data_01016a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H70 Cl12 I2 O6 W' _chemical_formula_weight 1966.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 '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 Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 26.574(4) _cell_length_b 10.2177(15) _cell_length_c 28.363(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.702(2) _cell_angle_gamma 90.00 _cell_volume 7693(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max .04 _exptl_crystal_size_mid .04 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 2.773 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6895 _exptl_absorpt_correction_T_max 0.9966 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11000 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.1005 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 20.00 _reflns_number_total 3576 _reflns_number_gt 2420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^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 0.00056(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3576 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2144 _refine_ls_wR_factor_gt 0.1970 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2642(6) -0.2705(17) 0.0195(6) 0.034(3) Uiso 1 1 d . . . C2 C 0.2779(7) -0.3905(19) 0.0442(7) 0.053(4) Uiso 1 1 d . . . C3 C 0.2617(7) -0.5107(18) 0.0177(6) 0.056(4) Uiso 1 1 d . . . C4 C 0.3038(6) 0.1616(15) 0.0820(6) 0.031(4) Uiso 1 1 d . . . C5 C 0.2778(5) 0.1851(14) 0.1209(5) 0.019(4) Uiso 1 1 d . . . C6 C 0.3043(5) 0.2399(14) 0.1600(5) 0.024(4) Uiso 1 1 d . . . H6 H 0.2866 0.2608 0.1873 0.028 Uiso 1 1 calc R . . C7 C 0.3560(6) 0.2646(15) 0.1597(5) 0.028(4) Uiso 1 1 d . . . C8 C 0.3805(6) 0.2342(14) 0.1193(5) 0.027(4) Uiso 1 1 d . . . H8 H 0.4157 0.2494 0.1190 0.032 Uiso 1 1 calc R . . C9 C 0.3555(6) 0.1813(15) 0.0782(6) 0.034(3) Uiso 1 1 d . . . C10 C 0.3811(6) 0.1396(14) 0.0359(5) 0.023(4) Uiso 1 1 d . . . H10A H 0.3767 0.0438 0.0325 0.027 Uiso 1 1 calc R . . H10B H 0.4176 0.1564 0.0414 0.027 Uiso 1 1 calc R . . C11 C 0.3640(7) 0.2041(19) -0.0113(7) 0.053(4) Uiso 1 1 d . . . C12 C 0.3814(7) 0.3280(18) -0.0212(7) 0.051(4) Uiso 1 1 d . . . H12 H 0.4044 0.3695 0.0008 0.061 Uiso 1 1 calc R . . C13 C 0.3662(6) 0.3940(14) -0.0628(5) 0.026(4) Uiso 1 1 d . . . C14 C 0.3326(7) 0.3316(19) -0.0934(7) 0.056(4) Uiso 1 1 d . . . H14 H 0.3223 0.3758 -0.1218 0.067 Uiso 1 1 calc R . . C15 C 0.3125(6) 0.2075(15) -0.0857(5) 0.028(4) Uiso 1 1 d . . . C16 C 0.3299(6) 0.1451(16) -0.0436(6) 0.031(4) Uiso 1 1 d . . . C17 C 0.2222(6) 0.1443(15) 0.1226(5) 0.028(4) Uiso 1 1 d . . . H17A H 0.2199 0.0482 0.1189 0.034 Uiso 1 1 calc R . . H17B H 0.2101 0.1663 0.1542 0.034 Uiso 1 1 calc R . . C18 C 0.3865(6) 0.3188(15) 0.2027(5) 0.027(4) Uiso 1 1 d . . . C19 C 0.4261(10) 0.412(3) 0.1908(9) 0.106(9) Uiso 1 1 d . . . H19A H 0.4101 0.4925 0.1776 0.127 Uiso 1 1 calc R . . H19B H 0.4465 0.3732 0.1660 0.127 Uiso 1 1 calc R . . C20 C 0.4117(9) 0.207(2) 0.2290(8) 0.092(8) Uiso 1 1 d . . . H20A H 0.4355 0.1635 0.2082 0.111 Uiso 1 1 calc R . . H20B H 0.3858 0.1414 0.2368 0.111 Uiso 1 1 calc R . . C21 C 0.3525(9) 0.386(2) 0.2375(8) 0.087(8) Uiso 1 1 d . . . H21A H 0.3279 0.3225 0.2491 0.105 Uiso 1 1 calc R . . H21B H 0.3336 0.4581 0.2214 0.105 Uiso 1 1 calc R . . C22 C 0.3854(8) 0.443(2) 0.2805(8) 0.072(7) Uiso 1 1 d . . . H22 H 0.3634 0.4924 0.3018 0.086 Uiso 1 1 calc R . . C23 C 0.4248(9) 0.532(2) 0.2627(9) 0.088(8) Uiso 1 1 d . . . H23A H 0.4411 0.5802 0.2894 0.106 Uiso 1 1 calc R . . H23B H 0.4090 0.5959 0.2405 0.106 Uiso 1 1 calc R . . C24 C 0.4646(7) 0.4528(18) 0.2374(7) 0.051(4) Uiso 1 1 d . . . H24 H 0.4939 0.5074 0.2284 0.061 Uiso 1 1 calc R . . C25 C 0.4793(9) 0.333(2) 0.2574(8) 0.080(7) Uiso 1 1 d . . . H25 H 0.5133 0.3042 0.2564 0.096 Uiso 1 1 calc R . . C26 C 0.4430(9) 0.253(2) 0.2792(8) 0.087(8) Uiso 1 1 d . . . H26 H 0.4583 0.1782 0.2974 0.105 Uiso 1 1 calc R . . C27 C 0.4053(9) 0.325(2) 0.3050(9) 0.094(8) Uiso 1 1 d . . . H27 H 0.3946 0.2976 0.3349 0.112 Uiso 1 1 calc R . . C28 C 0.3887(6) 0.5307(14) -0.0741(5) 0.030(4) Uiso 1 1 d . . . C29 C 0.4093(10) 0.533(2) -0.1221(10) 0.104(9) Uiso 1 1 d . . . H29A H 0.3819 0.5114 -0.1457 0.125 Uiso 1 1 calc R . . H29B H 0.4355 0.4644 -0.1239 0.125 Uiso 1 1 calc R . . C30 C 0.3457(10) 0.630(3) -0.0750(11) 0.118(10) Uiso 1 1 d . . . H30A H 0.3299 0.6298 -0.0440 0.141 Uiso 1 1 calc R . . H30B H 0.3197 0.6042 -0.0994 0.141 Uiso 1 1 calc R . . C31 C 0.4267(10) 0.575(3) -0.0391(9) 0.100(8) Uiso 1 1 d . . . H31A H 0.4546 0.5104 -0.0378 0.120 Uiso 1 1 calc R . . H31B H 0.4116 0.5742 -0.0078 0.120 Uiso 1 1 calc R . . C32 C 0.4510(8) 0.723(2) -0.0479(7) 0.063(6) Uiso 1 1 d . . . H32 H 0.4772 0.7516 -0.0235 0.076 Uiso 1 1 calc R . . C33 C 0.4028(8) 0.800(2) -0.0481(8) 0.074(7) Uiso 1 1 d . . . H33 H 0.3962 0.8579 -0.0231 0.089 Uiso 1 1 calc R . . C34 C 0.4698(10) 0.695(2) -0.0938(9) 0.092(8) Uiso 1 1 d . . . H34 H 0.5050 0.6864 -0.0973 0.111 Uiso 1 1 calc R . . C35 C 0.3669(9) 0.783(2) -0.0868(9) 0.088(8) Uiso 1 1 d . . . H35 H 0.3398 0.8512 -0.0881 0.106 Uiso 1 1 calc R . . C36 C 0.4343(9) 0.678(2) -0.1357(9) 0.080(7) Uiso 1 1 d . . . H36 H 0.4503 0.6816 -0.1669 0.096 Uiso 1 1 calc R . . C37 C 0.3863(8) 0.751(2) -0.1334(8) 0.064(6) Uiso 1 1 d . . . H37 H 0.3682 0.7775 -0.1616 0.077 Uiso 1 1 calc R . . C38 C 0.1999(10) 0.566(3) 0.2778(10) 0.103(9) Uiso 1 1 d . . . H38 H 0.1899 0.4948 0.2996 0.123 Uiso 1 1 calc R . . C39 C 0.0415(9) 0.675(2) 0.4142(9) 0.085(7) Uiso 1 1 d . . . H39 H 0.0673 0.6780 0.4410 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.0354(4) 0.8261(8) 0.3921(5) 0.186(5) Uani 1 1 d . . . Cl2 Cl 0.0626(4) 0.5662(9) 0.3733(3) 0.148(4) Uani 1 1 d . . . Cl3 Cl 0.2508(5) 0.6441(9) 0.3041(4) 0.188(5) Uani 1 1 d . . . Cl4 Cl 0.1469(4) 0.6593(9) 0.2651(3) 0.148(4) Uani 1 1 d . . . Cl5 Cl 0.2184(3) 0.4920(8) 0.2267(4) 0.133(3) Uani 1 1 d . . . Cl6 Cl -0.0116(4) 0.6201(10) 0.4353(3) 0.168(4) Uani 1 1 d . . . I I 0.31972(10) -0.3885(3) 0.10543(11) 0.1950(17) Uani 1 1 d . . . O1 O 0.2789(4) 0.1113(10) 0.0440(4) 0.034(3) Uani 1 1 d . . . O2 O 0.3103(4) 0.0206(9) -0.0330(4) 0.028(3) Uani 1 1 d . . . O3 O 0.2752(4) -0.1503(11) 0.0377(4) 0.038(3) Uani 1 1 d . . . W W 0.2500 -0.00390(10) 0.0000 0.0269(5) Uani 1 2 d S . . 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 Cl1 0.168(9) 0.067(5) 0.321(15) 0.042(7) 0.003(9) 0.011(5) Cl2 0.197(9) 0.156(7) 0.089(6) -0.026(5) -0.017(6) 0.109(7) Cl3 0.245(12) 0.118(7) 0.188(10) 0.052(7) -0.122(9) -0.045(7) Cl4 0.186(9) 0.132(7) 0.126(7) 0.029(6) 0.014(6) 0.090(6) Cl5 0.090(5) 0.116(6) 0.193(9) 0.005(6) 0.021(5) 0.018(5) Cl6 0.212(10) 0.185(9) 0.111(7) -0.044(7) 0.047(6) -0.109(8) I 0.146(2) 0.220(3) 0.221(3) 0.174(3) 0.014(2) 0.074(2) O1 0.048(8) 0.026(6) 0.027(7) -0.006(5) 0.008(6) -0.011(6) O2 0.022(6) 0.023(6) 0.040(7) 0.003(5) 0.005(5) 0.000(5) O3 0.029(7) 0.045(8) 0.040(8) 0.007(6) 0.000(6) 0.012(6) W 0.0288(7) 0.0186(6) 0.0331(7) 0.000 -0.0010(4) 0.000 _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 C1 C1 1.31(3) 2 ? C1 O3 1.360(18) . ? C1 C2 1.45(2) . ? C2 C3 1.49(2) . ? C2 I 2.015(19) . ? C3 C3 1.16(3) 2 ? C4 O1 1.342(18) . ? C4 C5 1.35(2) . ? C4 C9 1.40(2) . ? C5 C6 1.399(19) . ? C5 C17 1.54(2) . ? C6 C7 1.40(2) . ? C7 C8 1.38(2) . ? C7 C18 1.54(2) . ? C8 C9 1.42(2) . ? C9 C10 1.47(2) . ? C10 C11 1.54(2) . ? C11 C12 1.38(2) . ? C11 C16 1.40(2) . ? C12 C13 1.40(2) . ? C13 C14 1.38(2) . ? C13 C28 1.56(2) . ? C14 C15 1.40(2) . ? C15 C16 1.41(2) . ? C15 C17 1.51(2) 2 ? C16 O2 1.412(18) . ? C17 C15 1.51(2) 2 ? C18 C19 1.47(3) . ? C18 C20 1.51(3) . ? C18 C21 1.53(3) . ? C19 C24 1.69(3) . ? C20 C26 1.68(3) . ? C21 C22 1.57(3) . ? C22 C27 1.48(3) . ? C22 C23 1.49(3) . ? C23 C24 1.53(3) . ? C24 C25 1.40(3) . ? C25 C26 1.42(3) . ? C26 C27 1.46(3) . ? C28 C31 1.45(3) . ? C28 C29 1.49(3) . ? C28 C30 1.53(3) . ? C29 C36 1.68(3) . ? C30 C35 1.71(3) . ? C31 C32 1.67(3) . ? C32 C34 1.45(3) . ? C32 C33 1.50(3) . ? C33 C35 1.43(3) . ? C34 C36 1.49(3) . ? C35 C37 1.48(3) . ? C36 C37 1.48(3) . ? C38 Cl3 1.71(3) . ? C38 Cl4 1.72(3) . ? C38 Cl5 1.73(3) . ? C39 Cl6 1.65(2) . ? C39 Cl1 1.68(2) . ? C39 Cl2 1.72(2) . ? O1 W 1.855(10) . ? O2 W 1.910(10) . ? O3 W 1.940(10) . ? W O1 1.855(10) 2 ? W O2 1.910(10) 2 ? W O3 1.940(10) 2 ? 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 C1 O3 115.2(8) 2 . ? C1 C1 C2 122.1(10) 2 . ? O3 C1 C2 122.3(14) . . ? C1 C2 C3 113.0(16) . . ? C1 C2 I 121.6(13) . . ? C3 C2 I 125.2(13) . . ? C3 C3 C2 124.7(10) 2 . ? O1 C4 C5 118.2(15) . . ? O1 C4 C9 116.2(15) . . ? C5 C4 C9 125.5(15) . . ? C4 C5 C6 117.4(14) . . ? C4 C5 C17 120.4(13) . . ? C6 C5 C17 122.1(14) . . ? C5 C6 C7 121.7(15) . . ? C8 C7 C6 117.8(14) . . ? C8 C7 C18 119.3(14) . . ? C6 C7 C18 122.9(14) . . ? C7 C8 C9 123.2(15) . . ? C4 C9 C8 114.3(15) . . ? C4 C9 C10 121.1(14) . . ? C8 C9 C10 124.4(15) . . ? C9 C10 C11 117.1(13) . . ? C12 C11 C16 118.4(17) . . ? C12 C11 C10 118.7(16) . . ? C16 C11 C10 122.8(16) . . ? C11 C12 C13 121.7(18) . . ? C14 C13 C12 117.6(16) . . ? C14 C13 C28 121.9(14) . . ? C12 C13 C28 120.5(14) . . ? C13 C14 C15 124.2(17) . . ? C14 C15 C16 115.6(15) . . ? C14 C15 C17 120.2(15) . 2 ? C16 C15 C17 124.0(14) . 2 ? C11 C16 C15 122.4(15) . . ? C11 C16 O2 118.9(14) . . ? C15 C16 O2 118.6(13) . . ? C15 C17 C5 114.8(13) 2 . ? C19 C18 C20 107.5(18) . . ? C19 C18 C21 107.9(17) . . ? C20 C18 C21 106.5(16) . . ? C19 C18 C7 114.0(15) . . ? C20 C18 C7 108.9(14) . . ? C21 C18 C7 111.7(14) . . ? C18 C19 C24 113.2(19) . . ? C18 C20 C26 113.2(18) . . ? C18 C21 C22 109.9(18) . . ? C27 C22 C23 114(2) . . ? C27 C22 C21 103.8(19) . . ? C23 C22 C21 109.5(19) . . ? C22 C23 C24 110(2) . . ? C25 C24 C23 117(2) . . ? C25 C24 C19 104.4(17) . . ? C23 C24 C19 95.1(17) . . ? C24 C25 C26 120(2) . . ? C25 C26 C27 115(2) . . ? C25 C26 C20 96.5(19) . . ? C27 C26 C20 103.9(19) . . ? C26 C27 C22 114(2) . . ? C31 C28 C29 110.3(19) . . ? C31 C28 C30 107.5(18) . . ? C29 C28 C30 106.4(18) . . ? C31 C28 C13 113.3(15) . . ? C29 C28 C13 111.2(14) . . ? C30 C28 C13 107.8(15) . . ? C28 C29 C36 112.8(19) . . ? C28 C30 C35 111(2) . . ? C28 C31 C32 116.0(19) . . ? C34 C32 C33 116(2) . . ? C34 C32 C31 96.0(19) . . ? C33 C32 C31 97.9(17) . . ? C35 C33 C32 119(2) . . ? C32 C34 C36 120(2) . . ? C33 C35 C37 118(2) . . ? C33 C35 C30 100(2) . . ? C37 C35 C30 96.1(19) . . ? C37 C36 C34 115(2) . . ? C37 C36 C29 94.9(18) . . ? C34 C36 C29 99.2(19) . . ? C35 C37 C36 119(2) . . ? Cl3 C38 Cl4 117.0(17) . . ? Cl3 C38 Cl5 108.6(16) . . ? Cl4 C38 Cl5 109.3(15) . . ? Cl6 C39 Cl1 112.2(15) . . ? Cl6 C39 Cl2 109.9(14) . . ? Cl1 C39 Cl2 111.9(15) . . ? C4 O1 W 163.1(10) . . ? C16 O2 W 123.3(9) . . ? C1 O3 W 115.1(9) . . ? O1 W O1 101.2(6) . 2 ? O1 W O2 85.2(4) . . ? O1 W O2 85.2(4) 2 . ? O1 W O2 85.2(4) . 2 ? O1 W O2 85.2(4) 2 2 ? O2 W O2 164.9(6) . 2 ? O1 W O3 168.9(5) . 2 ? O1 W O3 89.8(5) 2 2 ? O2 W O3 96.1(4) . 2 ? O2 W O3 95.5(4) 2 2 ? O1 W O3 89.8(5) . . ? O1 W O3 168.9(5) 2 . ? O2 W O3 95.5(4) . . ? O2 W O3 96.1(4) 2 . ? O3 W O3 79.1(7) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.751 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.166