 0.064(9) Uiso 1 d . . . C64 C 0.446(3) 0.123(3) 0.047(3) 0.074(11) Uiso 1 d . . . H64A H 0.4889 0.1459 0.0911 0.089 Uiso 1 calc R . . H64B H 0.4660 0.1548 -0.0139 0.089 Uiso 1 calc R . . H64C H 0.4643 0.0557 0.0533 0.089 Uiso 1 calc R . . C100 C 0.049(5) 0.135(4) 0.078(4) 0.109(16) Uiso 1 d . . . O100 O -0.029(3) 0.086(2) 0.083(2) 0.094(9) Uiso 1 d . . . W2 W 0.50037(13) 0.50035(11) 0.65863(11) 0.0637(6) Uani 1 d . . . W3 W 0.69249(13) 0.53570(12) 0.48836(12) 0.0659(6) Uani 1 d . . . W4 W 0.44467(14) 0.66272(11) 0.46826(12) 0.0682(6) Uani 1 d . . . O1 O 0.829(3) 0.555(2) 0.482(2) 0.099(9) Uiso 1 d . . . O2 O 0.502(2) 0.498(2) 0.773(2) 0.082(8) Uiso 1 d . . . O3 O 0.399(2) 0.780(2) 0.449(2) 0.086(8) Uiso 1 d . . . O4 O 0.656(2) 0.5281(17) 0.6206(18) 0.068(6) Uiso 1 d . . . O5 O 0.652(2) 0.5325(17) 0.3645(18) 0.068(6) Uiso 1 d . . . O6 O 0.454(2) 0.6316(18) 0.6045(19) 0.073(7) Uiso 1 d . . . O7 O 0.545(2) 0.3616(17) 0.6556(17) 0.065(6) Uiso 1 d . . . O8 O 0.602(2) 0.6566(17) 0.4643(17) 0.063(6) Uiso 1 d . . . O9 O 0.698(2) 0.4053(19) 0.510(2) 0.079(7) Uiso 1 d . . . O10 O 0.5000 0.5000 0.5000 0.073(10) Uiso 1 d S . . C200 C 0.039(7) -0.102(6) 0.320(7) 0.07(2) Uiso 0.50 d P A 1 H20A H 0.0639 -0.1243 0.2652 0.088 Uiso 0.50 calc PR A 1 H20B H 0.0273 -0.0333 0.3070 0.088 Uiso 0.50 calc PR A 1 Cl21 Cl 0.115(5) -0.138(4) 0.399(4) 0.20(2) Uiso 0.50 d P A 1 Cl22 Cl -0.100(5) -0.168(4) 0.383(4) 0.22(2) Uiso 0.50 d P A 1 O200 O 0.038(12) -0.097(9) 0.377(10) 0.19(5) Uiso 0.50 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0577(9) 0.0540(10) 0.0517(11) -0.0109(7) -0.0026(6) -0.0035(6) I5 0.0578(15) 0.0691(17) 0.085(2) -0.0138(13) -0.0063(11) 0.0060(10) P1 0.062(6) 0.069(6) 0.058(7) -0.019(5) -0.001(4) -0.003(4) P4 0.062(6) 0.050(5) 0.062(7) -0.019(4) 0.003(4) -0.008(4) P7 0.063(6) 0.067(6) 0.043(6) -0.015(4) 0.003(4) -0.002(4) C41 0.05(2) 0.10(3) 0.05(2) -0.03(2) 0.004(14) 0.019(16) W2 0.0678(10) 0.0703(11) 0.0540(12) -0.0137(8) -0.0012(7) -0.0085(7) W3 0.0594(10) 0.0775(12) 0.0610(12) -0.0137(8) -0.0016(7) -0.0075(7) W4 0.0801(12) 0.0565(11) 0.0648(13) -0.0078(8) 0.0019(8) 0.0032(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C100 1.98(6) . ? W1 C63 1.97(4) . ? W1 C62 2.05(3) . ? W1 P7 2.544(10) . ? W1 P1 2.558(11) . ? W1 P4 2.569(9) . ? W1 I5 2.864(4) . ? P1 C11 1.76(3) . ? P1 C21 1.83(4) . ? P1 C2 1.89(5) . ? C11 C12 1.42(5) . ? C11 C16 1.47(6) . ? C12 C13 1.43(6) . ? C13 C14 1.34(6) . ? C14 C15 1.48(5) . ? C15 C16 1.52(6) . ? C21 C26 1.40(5) . ? C21 C22 1.54(6) . ? C22 C23 1.21(6) . ? C23 C24 1.50(7) . ? C24 C25 1.40(6) . ? C25 C26 1.43(6) . ? C2 C3 1.61(6) . ? C3 P4 1.80(4) . ? P4 C31 1.87(4) . ? P4 C5 1.87(3) . ? C31 C32 1.38(6) . ? C31 C36 1.53(5) . ? C32 C33 1.35(6) . ? C33 C34 1.40(6) . ? C34 C35 1.40(6) . ? C35 C36 1.41(6) . ? C5 C6 1.55(5) . ? C6 P7 1.86(4) . ? P7 C51 1.81(4) . ? P7 C41 1.83(3) . ? C41 C42 1.39(6) . ? C41 C46 1.41(6) . ? C42 C43 1.66(7) . ? C43 C44 1.16(7) . ? C44 C45 1.48(7) . ? C45 C46 1.48(7) . ? C51 C52 1.40(5) . ? C51 C56 1.60(8) . ? C52 C53 1.43(7) . ? C53 C54 1.35(8) . ? C54 C55 1.33(10) . ? C55 C56 1.30(11) . ? C61 C62 1.53(6) . ? C62 C63 1.37(5) . ? C63 C64 1.41(5) . ? C100 O100 1.19(6) . ? W2 O2 1.69(3) . ? W2 O6 1.95(3) . ? W2 O5 1.94(2) 2_666 ? W2 O4 1.95(2) . ? W2 O7 2.04(2) . ? W2 O10 2.358(3) . ? W3 O1 1.64(3) . ? W3 O9 1.84(3) . ? W3 O5 1.92(3) . ? W3 O8 1.95(2) . ? W3 O4 1.98(3) . ? W3 O10 2.350(3) . ? W4 O3 1.71(3) . ? W4 O8 1.84(2) . ? W4 O7 1.94(3) 2_666 ? W4 O6 1.98(3) . ? W4 O9 1.99(3) 2_666 ? W4 O10 2.347(3) . ? O5 W2 1.94(2) 2_666 ? O7 W4 1.94(3) 2_666 ? O9 W4 1.99(3) 2_666 ? O10 W4 2.347(3) 2_666 ? O10 W3 2.350(3) 2_666 ? O10 W2 2.358(3) 2_666 ? C200 Cl21 1.47(11) . ? C200 Cl22 2.06(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 C100 W1 C63 112.6(19) . . ? C100 W1 C62 72.9(18) . . ? C63 W1 C62 39.8(14) . . ? C100 W1 P7 94.4(17) . . ? C63 W1 P7 104.8(12) . . ? C62 W1 P7 106.5(10) . . ? C100 W1 P1 100.8(17) . . ? C63 W1 P1 90.2(12) . . ? C62 W1 P1 99.6(10) . . ? P7 W1 P1 152.7(3) . . ? C100 W1 P4 161.4(16) . . ? C63 W1 P4 86.0(11) . . ? C62 W1 P4 125.6(9) . . ? P7 W1 P4 78.6(3) . . ? P1 W1 P4 79.9(3) . . ? C100 W1 I5 80.4(16) . . ? C63 W1 I5 166.0(11) . . ? C62 W1 I5 153.0(9) . . ? P7 W1 I5 78.4(2) . . ? P1 W1 I5 82.0(2) . . ? P4 W1 I5 81.3(2) . . ? C11 P1 C21 103.3(17) . . ? C11 P1 C2 102.5(18) . . ? C21 P1 C2 103.9(19) . . ? C11 P1 W1 116.0(13) . . ? C21 P1 W1 121.6(11) . . ? C2 P1 W1 107.3(16) . . ? C12 C11 C16 116(3) . . ? C12 C11 P1 128(3) . . ? C16 C11 P1 116(3) . . ? C11 C12 C13 121(4) . . ? C14 C13 C12 126(5) . . ? C13 C14 C15 117(4) . . ? C14 C15 C16 118(4) . . ? C11 C16 C15 120(4) . . ? C26 C21 C22 118(4) . . ? C26 C21 P1 124(3) . . ? C22 C21 P1 118(3) . . ? C23 C22 C21 118(5) . . ? C22 C23 C24 128(5) . . ? C25 C24 C23 113(5) . . ? C24 C25 C26 123(4) . . ? C21 C26 C25 119(4) . . ? C3 C2 P1 111(3) . . ? C2 C3 P4 109(3) . . ? C3 P4 C31 111.9(18) . . ? C3 P4 C5 107.9(17) . . ? C31 P4 C5 102.5(16) . . ? C3 P4 W1 108.0(14) . . ? C31 P4 W1 116.2(12) . . ? C5 P4 W1 109.9(11) . . ? C32 C31 C36 123(4) . . ? C32 C31 P4 118(3) . . ? C36 C31 P4 119(3) . . ? C33 C32 C31 113(4) . . ? C32 C33 C34 132(6) . . ? C33 C34 C35 113(4) . . ? C36 C35 C34 124(4) . . ? C35 C36 C31 115(4) . . ? C6 C5 P4 112(2) . . ? C5 C6 P7 119(3) . . ? C51 P7 C41 103.2(17) . . ? C51 P7 C6 103.6(18) . . ? C41 P7 C6 107.7(18) . . ? C51 P7 W1 114.0(12) . . ? C41 P7 W1 116.8(12) . . ? C6 P7 W1 110.4(14) . . ? C42 C41 C46 117(4) . . ? C42 C41 P7 123(3) . . ? C46 C41 P7 120(3) . . ? C41 C42 C43 124(5) . . ? C44 C43 C42 111(6) . . ? C43 C44 C45 131(7) . . ? C46 C45 C44 117(5) . . ? C41 C46 C45 119(4) . . ? C52 C51 C56 112(4) . . ? C52 C51 P7 125(3) . . ? C56 C51 P7 121(3) . . ? C51 C52 C53 126(5) . . ? C54 C53 C52 111(5) . . ? C55 C54 C53 129(8) . . ? C54 C55 C56 121(10) . . ? C55 C56 C51 118(8) . . ? C63 C62 C61 140(4) . . ? C63 C62 W1 67(2) . . ? C61 C62 W1 153(3) . . ? C62 C63 C64 129(4) . . ? C62 C63 W1 73(2) . . ? C64 C63 W1 157(3) . . ? O100 C100 W1 177(5) . . ? O2 W2 O6 103.9(12) . . ? O2 W2 O5 104.8(12) . 2_666 ? O6 W2 O5 88.0(11) . 2_666 ? O2 W2 O4 102.5(13) . . ? O6 W2 O4 88.2(10) . . ? O5 W2 O4 152.5(11) 2_666 . ? O2 W2 O7 101.4(12) . . ? O6 W2 O7 154.7(11) . . ? O5 W2 O7 84.3(10) 2_666 . ? O4 W2 O7 87.6(10) . . ? O2 W2 O10 178.8(10) . . ? O6 W2 O10 77.3(8) . . ? O5 W2 O10 75.3(8) 2_666 . ? O4 W2 O10 77.3(8) . . ? O7 W2 O10 77.4(7) . . ? O1 W3 O9 101.3(14) . . ? O1 W3 O5 104.6(14) . . ? O9 W3 O5 86.6(12) . . ? O1 W3 O8 109.5(13) . . ? O9 W3 O8 149.1(11) . . ? O5 W3 O8 83.4(10) . . ? O1 W3 O4 102.6(14) . . ? O9 W3 O4 88.3(11) . . ? O5 W3 O4 152.7(11) . . ? O8 W3 O4 87.4(10) . . ? O1 W3 O10 177.4(11) . . ? O9 W3 O10 76.1(9) . . ? O5 W3 O10 75.8(7) . . ? O8 W3 O10 73.1(7) . . ? O4 W3 O10 76.9(7) . . ? O3 W4 O8 107.3(12) . . ? O3 W4 O7 102.0(13) . 2_666 ? O8 W4 O7 85.8(11) . 2_666 ? O3 W4 O6 101.5(13) . . ? O8 W4 O6 87.9(11) . . ? O7 W4 O6 156.5(10) 2_666 . ? O3 W4 O9 104.1(13) . 2_666 ? O8 W4 O9 148.5(11) . 2_666 ? O7 W4 O9 89.6(11) 2_666 2_666 ? O6 W4 O9 84.0(11) . 2_666 ? O3 W4 O10 177.2(10) . . ? O8 W4 O10 75.0(7) . . ? O7 W4 O10 79.6(7) 2_666 . ? O6 W4 O10 76.9(7) . . ? O9 W4 O10 73.6(8) 2_666 . ? W2 O4 W3 115.8(13) . . ? W3 O5 W2 118.8(13) . 2_666 ? W2 O6 W4 115.8(13) . . ? W4 O7 W2 113.1(12) 2_666 . ? W4 O8 W3 122.0(12) . . ? W3 O9 W4 120.2(14) . 2_666 ? W4 O10 W4 180.0 2_666 . ? W4 O10 W3 90.03(7) 2_666 . ? W4 O10 W3 89.97(7) . . ? W4 O10 W3 89.97(7) 2_666 2_666 ? W4 O10 W3 90.03(7) . 2_666 ? W3 O10 W3 179.998(1) . 2_666 ? W4 O10 W2 90.07(6) 2_666 2_666 ? W4 O10 W2 89.93(6) . 2_666 ? W3 O10 W2 90.02(6) . 2_666 ? W3 O10 W2 89.98(6) 2_666 2_666 ? W4 O10 W2 89.93(6) 2_666 . ? W4 O10 W2 90.07(6) . . ? W3 O10 W2 89.98(6) . . ? W3 O10 W2 90.02(6) 2_666 . ? W2 O10 W2 180.0 2_666 . ? Cl21 C200 Cl22 94(6) . . ? _refine_diff_density_max 2.925 _refine_diff_density_min -3.419 _refine_diff_density_rms 0.448 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H61 B Cl2 I O P3 W' _chemical_formula_weight 1331.50 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.76(2) _cell_length_b 18.88(2) _cell_length_c 20.21(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.913(10) _cell_angle_gamma 90.00 _cell_volume 6015(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 2.642 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12735 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.05 _reflns_number_total 8386 _reflns_number_gt 5428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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^)+(0.1462P)^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_number_reflns 8386 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.2271 _refine_ls_wR_factor_gt 0.1981 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.75114(3) 0.22594(2) 0.45297(2) 0.0533(2) Uani 1 d . . . I1 I 0.83771(6) 0.18603(5) 0.35871(5) 0.0749(3) Uani 1 d . . . C100 C 0.7191(8) 0.3060(6) 0.3825(7) 0.063(3) Uani 1 d . . . O100 O 0.7039(8) 0.3528(5) 0.3439(7) 0.112(4) Uani 1 d . . . C64 C 0.6553(9) 0.1962(7) 0.5682(9) 0.097(5) Uani 1 d . . . H11A H 0.5980 0.2109 0.5605 0.117 Uiso 1 calc R . . H11B H 0.6906 0.2091 0.6149 0.117 Uiso 1 calc R . . H11C H 0.6569 0.1457 0.5627 0.117 Uiso 1 calc R . . C63 C 0.6856(8) 0.2301(6) 0.5182(7) 0.062(3) Uani 1 d . . . C62 C 0.6666(10) 0.2863(6) 0.4817(9) 0.085(4) Uani 1 d . . . C61 C 0.6119(13) 0.3478(8) 0.4672(12) 0.138(8) Uani 1 d . . . H14A H 0.6448 0.3891 0.4867 0.165 Uiso 1 calc R . . H14B H 0.5688 0.3415 0.4881 0.165 Uiso 1 calc R . . H14C H 0.5858 0.3535 0.4173 0.165 Uiso 1 calc R . . P1 P 0.6524(2) 0.12892(15) 0.38770(18) 0.0604(8) Uani 1 d . . . C2 C 0.6974(9) 0.0426(6) 0.4327(8) 0.081(4) Uani 1 d . . . H2A H 0.6752 0.0341 0.4705 0.097 Uiso 1 calc R . . H2B H 0.6783 0.0043 0.3991 0.097 Uiso 1 calc R . . C3 C 0.7933(8) 0.0416(6) 0.4627(7) 0.066(3) Uani 1 d . . . H4A H 0.8166 0.0428 0.4248 0.079 Uiso 1 calc R . . H4B H 0.8127 -0.0013 0.4897 0.079 Uiso 1 calc R . . P4 P 0.8287(2) 0.11874(15) 0.51885(17) 0.0587(8) Uani 1 d . . . C5 C 0.9416(8) 0.1287(6) 0.5330(7) 0.070(3) Uani 1 d . . . H6A H 0.9733 0.0954 0.5688 0.084 Uiso 1 calc R . . H6B H 0.9517 0.1171 0.4898 0.084 Uiso 1 calc R . . C6 C 0.9741(8) 0.2029(6) 0.5555(7) 0.065(3) Uani 1 d . . . H61 H 1.0243 0.2106 0.5428 0.078 Uiso 1 calc R . . H62 H 0.9914 0.2057 0.6064 0.078 Uiso 1 calc R . . P7 P 0.8974(2) 0.27607(14) 0.51718(16) 0.0519(7) Uani 1 d . . . C31 C 0.8236(8) 0.0960(6) 0.6045(6) 0.061(3) Uani 1 d . . . C32 C 0.7967(10) 0.0309(8) 0.6183(7) 0.084(4) Uani 1 d . . . H32 H 0.7817 -0.0034 0.5832 0.101 Uiso 1 calc R . . C33 C 0.7911(12) 0.0149(9) 0.6851(9) 0.110(6) Uani 1 d . . . H33 H 0.7720 -0.0289 0.6947 0.132 Uiso 1 calc R . . C34 C 0.8163(11) 0.0689(10) 0.7367(8) 0.100(5) Uani 1 d . . . H34 H 0.8116 0.0609 0.7806 0.120 Uiso 1 calc R . . C35 C 0.8462(12) 0.1303(9) 0.7245(8) 0.100(5) Uani 1 d . . . H35 H 0.8653 0.1637 0.7602 0.120 Uiso 1 calc R . . C36 C 0.8490(12) 0.1449(9) 0.6576(8) 0.099(5) Uani 1 d . . . H36 H 0.8686 0.1888 0.6490 0.119 Uiso 1 calc R . . C51 C 0.9122(8) 0.3294(6) 0.5956(6) 0.059(3) Uani 1 d . . . C52 C 0.8483(9) 0.3446(7) 0.6230(7) 0.073(4) Uani 1 d . . . H52 H 0.7936 0.3281 0.5998 0.088 Uiso 1 calc R . . C53 C 0.8641(10) 0.3828(7) 0.6824(8) 0.080(4) Uani 1 d . . . H53 H 0.8202 0.3924 0.6994 0.096 Uiso 1 calc R . . C54 C 0.9451(12) 0.4080(8) 0.7186(7) 0.086(4) Uani 1 d . . . H54 H 0.9556 0.4340 0.7597 0.103 Uiso 1 calc R . . C55 C 1.0103(10) 0.3940(7) 0.6927(7) 0.080(4) Uani 1 d . . . H55 H 1.0648 0.4105 0.7167 0.097 Uiso 1 calc R . . C56 C 0.9942(9) 0.3561(6) 0.6323(7) 0.069(3) Uani 1 d . . . H56 H 1.0380 0.3476 0.6148 0.082 Uiso 1 calc R . . C41 C 0.9467(8) 0.3336(6) 0.4684(6) 0.056(3) Uani 1 d . . . C42 C 0.9204(8) 0.4025(6) 0.4577(6) 0.062(3) Uani 1 d . . . H42 H 0.8789 0.4185 0.4751 0.074 Uiso 1 calc R . . C43 C 0.9537(8) 0.4475(7) 0.4224(7) 0.075(4) Uani 1 d . . . H43 H 0.9334 0.4936 0.4142 0.090 Uiso 1 calc R . . C44 C 1.0183(8) 0.4259(7) 0.3979(7) 0.074(4) Uani 1 d . . . H44 H 1.0426 0.4572 0.3747 0.089 Uiso 1 calc R . . C45 C 1.0445(10) 0.3570(7) 0.4094(7) 0.080(4) Uani 1 d . . . H45 H 1.0885 0.3414 0.3949 0.096 Uiso 1 calc R . . C46 C 1.0063(9) 0.3098(7) 0.4425(7) 0.072(4) Uani 1 d . . . H46 H 1.0217 0.2623 0.4468 0.086 Uiso 1 calc R . . C11 C 0.5451(8) 0.1302(6) 0.3930(8) 0.071(4) Uani 1 d . . . C12 C 0.4971(11) 0.1914(8) 0.3782(10) 0.106(5) Uani 1 d . . . H12 H 0.5185 0.2327 0.3656 0.127 Uiso 1 calc R . . C13 C 0.4136(13) 0.1900(13) 0.3827(14) 0.148(9) Uani 1 d . . . H13 H 0.3804 0.2307 0.3741 0.177 Uiso 1 calc R . . C14 C 0.3847(13) 0.1295(15) 0.3994(13) 0.144(10) Uani 1 d . . . H14 H 0.3307 0.1285 0.4027 0.173 Uiso 1 calc R . . C15 C 0.4313(13) 0.0690(12) 0.4120(13) 0.141(9) Uani 1 d . . . H15 H 0.4086 0.0269 0.4215 0.169 Uiso 1 calc R . . C16 C 0.5104(12) 0.0709(8) 0.4103(10) 0.105(6) Uani 1 d . . . H16 H 0.5431 0.0300 0.4215 0.126 Uiso 1 calc R . . C21 C 0.6307(10) 0.1153(9) 0.2934(7) 0.088(5) Uani 1 d . . . C22 C 0.5988(13) 0.1746(11) 0.2530(10) 0.123(7) Uani 1 d . . . H22 H 0.5934 0.2173 0.2742 0.148 Uiso 1 calc R . . C23 C 0.5741(17) 0.1694(17) 0.1781(15) 0.166(10) Uani 1 d . . . H23 H 0.5489 0.2071 0.1488 0.200 Uiso 1 calc R . . C24 C 0.5897(19) 0.1054(17) 0.1513(11) 0.151(10) Uani 1 d . . . H24 H 0.5763 0.0998 0.1030 0.181 Uiso 1 calc R . . C25 C 0.6237(15) 0.0519(16) 0.1946(13) 0.156(9) Uani 1 d . . . H25 H 0.6356 0.0108 0.1743 0.187 Uiso 1 calc R . . C26 C 0.6433(13) 0.0511(12) 0.2670(10) 0.137(8) Uani 1 d . . . H26 H 0.6629 0.0112 0.2948 0.164 Uiso 1 calc R . . B1 B 1.2608(11) 0.2030(8) 0.6215(9) 0.070(4) Uani 1 d . . . C101 C 1.2057(8) 0.1738(6) 0.6674(6) 0.061(3) Uani 1 d . . . C102 C 1.1936(10) 0.0998(8) 0.6717(7) 0.085(4) Uani 1 d . . . H102 H 1.2234 0.0689 0.6529 0.103 Uiso 1 calc R . . C103 C 1.1387(14) 0.0720(10) 0.7032(10) 0.121(6) Uani 1 d . . . H103 H 1.1286 0.0234 0.7013 0.145 Uiso 1 calc R . . C104 C 1.0982(11) 0.1162(13) 0.7379(8) 0.109(6) Uani 1 d . . . H104 H 1.0633 0.0978 0.7610 0.131 Uiso 1 calc R . . C105 C 1.1121(11) 0.1873(11) 0.7364(7) 0.098(5) Uani 1 d . . . H105 H 1.0875 0.2180 0.7599 0.117 Uiso 1 calc R . . C106 C 1.1624(9) 0.2144(8) 0.7004(7) 0.077(4) Uani 1 d . . . H106 H 1.1671 0.2634 0.6984 0.092 Uiso 1 calc R . . C71 C 1.2115(8) 0.1889(6) 0.5366(6) 0.058(3) Uani 1 d . . . C72 C 1.1468(10) 0.1409(7) 0.5105(7) 0.076(4) Uani 1 d . . . H72 H 1.1295 0.1144 0.5420 0.091 Uiso 1 calc R . . C73 C 1.1057(9) 0.1302(7) 0.4378(7) 0.075(4) Uani 1 d . . . H73 H 1.0612 0.0981 0.4218 0.090 Uiso 1 calc R . . C74 C 1.1320(11) 0.1675(9) 0.3913(8) 0.086(4) Uani 1 d . . . H74 H 1.1055 0.1599 0.3433 0.104 Uiso 1 calc R . . C75 C 1.1957(12) 0.2150(8) 0.4131(8) 0.087(5) Uani 1 d . . . H75 H 1.2131 0.2407 0.3813 0.104 Uiso 1 calc R . . C76 C 1.2345(9) 0.2239(7) 0.4860(8) 0.074(4) Uani 1 d . . . H76 H 1.2792 0.2559 0.5014 0.089 Uiso 1 calc R . . C81 C 1.2770(10) 0.2886(7) 0.6341(7) 0.075(4) Uani 1 d . . . C82 C 1.3507(11) 0.3206(8) 0.6811(9) 0.099(5) Uani 1 d . . . H82 H 1.3960 0.2912 0.7047 0.119 Uiso 1 calc R . . C83 C 1.3603(14) 0.3913(10) 0.6945(12) 0.131(7) Uani 1 d . . . H83 H 1.4086 0.4102 0.7279 0.157 Uiso 1 calc R . . C84 C 1.2925(16) 0.4337(8) 0.6545(14) 0.130(8) Uani 1 d . . . H84 H 1.2976 0.4825 0.6609 0.156 Uiso 1 calc R . . C85 C 1.2225(11) 0.4092(7) 0.6088(9) 0.088(5) Uani 1 d . . . H85 H 1.1794 0.4401 0.5841 0.105 Uiso 1 calc R . . C86 C 1.2129(9) 0.3368(7) 0.5973(8) 0.085(4) Uani 1 d . . . H86 H 1.1630 0.3197 0.5645 0.102 Uiso 1 calc R . . C91 C 1.3562(8) 0.1626(6) 0.6492(7) 0.068(3) Uani 1 d . . . C92 C 1.4012(9) 0.1451(7) 0.6048(8) 0.078(4) Uani 1 d . . . H92 H 1.3753 0.1525 0.5568 0.094 Uiso 1 calc R . . C93 C 1.4837(11) 0.1170(9) 0.6291(10) 0.101(5) Uani 1 d . . . H93 H 1.5142 0.1106 0.5988 0.121 Uiso 1 calc R . . C94 C 1.5169(11) 0.0998(10) 0.6969(14) 0.119(7) Uani 1 d . . . H94 H 1.5692 0.0770 0.7130 0.143 Uiso 1 calc R . . C95 C 1.4759(13) 0.1147(10) 0.7435(12) 0.121(6) Uani 1 d . . . H95 H 1.5004 0.1034 0.7910 0.145 Uiso 1 calc R . . C96 C 1.3973(12) 0.1469(8) 0.7183(10) 0.108(6) Uani 1 d . . . H96 H 1.3709 0.1586 0.7505 0.130 Uiso 1 calc R . . C10 C 0.6950(17) 0.5798(13) 0.5400(13) 0.153(8) Uiso 1 d . . . Cl11 Cl 0.7502(9) 0.5014(8) 0.5435(9) 0.074(4) Uiso 0.25 d P . . Cl12 Cl 0.6091(17) 0.5759(15) 0.4832(14) 0.141(8) Uiso 0.25 d P . . Cl21 Cl 0.7537(10) 0.5148(8) 0.5710(9) 0.072(4) Uiso 0.25 d P . . Cl22 Cl 0.6816(15) 0.6253(9) 0.6095(10) 0.087(5) Uiso 0.25 d P . . Cl31 Cl 0.7231(15) 0.6166(10) 0.6091(11) 0.107(6) Uiso 0.25 d P . . Cl32 Cl 0.5793(11) 0.5385(9) 0.5025(11) 0.092(5) Uiso 0.25 d P . . Cl41 Cl 0.6365(19) 0.6363(14) 0.5711(16) 0.148(8) Uiso 0.25 d P . . Cl42 Cl 0.5848(14) 0.5346(12) 0.4688(12) 0.109(6) Uiso 0.25 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0534(4) 0.0504(3) 0.0553(3) -0.0020(2) 0.0176(3) 0.00100(19) I1 0.0788(7) 0.0834(6) 0.0673(6) -0.0076(4) 0.0311(5) -0.0053(4) C100 0.056(9) 0.056(7) 0.074(9) -0.006(7) 0.017(7) 0.001(6) O100 0.117(10) 0.080(6) 0.119(9) 0.046(7) 0.016(7) 0.015(6) C64 0.047(10) 0.078(8) 0.137(15) 0.022(10) -0.007(9) -0.003(7) C63 0.059(9) 0.058(7) 0.075(8) -0.004(6) 0.031(7) -0.007(5) C62 0.081(11) 0.056(8) 0.098(11) -0.015(8) 0.007(9) 0.007(6) C61 0.16(2) 0.082(10) 0.19(2) -0.022(12) 0.093(18) 0.039(11) P1 0.062(2) 0.0541(16) 0.066(2) -0.0057(15) 0.0227(17) -0.0020(13) C2 0.082(12) 0.056(7) 0.098(11) -0.006(7) 0.022(9) -0.014(6) C3 0.061(9) 0.059(7) 0.076(9) 0.009(6) 0.022(7) 0.023(6) P4 0.070(2) 0.0529(16) 0.0526(18) -0.0003(14) 0.0200(16) 0.0053(14) C5 0.080(10) 0.060(7) 0.074(9) 0.020(6) 0.032(7) 0.016(6) C6 0.059(9) 0.056(6) 0.075(9) 0.000(6) 0.017(7) 0.002(5) P7 0.050(2) 0.0534(15) 0.0506(17) -0.0019(13) 0.0149(15) 0.0015(12) C31 0.066(9) 0.061(7) 0.054(7) 0.012(6) 0.016(6) 0.008(6) C32 0.101(12) 0.101(10) 0.040(7) 0.007(7) 0.012(7) -0.013(8) C33 0.141(17) 0.105(12) 0.084(12) 0.005(10) 0.038(11) -0.011(11) C34 0.120(15) 0.115(13) 0.063(10) 0.025(10) 0.030(9) -0.002(10) C35 0.123(15) 0.108(12) 0.073(11) -0.007(9) 0.039(10) -0.003(10) C36 0.133(16) 0.097(11) 0.068(10) 0.002(9) 0.034(10) -0.012(10) C51 0.078(10) 0.064(7) 0.038(6) 0.003(5) 0.023(6) 0.005(6) C52 0.073(10) 0.075(8) 0.081(9) -0.013(7) 0.036(8) 0.008(6) C53 0.084(12) 0.087(9) 0.077(9) -0.011(8) 0.039(9) 0.019(8) C54 0.123(15) 0.086(9) 0.051(8) -0.013(7) 0.032(9) 0.003(9) C55 0.091(12) 0.086(9) 0.051(8) -0.004(7) 0.005(8) -0.011(7) C56 0.076(10) 0.068(7) 0.060(8) -0.008(6) 0.020(7) -0.009(6) C41 0.059(8) 0.062(7) 0.040(6) -0.009(5) 0.007(6) -0.001(5) C42 0.074(9) 0.056(7) 0.060(8) -0.002(6) 0.030(7) 0.007(6) C43 0.056(9) 0.077(8) 0.085(10) -0.007(7) 0.015(8) 0.005(6) C44 0.058(9) 0.086(9) 0.079(9) 0.014(7) 0.024(7) 0.007(7) C45 0.092(11) 0.087(9) 0.076(9) 0.011(7) 0.047(9) 0.013(8) C46 0.082(10) 0.081(8) 0.067(8) 0.004(7) 0.043(8) 0.007(7) C11 0.055(9) 0.057(7) 0.090(10) -0.014(7) 0.009(7) -0.015(6) C12 0.098(14) 0.075(9) 0.152(17) -0.013(10) 0.054(12) 0.010(8) C13 0.058(14) 0.149(18) 0.23(3) -0.027(18) 0.040(15) 0.000(12) C14 0.069(15) 0.21(3) 0.17(2) -0.08(2) 0.069(15) -0.062(17) C15 0.101(17) 0.141(16) 0.22(2) 0.050(17) 0.099(18) 0.032(13) C16 0.115(15) 0.088(10) 0.143(16) 0.008(10) 0.083(13) 0.010(9) C21 0.093(12) 0.116(12) 0.053(8) -0.010(9) 0.020(8) -0.030(9) C22 0.141(18) 0.139(16) 0.072(12) 0.004(12) 0.012(11) -0.027(13) C23 0.15(2) 0.20(3) 0.14(2) 0.02(2) 0.049(19) -0.07(2) C24 0.19(3) 0.19(3) 0.058(12) -0.014(15) 0.032(15) -0.03(2) C25 0.14(2) 0.22(3) 0.114(19) -0.065(19) 0.046(16) 0.021(19) C26 0.157(19) 0.162(17) 0.085(13) -0.071(13) 0.033(12) -0.004(14) B1 0.065(11) 0.071(8) 0.074(11) -0.009(8) 0.022(9) 0.004(7) C101 0.059(9) 0.066(7) 0.050(7) 0.000(6) 0.008(6) 0.006(6) C102 0.099(12) 0.092(10) 0.069(9) -0.007(8) 0.034(9) -0.012(8) C103 0.150(19) 0.113(13) 0.109(14) 0.017(11) 0.056(14) -0.015(12) C104 0.101(14) 0.171(19) 0.064(10) 0.026(11) 0.040(10) 0.006(13) C105 0.116(15) 0.141(15) 0.034(8) -0.002(9) 0.022(8) 0.015(12) C106 0.069(10) 0.100(10) 0.059(8) 0.002(7) 0.020(7) 0.015(7) C71 0.056(9) 0.059(7) 0.055(7) 0.003(6) 0.015(6) 0.007(6) C72 0.100(12) 0.067(8) 0.063(9) 0.000(7) 0.031(8) 0.019(7) C73 0.053(9) 0.095(9) 0.061(9) -0.018(7) -0.003(7) 0.026(7) C74 0.097(13) 0.096(11) 0.069(10) -0.005(9) 0.032(9) 0.025(9) C75 0.118(15) 0.093(11) 0.054(9) 0.015(8) 0.036(9) 0.027(9) C76 0.058(10) 0.088(9) 0.072(9) 0.014(7) 0.017(7) 0.028(6) C81 0.093(12) 0.073(8) 0.059(8) 0.004(7) 0.024(8) 0.018(7) C82 0.099(13) 0.071(9) 0.102(12) -0.016(9) 0.002(10) -0.001(8) C83 0.134(19) 0.091(12) 0.153(19) -0.014(13) 0.030(15) -0.015(12) C84 0.15(2) 0.048(8) 0.22(3) -0.003(12) 0.100(19) 0.009(10) C85 0.080(13) 0.061(8) 0.127(14) 0.005(9) 0.042(11) 0.017(7) C86 0.055(10) 0.081(9) 0.118(13) 0.010(8) 0.027(9) 0.024(7) C91 0.068(10) 0.050(6) 0.080(10) 0.008(6) 0.016(8) 0.002(5) C92 0.064(11) 0.083(8) 0.088(10) 0.007(8) 0.026(8) 0.004(7) C93 0.074(13) 0.119(13) 0.104(13) 0.002(11) 0.025(11) 0.003(10) C94 0.056(13) 0.113(13) 0.18(2) 0.012(14) 0.024(14) 0.019(9) C95 0.092(16) 0.111(13) 0.130(17) 0.015(12) 0.000(13) 0.018(11) C96 0.107(15) 0.093(11) 0.097(13) -0.007(10) -0.001(11) 0.036(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 W1 C63 1.983(12) . ? W1 C100 2.020(14) . ? W1 C62 2.050(15) . ? W1 P1 2.520(4) . ? W1 P4 2.526(4) . ? W1 P7 2.534(4) . ? W1 I1 2.861(2) . ? C100 O100 1.149(14) . ? C64 C63 1.429(19) . ? C63 C62 1.269(18) . ? C62 C61 1.446(19) . ? P1 C21 1.833(14) . ? P1 C11 1.839(14) . ? P1 C2 1.894(13) . ? C2 C3 1.513(19) . ? C3 P4 1.817(12) . ? P4 C31 1.813(12) . ? P4 C5 1.825(14) . ? C5 C6 1.515(16) . ? C6 P7 1.867(12) . ? P7 C51 1.823(11) . ? P7 C41 1.841(12) . ? C31 C36 1.369(19) . ? C31 C32 1.372(17) . ? C32 C33 1.42(2) . ? C33 C34 1.42(2) . ? C34 C35 1.32(2) . ? C35 C36 1.40(2) . ? C51 C52 1.392(16) . ? C51 C56 1.414(17) . ? C52 C53 1.347(18) . ? C53 C54 1.39(2) . ? C54 C55 1.39(2) . ? C55 C56 1.361(17) . ? C41 C46 1.352(16) . ? C41 C42 1.368(15) . ? C42 C43 1.348(17) . ? C43 C44 1.396(17) . ? C44 C45 1.367(18) . ? C45 C46 1.394(17) . ? C11 C16 1.361(18) . ? C11 C12 1.381(19) . ? C12 C13 1.43(2) . ? C13 C14 1.33(3) . ? C14 C15 1.36(3) . ? C15 C16 1.34(2) . ? C21 C26 1.37(2) . ? C21 C22 1.38(2) . ? C22 C23 1.43(3) . ? C23 C24 1.38(3) . ? C24 C25 1.33(3) . ? C25 C26 1.39(3) . ? B1 C101 1.61(2) . ? B1 C81 1.644(19) . ? B1 C71 1.65(2) . ? B1 C91 1.69(2) . ? C101 C106 1.376(17) . ? C101 C102 1.419(18) . ? C102 C103 1.39(2) . ? C103 C104 1.41(2) . ? C104 C105 1.36(2) . ? C105 C106 1.38(2) . ? C71 C72 1.374(18) . ? C71 C76 1.377(17) . ? C72 C73 1.408(18) . ? C73 C74 1.36(2) . ? C74 C75 1.35(2) . ? C75 C76 1.40(2) . ? C81 C86 1.413(18) . ? C81 C82 1.41(2) . ? C82 C83 1.36(2) . ? C83 C84 1.40(3) . ? C84 C85 1.31(3) . ? C85 C86 1.386(19) . ? C91 C96 1.36(2) . ? C91 C92 1.395(18) . ? C92 C93 1.40(2) . ? C93 C94 1.33(2) . ? C94 C95 1.37(3) . ? C95 C96 1.38(2) . ? C10 Cl31 1.49(3) . ? C10 Cl12 1.51(3) . ? C10 Cl21 1.56(3) . ? C10 Cl41 1.71(3) . ? C10 Cl22 1.73(3) . ? C10 Cl11 1.73(3) . ? C10 Cl32 1.99(3) . ? C10 Cl42 2.10(3) . ? 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 C63 W1 C100 111.4(5) . . ? C63 W1 C62 36.6(5) . . ? C100 W1 C62 75.0(6) . . ? C63 W1 P1 87.9(4) . . ? C100 W1 P1 101.8(4) . . ? C62 W1 P1 99.1(4) . . ? C63 W1 P4 89.0(4) . . ? C100 W1 P4 159.5(3) . . ? C62 W1 P4 125.3(5) . . ? P1 W1 P4 79.72(14) . . ? C63 W1 P7 107.6(4) . . ? C100 W1 P7 93.4(4) . . ? C62 W1 P7 106.8(4) . . ? P1 W1 P7 152.63(10) . . ? P4 W1 P7 78.18(12) . . ? C63 W1 I1 166.9(3) . . ? C100 W1 I1 78.5(3) . . ? C62 W1 I1 153.0(5) . . ? P1 W1 I1 81.46(11) . . ? P4 W1 I1 81.58(10) . . ? P7 W1 I1 79.51(11) . . ? O100 C100 W1 177.2(11) . . ? C62 C63 C64 134.9(14) . . ? C62 C63 W1 74.6(9) . . ? C64 C63 W1 149.7(10) . . ? C63 C62 C61 143.6(17) . . ? C63 C62 W1 68.8(8) . . ? C61 C62 W1 147.2(14) . . ? C21 P1 C11 102.2(7) . . ? C21 P1 C2 106.6(8) . . ? C11 P1 C2 102.8(6) . . ? C21 P1 W1 120.6(5) . . ? C11 P1 W1 116.2(4) . . ? C2 P1 W1 106.9(4) . . ? C3 C2 P1 113.4(8) . . ? C2 C3 P4 108.4(8) . . ? C31 P4 C3 107.2(6) . . ? C31 P4 C5 105.0(6) . . ? C3 P4 C5 106.3(6) . . ? C31 P4 W1 120.7(4) . . ? C3 P4 W1 108.2(4) . . ? C5 P4 W1 108.6(4) . . ? C6 C5 P4 113.0(8) . . ? C5 C6 P7 115.6(9) . . ? C51 P7 C41 100.8(5) . . ? C51 P7 C6 100.2(6) . . ? C41 P7 C6 106.7(6) . . ? C51 P7 W1 118.2(4) . . ? C41 P7 W1 118.6(4) . . ? C6 P7 W1 110.2(4) . . ? C36 C31 C32 118.7(12) . . ? C36 C31 P4 119.1(10) . . ? C32 C31 P4 122.2(10) . . ? C31 C32 C33 121.2(14) . . ? C34 C33 C32 116.6(15) . . ? C35 C34 C33 122.2(15) . . ? C34 C35 C36 119.7(16) . . ? C31 C36 C35 121.5(15) . . ? C52 C51 C56 117.4(11) . . ? C52 C51 P7 124.4(11) . . ? C56 C51 P7 118.2(9) . . ? C53 C52 C51 121.4(14) . . ? C52 C53 C54 120.8(13) . . ? C55 C54 C53 119.4(13) . . ? C56 C55 C54 119.8(14) . . ? C55 C56 C51 121.2(13) . . ? C46 C41 C42 119.7(11) . . ? C46 C41 P7 122.5(9) . . ? C42 C41 P7 117.7(9) . . ? C43 C42 C41 120.9(11) . . ? C42 C43 C44 121.1(12) . . ? C45 C44 C43 117.4(13) . . ? C44 C45 C46 121.1(13) . . ? C41 C46 C45 119.7(12) . . ? C16 C11 C12 118.5(14) . . ? C16 C11 P1 121.0(11) . . ? C12 C11 P1 120.5(11) . . ? C11 C12 C13 118.7(17) . . ? C14 C13 C12 119(2) . . ? C13 C14 C15 122.3(19) . . ? C16 C15 C14 119.0(19) . . ? C15 C16 C11 122.8(16) . . ? C26 C21 C22 124.6(16) . . ? C26 C21 P1 121.7(15) . . ? C22 C21 P1 113.6(14) . . ? C21 C22 C23 119(2) . . ? C24 C23 C22 117(3) . . ? C25 C24 C23 120(2) . . ? C24 C25 C26 127(2) . . ? C21 C26 C25 113(2) . . ? C101 B1 C81 110.1(11) . . ? C101 B1 C71 111.1(12) . . ? C81 B1 C71 108.5(11) . . ? C101 B1 C91 108.6(11) . . ? C81 B1 C91 107.8(11) . . ? C71 B1 C91 110.7(11) . . ? C106 C101 C102 114.1(13) . . ? C106 C101 B1 126.1(11) . . ? C102 C101 B1 119.6(11) . . ? C103 C102 C101 122.2(15) . . ? C102 C103 C104 120.8(17) . . ? C105 C104 C103 117.3(16) . . ? C104 C105 C106 121.0(15) . . ? C101 C106 C105 124.4(15) . . ? C72 C71 C76 114.5(12) . . ? C72 C71 B1 123.7(11) . . ? C76 C71 B1 121.7(12) . . ? C71 C72 C73 122.5(14) . . ? C74 C73 C72 119.1(15) . . ? C75 C74 C73 121.6(15) . . ? C74 C75 C76 117.1(14) . . ? C71 C76 C75 125.1(15) . . ? C86 C81 C82 114.4(12) . . ? C86 C81 B1 119.8(13) . . ? C82 C81 B1 125.8(12) . . ? C83 C82 C81 124.8(17) . . ? C82 C83 C84 115.4(19) . . ? C85 C84 C83 124.2(15) . . ? C84 C85 C86 119.6(15) . . ? C85 C86 C81 121.6(15) . . ? C96 C91 C92 114.3(14) . . ? C96 C91 B1 122.0(14) . . ? C92 C91 B1 123.6(13) . . ? C91 C92 C93 123.3(15) . . ? C94 C93 C92 117.9(17) . . ? C93 C94 C95 121.7(18) . . ? C94 C95 C96 118.3(19) . . ? C91 C96 C95 124.1(19) . . ? Cl21 C10 Cl22 107.6(18) . . ? Cl12 C10 Cl11 110.3(19) . . ? Cl31 C10 Cl32 119.9(18) . . ? Cl41 C10 Cl42 91.4(17) . . ? _refine_diff_density_max 3.750 _refine_diff_density_min -1.442 _refine_diff_density_rms 0.151 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_19 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H29 Br2 Mo N0 P3' _chemical_formula_weight 818.24 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 12.630(19) _cell_length_b 14.308(14) _cell_length_c 18.708(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.02(1) _cell_angle_gamma 90.00 _cell_volume 3355.4 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 2.945 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.178 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8359 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5302 _reflns_number_gt 2069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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^)+(0.2000P)^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_number_reflns 5302 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2146 _refine_ls_R_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.3046 _refine_ls_wR_factor_gt 0.2419 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.013 _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 Mo Mo 0.82102(15) 0.89821(11) 0.23573(9) 0.0841(7) Uani 1 d . . . O1 O 0.7277(14) 0.9680(9) 0.2756(6) 0.108(5) Uani 1 d . . . O2 O 0.9183(11) 0.7885(8) 0.1975(7) 0.097(4) Uani 1 d . . . Br2 Br 0.7848(2) 0.95980(15) 0.10512(12) 0.1011(9) Uani 1 d . . . Br3 Br 0.9955(2) 0.99701(14) 0.25207(13) 0.1062(9) Uani 1 d . . . P4 P 0.6795(5) 0.7799(3) 0.2162(3) 0.0844(16) Uani 1 d . . . C3 C 0.7107(19) 0.6757(16) 0.1625(14) 0.123(8) Uani 1 d . . . H3A H 0.7517 0.6319 0.1944 0.148 Uiso 1 calc R . . H3B H 0.6442 0.6454 0.1443 0.148 Uiso 1 calc R . . C2 C 0.7689(19) 0.6946(15) 0.1029(12) 0.110(8) Uani 1 d . . . H2A H 0.7356 0.7464 0.0752 0.133 Uiso 1 calc R . . H2B H 0.7662 0.6402 0.0716 0.133 Uiso 1 calc R . . P1 P 0.9084(5) 0.7234(4) 0.1336(3) 0.0993(19) Uani 1 d . . . C5 C 0.664(2) 0.7206(18) 0.3004(12) 0.130(9) Uani 1 d . . . H5A H 0.6163 0.7562 0.3268 0.156 Uiso 1 calc R . . H5B H 0.6330 0.6594 0.2901 0.156 Uiso 1 calc R . . C6 C 0.7676(17) 0.7104(13) 0.3442(10) 0.089(6) Uani 1 d . . . H6A H 0.8050 0.6585 0.3250 0.106 Uiso 1 calc R . . H6B H 0.7548 0.6934 0.3926 0.106 Uiso 1 calc R . . P7 P 0.8558(5) 0.8114(3) 0.3507(3) 0.0838(16) Uani 1 d . . . C31 C 0.546(2) 0.8102(14) 0.1781(11) 0.093(6) Uani 1 d . . . C32 C 0.473(3) 0.7445(19) 0.1700(14) 0.142(10) Uani 1 d . . . H32 H 0.4876 0.6824 0.1819 0.170 Uiso 1 calc R . . C33 C 0.368(2) 0.776(3) 0.141(2) 0.174(14) Uani 1 d . . . H33 H 0.3119 0.7333 0.1395 0.208 Uiso 1 calc R . . C34 C 0.346(2) 0.858(2) 0.1178(16) 0.137(11) Uani 1 d . . . H34 H 0.2774 0.8725 0.0960 0.165 Uiso 1 calc R . . C35 C 0.425(2) 0.9234(17) 0.1255(14) 0.115(8) Uani 1 d . . . H35 H 0.4100 0.9850 0.1119 0.138 Uiso 1 calc R . . C36 C 0.524(2) 0.898(2) 0.1528(15) 0.135(10) Uani 1 d . . . H36 H 0.5793 0.9411 0.1543 0.162 Uiso 1 calc R . . C41 C 0.8194(17) 0.8783(13) 0.4278(11) 0.082(6) Uani 1 d . . . C42 C 0.7415(19) 0.8506(18) 0.4676(17) 0.119(9) Uani 1 d . . . H42 H 0.7018 0.7966 0.4571 0.143 Uiso 1 calc R . . C43 C 0.726(2) 0.906(2) 0.5226(14) 0.125(9) Uani 1 d . . . H43 H 0.6748 0.8886 0.5514 0.150 Uiso 1 calc R . . C44 C 0.781(3) 0.987(2) 0.5397(14) 0.132(11) Uani 1 d . . . H44 H 0.7673 1.0229 0.5791 0.158 Uiso 1 calc R . . C45 C 0.854(2) 1.0132(19) 0.4979(14) 0.112(8) Uani 1 d . . . H45 H 0.8917 1.0685 0.5076 0.134 Uiso 1 calc R . . C46 C 0.8733(18) 0.9602(14) 0.4424(12) 0.092(6) Uani 1 d . . . H46 H 0.9238 0.9791 0.4132 0.111 Uiso 1 calc R . . C51 C 0.9853(19) 0.7628(12) 0.3828(10) 0.076(5) Uani 1 d . . . C52 C 1.071(2) 0.7805(14) 0.3531(13) 0.104(8) Uani 1 d . . . H52 H 1.0679 0.8216 0.3146 0.125 Uiso 1 calc R . . C53 C 1.161(2) 0.7394(18) 0.3783(14) 0.113(8) Uani 1 d . . . H53 H 1.2220 0.7538 0.3568 0.136 Uiso 1 calc R . . C54 C 1.172(2) 0.6800(18) 0.4315(15) 0.111(8) Uani 1 d . . . H54 H 1.2377 0.6528 0.4457 0.134 Uiso 1 calc R . . C55 C 1.089(3) 0.6577(16) 0.4657(13) 0.114(9) Uani 1 d . . . H55 H 1.0956 0.6131 0.5020 0.137 Uiso 1 calc R . . C56 C 0.994(2) 0.7032(17) 0.4451(13) 0.117(8) Uani 1 d . . . H56 H 0.9369 0.6956 0.4712 0.140 Uiso 1 calc R . . C11 C 0.980(3) 0.622(2) 0.1577(15) 0.142(11) Uani 1 d . . . C12 C 0.955(3) 0.5401(18) 0.126(2) 0.177(15) Uani 1 d . . . H12 H 0.8940 0.5334 0.0934 0.212 Uiso 1 calc R . . C13 C 1.024(4) 0.464(2) 0.143(2) 0.196(18) Uani 1 d . . . H13 H 1.0130 0.4073 0.1194 0.235 Uiso 1 calc R . . C14 C 1.113(4) 0.477(4) 0.198(2) 0.21(2) Uani 1 d . . . H14 H 1.1441 0.4250 0.2215 0.254 Uiso 1 calc R . . C15 C 1.156(4) 0.565(3) 0.217(2) 0.24(2) Uani 1 d . . . H15 H 1.2251 0.5774 0.2374 0.283 Uiso 1 calc R . . C16 C 1.078(3) 0.631(2) 0.2000(13) 0.155(13) Uani 1 d . . . H16 H 1.0922 0.6899 0.2196 0.186 Uiso 1 calc R . . C21 C 0.9609(15) 0.7724(12) 0.0605(11) 0.081(6) Uani 1 d . . . C22 C 1.0225(18) 0.8498(14) 0.0713(14) 0.112(7) Uani 1 d . . . H22 H 1.0366 0.8743 0.1175 0.134 Uiso 1 calc R . . C23 C 1.067(2) 0.8960(15) 0.0116(16) 0.104(8) Uani 1 d . . . H23 H 1.1161 0.9448 0.0193 0.125 Uiso 1 calc R . . C24 C 1.036(2) 0.865(2) -0.050(2) 0.122(10) Uani 1 d . . . H24 H 1.0575 0.8959 -0.0901 0.147 Uiso 1 calc R . . C25 C 0.974(2) 0.791(2) -0.0613(12) 0.111(8) Uani 1 d . . . H25 H 0.9564 0.7701 -0.1084 0.133 Uiso 1 calc R . . C26 C 0.935(2) 0.7446(13) -0.0092(15) 0.109(7) Uani 1 d . . . H26 H 0.8897 0.6938 -0.0201 0.131 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 Mo 0.0881(16) 0.0770(10) 0.0860(12) 0.0007(8) 0.0058(10) -0.0013(9) O1 0.165(15) 0.096(8) 0.060(8) -0.015(6) 0.005(8) -0.024(9) O2 0.104(11) 0.074(7) 0.117(10) -0.015(7) 0.030(9) 0.009(7) Br2 0.109(2) 0.0998(14) 0.0938(16) 0.0071(11) 0.0084(13) -0.0027(13) Br3 0.104(2) 0.0942(14) 0.1179(18) -0.0019(12) 0.0015(15) -0.0152(12) P4 0.081(4) 0.085(3) 0.086(4) 0.008(3) 0.007(3) -0.002(3) C3 0.09(2) 0.119(16) 0.15(2) -0.027(16) 0.006(17) 0.004(14) C2 0.13(2) 0.104(14) 0.110(17) -0.031(13) 0.080(16) -0.045(14) P1 0.107(5) 0.085(3) 0.110(5) -0.009(3) 0.030(4) -0.007(3) C5 0.13(2) 0.16(2) 0.100(16) 0.063(15) -0.012(16) 0.002(17) C6 0.101(18) 0.094(12) 0.071(12) -0.010(10) 0.013(12) -0.010(11) P7 0.080(4) 0.088(3) 0.084(3) 0.006(3) 0.015(3) 0.007(3) C31 0.12(2) 0.067(11) 0.087(14) -0.009(10) 0.002(13) 0.001(13) C32 0.14(3) 0.12(2) 0.15(2) 0.029(17) -0.03(2) 0.002(19) C33 0.09(3) 0.22(4) 0.20(3) -0.08(3) 0.00(2) -0.01(3) C34 0.10(3) 0.13(2) 0.18(3) -0.02(2) -0.010(19) 0.05(2) C35 0.10(2) 0.096(15) 0.15(2) 0.007(15) 0.035(18) 0.025(16) C36 0.053(19) 0.18(3) 0.18(3) 0.00(2) 0.030(17) 0.034(17) C41 0.055(15) 0.090(13) 0.095(14) 0.011(11) -0.018(12) 0.013(10) C42 0.063(17) 0.119(17) 0.18(3) 0.033(19) 0.041(17) -0.007(14) C43 0.14(3) 0.15(2) 0.091(17) -0.018(17) 0.052(17) 0.05(2) C44 0.14(3) 0.18(3) 0.073(17) -0.061(18) -0.011(17) 0.05(2) C45 0.09(2) 0.17(2) 0.077(16) -0.016(17) 0.017(14) 0.042(17) C46 0.091(17) 0.096(13) 0.089(15) 0.022(12) 0.005(13) 0.009(13) C51 0.079(17) 0.074(11) 0.075(13) -0.003(9) 0.006(12) 0.004(11) C52 0.08(2) 0.095(14) 0.124(19) 0.025(13) -0.033(17) -0.019(14) C53 0.10(2) 0.128(18) 0.109(19) -0.004(16) 0.000(16) -0.031(17) C54 0.10(2) 0.117(18) 0.110(19) -0.013(15) -0.033(17) 0.010(16) C55 0.11(2) 0.119(17) 0.110(18) 0.038(14) -0.005(17) -0.028(18) C56 0.065(17) 0.151(19) 0.14(2) 0.046(17) 0.010(14) 0.019(15) C11 0.15(3) 0.18(3) 0.11(2) -0.063(19) 0.044(19) -0.01(2) C12 0.17(3) 0.075(15) 0.29(4) -0.02(2) 0.07(3) -0.006(18) C13 0.26(5) 0.10(2) 0.26(5) 0.05(3) 0.16(4) -0.04(3) C14 0.19(4) 0.25(5) 0.19(4) 0.14(4) 0.00(3) 0.03(4) C15 0.36(7) 0.12(2) 0.25(5) 0.05(3) 0.11(5) 0.05(3) C16 0.25(4) 0.14(2) 0.078(16) 0.023(15) 0.01(2) 0.08(3) C21 0.067(15) 0.075(11) 0.102(16) -0.028(10) 0.021(11) -0.007(10) C22 0.091(18) 0.090(14) 0.15(2) -0.010(15) 0.017(16) 0.004(13) C23 0.11(2) 0.093(14) 0.109(17) 0.016(15) 0.030(17) -0.020(13) C24 0.07(2) 0.14(2) 0.18(3) 0.06(2) 0.06(2) 0.021(16) C25 0.072(18) 0.19(3) 0.076(15) 0.002(17) 0.013(13) 0.010(18) C26 0.13(2) 0.076(12) 0.13(2) -0.033(14) 0.031(18) -0.019(13) _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 O1 1.775(16) . ? Mo O2 2.164(12) . ? Mo P4 2.459(6) . ? Mo P7 2.477(5) . ? Mo Br2 2.587(3) . ? Mo Br3 2.608(3) . ? O2 P1 1.507(14) . ? P4 C31 1.80(2) . ? P4 C5 1.82(2) . ? P4 C3 1.86(2) . ? C3 C2 1.44(3) . ? C2 P1 1.83(2) . ? P1 C21 1.74(2) . ? P1 C11 1.74(4) . ? C5 C6 1.46(3) . ? C6 P7 1.822(19) . ? P7 C51 1.81(2) . ? P7 C41 1.83(2) . ? C31 C32 1.32(3) . ? C31 C36 1.36(3) . ? C32 C33 1.44(4) . ? C33 C34 1.27(4) . ? C34 C35 1.37(3) . ? C35 C36 1.35(3) . ? C41 C42 1.37(3) . ? C41 C46 1.37(3) . ? C42 C43 1.33(3) . ? C43 C44 1.37(4) . ? C44 C45 1.34(4) . ? C45 C46 1.33(3) . ? C51 C52 1.30(3) . ? C51 C56 1.44(3) . ? C52 C53 1.32(3) . ? C53 C54 1.30(3) . ? C54 C55 1.32(3) . ? C55 C56 1.38(3) . ? C11 C12 1.33(4) . ? C11 C16 1.39(4) . ? C12 C13 1.40(5) . ? C13 C14 1.44(5) . ? C14 C15 1.40(6) . ? C15 C16 1.37(4) . ? C21 C22 1.36(3) . ? C21 C26 1.37(3) . ? C22 C23 1.47(3) . ? C23 C24 1.26(3) . ? C24 C25 1.33(3) . ? C25 C26 1.32(3) . ? 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 O1 Mo O2 167.6(5) . . ? O1 Mo P4 86.6(5) . . ? O2 Mo P4 83.3(4) . . ? O1 Mo P7 88.5(4) . . ? O2 Mo P7 82.8(4) . . ? P4 Mo P7 80.23(18) . . ? O1 Mo Br2 99.0(4) . . ? O2 Mo Br2 88.7(4) . . ? P4 Mo Br2 93.14(14) . . ? P7 Mo Br2 169.79(14) . . ? O1 Mo Br3 104.0(4) . . ? O2 Mo Br3 85.8(4) . . ? P4 Mo Br3 168.94(16) . . ? P7 Mo Br3 96.57(15) . . ? Br2 Mo Br3 88.49(9) . . ? P1 O2 Mo 135.4(9) . . ? C31 P4 C5 105.1(11) . . ? C31 P4 C3 103.1(10) . . ? C5 P4 C3 98.3(12) . . ? C31 P4 Mo 121.5(7) . . ? C5 P4 Mo 110.3(9) . . ? C3 P4 Mo 115.7(8) . . ? C2 C3 P4 115.4(17) . . ? C3 C2 P1 111.3(17) . . ? O2 P1 C21 111.8(8) . . ? O2 P1 C11 108.6(11) . . ? C21 P1 C11 108.0(11) . . ? O2 P1 C2 111.8(9) . . ? C21 P1 C2 106.8(10) . . ? C11 P1 C2 109.8(13) . . ? C6 C5 P4 110.4(17) . . ? C5 C6 P7 117.1(15) . . ? C51 P7 C6 103.8(10) . . ? C51 P7 C41 103.9(8) . . ? C6 P7 C41 104.8(10) . . ? C51 P7 Mo 122.6(8) . . ? C6 P7 Mo 107.5(6) . . ? C41 P7 Mo 112.8(6) . . ? C32 C31 C36 121(2) . . ? C32 C31 P4 119.0(18) . . ? C36 C31 P4 120(2) . . ? C31 C32 C33 115(3) . . ? C34 C33 C32 125(4) . . ? C33 C34 C35 118(3) . . ? C36 C35 C34 119(2) . . ? C35 C36 C31 121(3) . . ? C42 C41 C46 121(2) . . ? C42 C41 P7 123(2) . . ? C46 C41 P7 115.9(19) . . ? C43 C42 C41 115(2) . . ? C42 C43 C44 125(3) . . ? C45 C44 C43 118(2) . . ? C46 C45 C44 120(3) . . ? C45 C46 C41 121(2) . . ? C52 C51 C56 118(2) . . ? C52 C51 P7 123.1(18) . . ? C56 C51 P7 118.5(19) . . ? C51 C52 C53 119(2) . . ? C54 C53 C52 124(3) . . ? C53 C54 C55 121(3) . . ? C54 C55 C56 117(2) . . ? C55 C56 C51 119(2) . . ? C12 C11 C16 119(3) . . ? C12 C11 P1 122(3) . . ? C16 C11 P1 118(2) . . ? C11 C12 C13 118(4) . . ? C12 C13 C14 118(4) . . ? C15 C14 C13 123(4) . . ? C16 C15 C14 108(5) . . ? C15 C16 C11 129(4) . . ? C22 C21 C26 117(2) . . ? C22 C21 P1 118.8(17) . . ? C26 C21 P1 124.2(16) . . ? C21 C22 C23 122(2) . . ? C24 C23 C22 116(2) . . ? C23 C24 C25 122(3) . . ? C26 C25 C24 124(2) . . ? C25 C26 C21 119(2) . . ? _refine_diff_density_max 2.476 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.213 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ;