# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2073 data_wtwong014-WHL130 #compound 1 #------------------------------------------------------------------------------ _audit_creation_date 'Fri May 24 15:49:31 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 13.289(1) _cell_length_b 21.226(2) _cell_length_c 18.002(2) _cell_angle_alpha 90 _cell_angle_beta 101.50(2) _cell_angle_gamma 90 _cell_volume 4975.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.180 _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_meas ? _chemical_formula_weight 1204.12 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H42 Cl2 N2 O2 P4 Os S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2400.00 _exptl_absorpt_coefficient_mu 3.006 _exptl_absorpt_correction_type 'inter-image scaling' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 31452 _reflns_number_total 9527 _reflns_number_observed 2816 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.05 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.63 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 4 -1.216 7.603 'International Tables' O 0 8 0.011 0.006 'International Tables' P 0 16 0.102 0.094 'International Tables' S 0 16 0.125 0.123 'International Tables' N 0 8 0.006 0.003 'International Tables' C 0 196 0.003 0.002 'International Tables' H 0 168 0.000 0.000 'International Tables' Cl 0 8 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Os(1) 0.12519(2) 0.00222(1) 0.25454(2) 0.0261(1) Uij ? ? Cl(1) 0.2673(3) 0.2024(2) 0.1052(2) 0.162(2) Uij ? ? Cl(2) 0.2572(2) 0.0871(2) 0.0211(2) 0.112(1) Uij ? ? S(1) 0.3119(2) 0.01465(10) 0.2875(1) 0.0382(7) Uij ? ? S(2) 0.1114(2) -0.11022(10) 0.2213(1) 0.0381(7) Uij ? ? S(3) 0.1388(1) 0.11759(10) 0.2745(1) 0.0349(7) Uij ? ? S(4) -0.0626(2) -0.01107(9) 0.2207(1) 0.0388(8) Uij ? ? P(1) 0.3784(2) -0.07236(10) 0.2966(1) 0.0339(8) Uij ? ? P(2) 0.2172(2) -0.16059(9) 0.2947(1) 0.0293(7) Uij ? ? P(3) 0.0117(2) 0.14466(10) 0.3132(1) 0.0308(7) Uij ? ? P(4) -0.1193(2) 0.0769(1) 0.1966(1) 0.0304(7) Uij ? ? O(1) 0.1295(4) 0.0152(2) 0.1595(3) 0.035(1) Uij ? ? O(2) 0.1229(4) -0.0118(2) 0.3490(3) 0.039(2) Uij ? ? N(1) 0.3188(4) -0.1250(3) 0.3335(3) 0.027(2) Uij ? ? N(2) -0.0979(4) 0.1267(3) 0.2631(3) 0.030(2) Uij ? ? C(1) 0.4997(6) -0.0593(3) 0.3604(4) 0.037(2) Uij ? ? C(2) 0.5784(7) -0.0299(4) 0.3346(5) 0.058(3) Uij ? ? C(3) 0.6701(8) -0.0145(5) 0.3884(7) 0.081(4) Uij ? ? C(4) 0.6739(8) -0.0274(5) 0.4622(6) 0.080(3) Uij ? ? C(5) 0.5992(8) -0.0575(4) 0.4877(6) 0.076(3) Uij ? ? C(6) 0.5077(7) -0.0730(4) 0.4351(5) 0.054(3) Uij ? ? C(7) 0.4052(6) -0.0960(3) 0.2068(4) 0.033(2) Uij ? ? C(8) 0.3491(6) -0.0737(4) 0.1389(5) 0.040(2) Uij ? ? C(9) 0.3661(7) -0.0968(4) 0.0710(5) 0.058(3) Uij ? ? C(10) 0.4397(7) -0.1430(4) 0.0703(5) 0.064(3) Uij ? ? C(11) 0.4967(7) -0.1651(4) 0.1362(5) 0.059(3) Uij ? ? C(12) 0.4804(6) -0.1418(4) 0.2057(5) 0.051(3) Uij ? ? C(13) 0.2441(5) -0.2280(3) 0.2407(4) 0.029(2) Uij ? ? C(14) 0.2447(6) -0.2236(4) 0.1648(4) 0.038(2) Uij ? ? C(15) 0.2766(6) -0.2755(4) 0.1259(5) 0.052(3) Uij ? ? C(16) 0.3070(7) -0.3295(4) 0.1641(5) 0.059(3) Uij ? ? C(17) 0.3036(7) -0.3357(4) 0.2388(6) 0.070(3) Uij ? ? C(18) 0.2721(6) -0.2841(4) 0.2775(5) 0.053(3) Uij ? ? C(19) 0.1602(6) -0.1944(3) 0.3680(4) 0.032(2) Uij ? ? C(20) 0.2129(6) -0.1966(4) 0.4427(5) 0.052(3) Uij ? ? C(21) 0.1681(7) -0.2278(4) 0.4962(5) 0.067(3) Uij ? ? C(22) 0.0741(7) -0.2553(4) 0.4758(5) 0.063(3) Uij ? ? C(23) 0.0218(7) -0.2540(4) 0.4024(5) 0.059(3) Uij ? ? C(24) 0.0657(6) -0.2225(4) 0.3488(5) 0.052(3) Uij ? ? C(25) 0.0172(6) 0.2287(3) 0.3198(4) 0.030(2) Uij ? ? C(26) -0.0733(6) 0.2618(4) 0.3110(5) 0.043(2) Uij ? ? C(27) -0.0733(7) 0.3264(4) 0.3232(5) 0.060(3) Uij ? ? C(28) 0.0158(7) 0.3585(4) 0.3429(5) 0.061(3) Uij ? ? C(29) 0.1089(7) 0.3279(5) 0.3510(5) 0.070(3) Uij ? ? C(30) 0.1082(7) 0.2616(4) 0.3383(5) 0.061(3) Uij ? ? C(31) 0.0191(6) 0.1181(3) 0.4078(4) 0.030(2) Uij ? ? C(32) -0.0639(6) 0.0896(4) 0.4300(5) 0.050(3) Uij ? ? C(33) -0.0584(7) 0.0735(4) 0.5063(6) 0.062(3) Uij ? ? C(34) 0.0276(7) 0.0864(4) 0.5580(5) 0.054(3) Uij ? ? C(35) 0.1091(7) 0.1147(4) 0.5388(5) 0.056(3) Uij ? ? C(36) 0.1075(6) 0.1309(4) 0.4626(5) 0.051(3) Uij ? ? C(37) -0.0818(5) 0.1064(3) 0.1131(4) 0.028(2) Uij ? ? C(38) -0.0776(6) 0.0679(4) 0.0509(5) 0.043(2) Uij ? ? C(39) -0.0532(7) 0.0928(4) -0.0145(5) 0.055(3) Uij ? ? C(40) -0.0336(6) 0.1542(5) -0.0193(5) 0.056(3) Uij ? ? C(41) -0.0376(7) 0.1939(4) 0.0398(5) 0.062(3) Uij ? ? C(42) -0.0617(6) 0.1700(4) 0.1068(5) 0.048(3) Uij ? ? C(43) -0.2568(6) 0.0687(4) 0.1703(4) 0.034(2) Uij ? ? C(44) -0.3165(7) 0.1195(4) 0.1774(5) 0.063(3) Uij ? ? C(45) -0.4268(8) 0.1138(5) 0.1540(6) 0.081(3) Uij ? ? C(46) -0.4672(8) 0.0604(5) 0.1249(6) 0.075(3) Uij ? ? C(47) -0.4088(8) 0.0098(5) 0.1170(6) 0.074(3) Uij ? ? C(48) -0.3007(7) 0.0137(4) 0.1404(5) 0.055(3) Uij ? ? C(49) 0.2302(8) 0.1256(5) 0.1002(6) 0.084(3) Uij ? ? H(1) 0.5721 -0.0200 0.2822 0.0685 Uij ? ? H(2) 0.7268 0.0045 0.3723 0.0974 Uij ? ? H(3) 0.7329 -0.0143 0.4979 0.0962 Uij ? ? H(4) 0.6070 -0.0683 0.5398 0.0907 Uij ? ? H(5) 0.4520 -0.0928 0.4521 0.0639 Uij ? ? H(6) 0.2983 -0.0422 0.1391 0.0481 Uij ? ? H(7) 0.3277 -0.0810 0.0246 0.0688 Uij ? ? H(8) 0.4503 -0.1593 0.0233 0.0763 Uij ? ? H(9) 0.5474 -0.1967 0.1353 0.0704 Uij ? ? H(10) 0.5208 -0.1570 0.2518 0.0608 Uij ? ? H(11) 0.2235 -0.1855 0.1383 0.0456 Uij ? ? H(12) 0.2765 -0.2726 0.0732 0.0623 Uij ? ? H(13) 0.3315 -0.3636 0.1385 0.0709 Uij ? ? H(14) 0.3211 -0.3745 0.2644 0.0833 Uij ? ? H(15) 0.2708 -0.2878 0.3300 0.0629 Uij ? ? H(16) 0.2782 -0.1769 0.4571 0.0626 Uij ? ? H(17) 0.2035 -0.2299 0.5476 0.0794 Uij ? ? H(18) 0.0444 -0.2757 0.5131 0.0759 Uij ? ? H(19) -0.0429 -0.2746 0.3879 0.0703 Uij ? ? H(20) 0.0287 -0.2199 0.2978 0.0626 Uij ? ? H(21) -0.1369 0.2401 0.2964 0.0517 Uij ? ? H(22) -0.1368 0.3483 0.3177 0.0720 Uij ? ? H(23) 0.0143 0.4027 0.3512 0.0724 Uij ? ? H(24) 0.1717 0.3503 0.3645 0.0841 Uij ? ? H(25) 0.1716 0.2396 0.3429 0.0724 Uij ? ? H(26) -0.1246 0.0809 0.3935 0.0593 Uij ? ? H(27) -0.1150 0.0534 0.5215 0.0744 Uij ? ? H(28) 0.0303 0.0750 0.6094 0.0644 Uij ? ? H(29) 0.1680 0.1238 0.5767 0.0678 Uij ? ? H(30) 0.1657 0.1503 0.4486 0.0609 Uij ? ? H(31) -0.0917 0.0241 0.0534 0.0516 Uij ? ? H(32) -0.0505 0.0660 -0.0564 0.0650 Uij ? ? H(33) -0.0168 0.1705 -0.0645 0.0663 Uij ? ? H(34) -0.0236 0.2376 0.0357 0.0740 Uij ? ? H(35) -0.0642 0.1975 0.1480 0.0576 Uij ? ? H(36) -0.2864 0.1581 0.1979 0.0749 Uij ? ? H(37) -0.4700 0.1488 0.1588 0.0958 Uij ? ? H(38) -0.5398 0.0573 0.1091 0.0891 Uij ? ? H(39) -0.4400 -0.0282 0.0960 0.0885 Uij ? ? H(40) -0.2590 -0.0219 0.1355 0.0654 Uij ? ? H(41) 0.2650 0.1046 0.1444 0.0993 Uij ? ? H(42) 0.1582 0.1240 0.0979 0.0993 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0273(3) 0.0244(3) 0.0257(3) 0.0018(2) 0.0033(2) 0.0024(2) Cl(1) 0.232(5) 0.117(3) 0.127(3) -0.103(3) 0.013(3) 0.003(2) Cl(2) 0.107(2) 0.155(3) 0.073(2) 0.031(2) 0.014(2) 0.007(2) S(1) 0.028(1) 0.029(1) 0.053(2) -0.001(1) -0.001(1) -0.004(1) S(2) 0.042(1) 0.023(1) 0.042(2) 0.003(1) -0.010(1) -0.001(1) S(3) 0.033(1) 0.028(1) 0.046(2) 0.001(1) 0.012(1) -0.003(1) S(4) 0.027(1) 0.030(1) 0.056(2) -0.002(1) 0.000(1) 0.007(1) P(1) 0.028(1) 0.031(1) 0.039(2) 0.001(1) -0.001(1) -0.004(1) P(2) 0.031(1) 0.023(1) 0.031(1) 0.003(1) 0.000(1) 0.001(1) P(3) 0.031(1) 0.028(1) 0.033(2) 0.003(1) 0.004(1) -0.002(1) P(4) 0.026(1) 0.032(1) 0.031(2) 0.003(1) 0.001(1) -0.001(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2816 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0291 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0363 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.155 _refine_ls_shift/esd_max 0.0120 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.59 _refine_diff_density_max 0.52 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) S(1) 2.448(2) ? ? yes Os(1) S(2) 2.458(2) ? ? yes Os(1) S(3) 2.477(2) ? ? yes Os(1) S(4) 2.465(2) ? ? yes Os(1) O(1) 1.745(5) ? ? yes Os(1) O(2) 1.732(5) ? ? yes Cl(1) C(49) 1.70(1) ? ? yes Cl(2) C(49) 1.74(1) ? ? yes S(1) P(1) 2.040(3) ? ? yes S(2) P(2) 2.031(3) ? ? yes S(3) P(3) 2.034(3) ? ? yes S(4) P(4) 2.029(3) ? ? yes P(1) N(1) 1.589(6) ? ? yes P(1) C(1) 1.804(7) ? ? yes P(1) C(7) 1.795(8) ? ? yes P(2) N(1) 1.583(6) ? ? yes P(2) C(13) 1.805(8) ? ? yes P(2) C(19) 1.797(9) ? ? yes P(3) N(2) 1.599(6) ? ? yes P(3) C(25) 1.789(8) ? ? yes P(3) C(31) 1.777(8) ? ? yes P(4) N(2) 1.580(6) ? ? yes P(4) C(37) 1.789(8) ? ? yes P(4) C(43) 1.802(8) ? ? yes C(1) C(2) 1.38(1) ? ? yes C(1) C(6) 1.36(1) ? ? yes C(2) C(3) 1.44(1) ? ? yes C(3) C(4) 1.35(2) ? ? yes C(4) C(5) 1.34(2) ? ? yes C(5) C(6) 1.42(1) ? ? yes C(7) C(8) 1.38(1) ? ? yes C(7) C(12) 1.40(1) ? ? yes C(8) C(9) 1.38(1) ? ? yes C(9) C(10) 1.39(1) ? ? yes C(10) C(11) 1.36(1) ? ? yes C(11) C(12) 1.40(1) ? ? yes C(13) C(14) 1.37(1) ? ? yes C(13) C(18) 1.38(1) ? ? yes C(14) C(15) 1.41(1) ? ? yes C(15) C(16) 1.36(1) ? ? yes C(16) C(17) 1.36(1) ? ? yes C(17) C(18) 1.41(1) ? ? yes C(19) C(20) 1.39(1) ? ? yes C(19) C(24) 1.37(1) ? ? yes C(20) C(21) 1.40(1) ? ? yes C(21) C(22) 1.36(1) ? ? yes C(22) C(23) 1.36(1) ? ? yes C(23) C(24) 1.39(1) ? ? yes C(25) C(26) 1.37(1) ? ? yes C(25) C(30) 1.38(1) ? ? yes C(26) C(27) 1.39(1) ? ? yes C(27) C(28) 1.35(1) ? ? yes C(28) C(29) 1.38(1) ? ? yes C(29) C(30) 1.42(1) ? ? yes C(31) C(32) 1.39(1) ? ? yes C(31) C(36) 1.40(1) ? ? yes C(32) C(33) 1.40(1) ? ? yes C(33) C(34) 1.35(1) ? ? yes C(34) C(35) 1.34(1) ? ? yes C(35) C(36) 1.41(1) ? ? yes C(37) C(38) 1.40(1) ? ? yes C(37) C(42) 1.38(1) ? ? yes C(38) C(39) 1.39(1) ? ? yes C(39) C(40) 1.34(1) ? ? yes C(40) C(41) 1.37(1) ? ? yes C(41) C(42) 1.40(1) ? ? yes C(43) C(44) 1.36(1) ? ? yes C(43) C(48) 1.37(1) ? ? yes C(44) C(45) 1.45(1) ? ? yes C(45) C(46) 1.32(1) ? ? yes C(46) C(47) 1.35(1) ? ? yes C(47) C(48) 1.42(1) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Os(1) S(2) 100.75(7) ? ? ? yes S(1) Os(1) S(3) 79.46(7) ? ? ? yes S(1) Os(1) S(4) 179.54(7) ? ? ? yes S(1) Os(1) O(1) 89.5(2) ? ? ? yes S(1) Os(1) O(2) 89.8(2) ? ? ? yes S(2) Os(1) S(3) 174.32(7) ? ? ? yes S(2) Os(1) S(4) 78.82(7) ? ? ? yes S(2) Os(1) O(1) 86.0(2) ? ? ? yes S(2) Os(1) O(2) 93.3(2) ? ? ? yes S(3) Os(1) S(4) 100.95(7) ? ? ? yes S(3) Os(1) O(1) 88.3(2) ? ? ? yes S(3) Os(1) O(2) 92.4(2) ? ? ? yes S(4) Os(1) O(1) 90.3(2) ? ? ? yes S(4) Os(1) O(2) 90.4(2) ? ? ? yes O(1) Os(1) O(2) 178.9(2) ? ? ? yes Os(1) S(1) P(1) 108.9(1) ? ? ? yes Os(1) S(2) P(2) 110.2(1) ? ? ? yes Os(1) S(3) P(3) 106.7(1) ? ? ? yes Os(1) S(4) P(4) 105.2(1) ? ? ? yes S(1) P(1) N(1) 115.2(2) ? ? ? yes S(1) P(1) C(1) 103.3(3) ? ? ? yes S(1) P(1) C(7) 110.0(3) ? ? ? yes N(1) P(1) C(1) 107.4(3) ? ? ? yes N(1) P(1) C(7) 112.6(3) ? ? ? yes C(1) P(1) C(7) 107.7(4) ? ? ? yes S(2) P(2) N(1) 117.0(2) ? ? ? yes S(2) P(2) C(13) 104.6(2) ? ? ? yes S(2) P(2) C(19) 110.4(3) ? ? ? yes N(1) P(2) C(13) 111.9(3) ? ? ? yes N(1) P(2) C(19) 108.3(3) ? ? ? yes C(13) P(2) C(19) 103.7(4) ? ? ? yes S(3) P(3) N(2) 117.7(3) ? ? ? yes S(3) P(3) C(25) 106.2(3) ? ? ? yes S(3) P(3) C(31) 110.3(3) ? ? ? yes N(2) P(3) C(25) 107.2(3) ? ? ? yes N(2) P(3) C(31) 109.6(3) ? ? ? yes C(25) P(3) C(31) 105.0(3) ? ? ? yes S(4) P(4) N(2) 116.8(2) ? ? ? yes S(4) P(4) C(37) 110.4(3) ? ? ? yes S(4) P(4) C(43) 106.3(3) ? ? ? yes N(2) P(4) C(37) 111.4(3) ? ? ? yes N(2) P(4) C(43) 106.5(3) ? ? ? yes C(37) P(4) C(43) 104.5(3) ? ? ? yes P(1) N(1) P(2) 127.1(4) ? ? ? yes P(3) N(2) P(4) 126.4(4) ? ? ? yes P(1) C(1) C(2) 119.9(6) ? ? ? yes P(1) C(1) C(6) 118.7(6) ? ? ? yes C(2) C(1) C(6) 121.1(7) ? ? ? yes C(1) C(2) C(3) 118.4(9) ? ? ? yes C(2) C(3) C(4) 118(1) ? ? ? yes C(3) C(4) C(5) 123.5(10) ? ? ? yes C(4) C(5) C(6) 118.4(9) ? ? ? yes C(1) C(6) C(5) 119.8(9) ? ? ? yes P(1) C(7) C(8) 122.1(6) ? ? ? yes P(1) C(7) C(12) 118.6(6) ? ? ? yes C(8) C(7) C(12) 119.1(8) ? ? ? yes C(7) C(8) C(9) 120.5(7) ? ? ? yes C(8) C(9) C(10) 120.1(8) ? ? ? yes C(9) C(10) C(11) 120.5(9) ? ? ? yes C(10) C(11) C(12) 120.0(8) ? ? ? yes C(7) C(12) C(11) 119.8(7) ? ? ? yes P(2) C(13) C(14) 121.7(6) ? ? ? yes P(2) C(13) C(18) 119.3(6) ? ? ? yes C(14) C(13) C(18) 118.9(7) ? ? ? yes C(13) C(14) C(15) 120.2(7) ? ? ? yes C(14) C(15) C(16) 119.7(8) ? ? ? yes C(15) C(16) C(17) 121.1(9) ? ? ? yes C(16) C(17) C(18) 119.1(8) ? ? ? yes C(13) C(18) C(17) 120.9(8) ? ? ? yes P(2) C(19) C(20) 121.3(6) ? ? ? yes P(2) C(19) C(24) 119.2(6) ? ? ? yes C(20) C(19) C(24) 119.4(8) ? ? ? yes C(19) C(20) C(21) 118.8(8) ? ? ? yes C(20) C(21) C(22) 120.7(8) ? ? ? yes C(21) C(22) C(23) 121.1(9) ? ? ? yes C(22) C(23) C(24) 118.5(8) ? ? ? yes C(19) C(24) C(23) 121.5(8) ? ? ? yes P(3) C(25) C(26) 118.5(6) ? ? ? yes P(3) C(25) C(30) 122.9(6) ? ? ? yes C(26) C(25) C(30) 118.4(7) ? ? ? yes C(25) C(26) C(27) 120.9(7) ? ? ? yes C(26) C(27) C(28) 120.7(8) ? ? ? yes C(27) C(28) C(29) 120.8(9) ? ? ? yes C(28) C(29) C(30) 118.1(8) ? ? ? yes C(25) C(30) C(29) 121.0(8) ? ? ? yes P(3) C(31) C(32) 121.4(6) ? ? ? yes P(3) C(31) C(36) 119.4(6) ? ? ? yes C(32) C(31) C(36) 119.0(7) ? ? ? yes C(31) C(32) C(33) 120.0(7) ? ? ? yes C(32) C(33) C(34) 119.8(9) ? ? ? yes C(33) C(34) C(35) 121.9(9) ? ? ? yes C(34) C(35) C(36) 120.2(8) ? ? ? yes C(31) C(36) C(35) 119.0(8) ? ? ? yes P(4) C(37) C(38) 122.1(6) ? ? ? yes P(4) C(37) C(42) 120.1(6) ? ? ? yes C(38) C(37) C(42) 117.8(7) ? ? ? yes C(37) C(38) C(39) 120.7(7) ? ? ? yes C(38) C(39) C(40) 120.6(8) ? ? ? yes C(39) C(40) C(41) 120.9(9) ? ? ? yes C(40) C(41) C(42) 119.8(8) ? ? ? yes C(37) C(42) C(41) 120.3(8) ? ? ? yes P(4) C(43) C(44) 118.6(6) ? ? ? yes P(4) C(43) C(48) 121.1(6) ? ? ? yes C(44) C(43) C(48) 120.2(7) ? ? ? yes C(43) C(44) C(45) 118.8(8) ? ? ? yes C(44) C(45) C(46) 119.8(10) ? ? ? yes C(45) C(46) C(47) 121.9(10) ? ? ? yes C(46) C(47) C(48) 119.6(9) ? ? ? yes C(43) C(48) C(47) 119.6(8) ? ? ? yes Cl(1) C(49) Cl(2) 112.9(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; ##==========end of compound 1============ data_wtwong794-WHL242 #Compound 3 #------------------------------------------------------------------------------ _audit_creation_date 'Mon May 25 15:37:56 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.756(1) _cell_length_b 15.378(2) _cell_length_c 14.369(1) _cell_angle_alpha 90 _cell_angle_beta 99.64(2) _cell_angle_gamma 90 _cell_volume 2343.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'dark' _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.180 _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_meas ? _chemical_formula_weight 1306.79 _chemical_formula_analytical ? _chemical_formula_sum 'C48 H40 N2 O2 P4 Os Se4 ' _chemical_formula_moiety 'C48 H40 N2 O2 P4 Os Se4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1260.00 _exptl_absorpt_coefficient_mu 6.005 _exptl_absorpt_correction_type 'Inter-image scaling' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 22453 _reflns_number_total 4250 _reflns_number_observed 3663 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.08 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.58 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 2 -1.216 7.603 'International Tables' Se 0 8 -0.093 2.226 'International Tables' N 0 4 0.006 0.003 'International Tables' P 0 8 0.102 0.094 'International Tables' O 0 4 0.011 0.006 'International Tables' C 0 96 0.003 0.002 'International Tables' H 0 80 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Os(1) 1.0000 0.0000 1.0000 0.03848(7) Uij ? ? Se(1) 1.12494(4) -0.09424(3) 0.89873(3) 0.0474(1) Uij ? ? Se(2) 0.87620(4) 0.09661(3) 0.86856(3) 0.0476(1) Uij ? ? P(1) 1.03668(9) -0.07377(7) 0.75056(7) 0.0405(3) Uij ? ? P(2) 0.7933(1) -0.00062(6) 0.76472(8) 0.0418(3) Uij ? ? O(1) 0.8817(2) -0.0778(2) 0.9887(2) 0.0517(8) Uij ? ? N(1) 0.8872(3) -0.0678(2) 0.7289(2) 0.0484(10) Uij ? ? C(1) 1.1111(4) 0.0154(2) 0.6981(3) 0.045(1) Uij ? ? C(2) 1.2315(5) 0.0436(4) 0.7320(3) 0.067(2) Uij ? ? C(3) 1.2863(6) 0.1059(4) 0.6839(4) 0.084(2) Uij ? ? C(4) 1.2227(6) 0.1418(4) 0.6033(4) 0.078(2) Uij ? ? C(5) 1.1038(6) 0.1159(4) 0.5715(4) 0.084(2) Uij ? ? C(6) 1.0464(5) 0.0531(3) 0.6174(3) 0.066(2) Uij ? ? C(7) 1.0772(4) -0.1689(3) 0.6881(3) 0.042(1) Uij ? ? C(8) 1.2002(4) -0.1847(3) 0.6764(4) 0.064(2) Uij ? ? C(9) 1.2289(5) -0.2569(4) 0.6267(4) 0.070(2) Uij ? ? C(10) 1.1358(6) -0.3119(3) 0.5860(4) 0.070(2) Uij ? ? C(11) 1.0136(5) -0.2972(3) 0.5963(4) 0.061(1) Uij ? ? C(12) 0.9837(4) -0.2260(3) 0.6488(3) 0.052(1) Uij ? ? C(13) 0.7116(4) 0.0612(3) 0.6659(3) 0.049(1) Uij ? ? C(14) 0.6942(6) 0.0251(4) 0.5764(4) 0.072(2) Uij ? ? C(15) 0.6256(6) 0.0689(5) 0.5012(4) 0.092(2) Uij ? ? C(16) 0.5761(6) 0.1492(5) 0.5136(4) 0.085(2) Uij ? ? C(17) 0.5928(6) 0.1859(4) 0.6005(5) 0.084(2) Uij ? ? C(18) 0.6606(5) 0.1422(3) 0.6771(4) 0.068(2) Uij ? ? C(19) 0.6709(3) -0.0632(3) 0.8055(3) 0.045(1) Uij ? ? C(20) 0.6525(5) -0.1486(3) 0.7801(4) 0.072(2) Uij ? ? C(21) 0.5534(6) -0.1952(4) 0.8043(5) 0.084(2) Uij ? ? C(22) 0.4715(5) -0.1567(4) 0.8548(4) 0.070(2) Uij ? ? C(23) 0.4899(5) -0.0721(4) 0.8820(4) 0.067(2) Uij ? ? C(24) 0.5896(5) -0.0248(3) 0.8581(4) 0.060(1) Uij ? ? H(1) 1.2768 0.0199 0.7888 0.0798 Uij ? ? H(2) 1.3700 0.1243 0.7073 0.1009 Uij ? ? H(3) 1.2617 0.1844 0.5700 0.0938 Uij ? ? H(4) 1.0584 0.1417 0.5160 0.1013 Uij ? ? H(5) 0.9623 0.0358 0.5935 0.0792 Uij ? ? H(6) 1.2653 -0.1457 0.7026 0.0765 Uij ? ? H(7) 1.3140 -0.2683 0.6209 0.0838 Uij ? ? H(8) 1.1561 -0.3604 0.5505 0.0837 Uij ? ? H(9) 0.9489 -0.3354 0.5677 0.0733 Uij ? ? H(10) 0.8991 -0.2168 0.6574 0.0626 Uij ? ? H(11) 0.7297 -0.0301 0.5668 0.0863 Uij ? ? H(12) 0.6126 0.0431 0.4403 0.1103 Uij ? ? H(13) 0.5299 0.1793 0.4612 0.1020 Uij ? ? H(14) 0.5582 0.2416 0.6090 0.1004 Uij ? ? H(15) 0.6720 0.1682 0.7379 0.0819 Uij ? ? H(16) 0.7091 -0.1762 0.7453 0.0864 Uij ? ? H(17) 0.5419 -0.2544 0.7858 0.1008 Uij ? ? H(18) 0.4024 -0.1885 0.8708 0.0843 Uij ? ? H(19) 0.4337 -0.0452 0.9177 0.0800 Uij ? ? H(20) 0.6020 0.0340 0.8780 0.0719 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0426(1) 0.0379(1) 0.0362(1) -0.00543(8) 0.01055(8) -0.00053(9) Se(1) 0.0521(2) 0.0531(3) 0.0385(2) 0.0087(2) 0.0120(2) 0.0002(2) Se(2) 0.0590(3) 0.0393(2) 0.0438(2) -0.0009(2) 0.0072(2) 0.0006(2) P(1) 0.0446(5) 0.0393(6) 0.0389(5) 0.0009(4) 0.0109(4) -0.0019(4) P(2) 0.0417(6) 0.0416(6) 0.0430(6) 0.0013(4) 0.0099(4) -0.0013(4) O(1) 0.054(2) 0.048(2) 0.053(2) -0.008(1) 0.010(1) 0.001(1) N(1) 0.047(2) 0.047(2) 0.052(2) 0.000(1) 0.010(1) -0.008(2) C(1) 0.056(2) 0.039(2) 0.042(2) 0.000(2) 0.013(2) -0.003(2) C(2) 0.069(3) 0.071(3) 0.058(3) -0.021(3) 0.004(2) 0.006(3) C(3) 0.095(4) 0.080(4) 0.078(4) -0.038(3) 0.017(3) 0.002(3) C(4) 0.115(5) 0.053(3) 0.075(4) -0.018(3) 0.040(3) 0.003(3) C(5) 0.105(5) 0.084(4) 0.064(4) -0.001(3) 0.014(3) 0.028(3) C(6) 0.070(3) 0.071(3) 0.055(3) -0.006(2) 0.004(2) 0.016(3) C(7) 0.049(2) 0.041(2) 0.035(2) 0.001(2) 0.009(2) -0.001(2) C(8) 0.061(3) 0.055(3) 0.078(3) 0.000(2) 0.020(2) -0.015(2) C(9) 0.069(3) 0.063(3) 0.084(4) 0.013(2) 0.033(3) -0.012(3) C(10) 0.103(4) 0.050(3) 0.059(3) 0.012(3) 0.024(3) -0.009(2) C(11) 0.078(3) 0.043(3) 0.062(3) -0.005(2) 0.010(2) -0.008(2) C(12) 0.060(3) 0.048(3) 0.049(3) -0.003(2) 0.012(2) 0.001(2) C(13) 0.049(2) 0.051(3) 0.050(3) -0.001(2) 0.015(2) 0.003(2) C(14) 0.085(4) 0.076(3) 0.051(3) 0.013(3) 0.001(3) -0.003(3) C(15) 0.101(4) 0.122(6) 0.048(3) 0.006(4) 0.000(3) 0.002(3) C(16) 0.081(4) 0.105(5) 0.067(4) 0.016(3) 0.007(3) 0.033(4) C(17) 0.089(4) 0.077(4) 0.084(4) 0.028(3) 0.013(3) 0.029(3) C(18) 0.085(3) 0.061(3) 0.057(3) 0.018(3) 0.009(2) 0.003(2) C(19) 0.042(2) 0.043(2) 0.048(2) 0.001(2) 0.006(2) 0.004(2) C(20) 0.072(3) 0.057(3) 0.095(4) -0.008(2) 0.037(3) -0.014(3) C(21) 0.090(4) 0.058(3) 0.113(5) -0.026(3) 0.040(3) -0.020(3) C(22) 0.060(3) 0.078(4) 0.074(4) -0.012(2) 0.014(2) 0.011(3) C(23) 0.053(3) 0.077(4) 0.075(3) 0.006(2) 0.028(2) 0.016(3) C(24) 0.059(3) 0.050(3) 0.075(3) 0.005(2) 0.025(2) 0.002(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3663 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0303 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0356 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.757 _refine_ls_shift/esd_max 0.0210 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.44 _refine_diff_density_max 0.44 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Se(1) 2.5843(4) ? ? yes Os(1) Se(1) 2.5843(4) ? ? yes Os(1) Se(2) 2.5895(4) ? ? yes Os(1) Se(2) 2.5895(4) ? ? yes Os(1) O(1) 1.734(3) ? ? yes Os(1) O(1) 1.734(3) ? ? yes Se(1) P(1) 2.204(1) ? ? yes Se(2) P(2) 2.194(1) ? ? yes P(1) N(1) 1.588(3) ? ? yes P(1) C(1) 1.815(4) ? ? yes P(1) C(7) 1.808(4) ? ? yes P(2) N(1) 1.590(4) ? ? yes P(2) C(13) 1.809(4) ? ? yes P(2) C(19) 1.805(4) ? ? yes C(1) C(2) 1.375(6) ? ? yes C(1) C(6) 1.377(6) ? ? yes C(2) C(3) 1.370(9) ? ? yes C(3) C(4) 1.359(8) ? ? yes C(4) C(5) 1.344(9) ? ? yes C(5) C(6) 1.372(8) ? ? yes C(7) C(8) 1.382(6) ? ? yes C(7) C(12) 1.383(6) ? ? yes C(8) C(9) 1.383(8) ? ? yes C(9) C(10) 1.365(7) ? ? yes C(10) C(11) 1.366(8) ? ? yes C(11) C(12) 1.398(7) ? ? yes C(13) C(14) 1.384(7) ? ? yes C(13) C(18) 1.381(7) ? ? yes C(14) C(15) 1.378(8) ? ? yes C(15) C(16) 1.37(1) ? ? yes C(16) C(17) 1.354(9) ? ? yes C(17) C(18) 1.388(8) ? ? yes C(19) C(20) 1.368(7) ? ? yes C(19) C(24) 1.382(7) ? ? yes C(20) C(21) 1.377(8) ? ? yes C(21) C(22) 1.367(9) ? ? yes C(22) C(23) 1.363(8) ? ? yes C(23) C(24) 1.386(8) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Os(1) Se(1) 180.0000(1) ? ? ? yes Se(1) Os(1) Se(2) 99.41(1) ? ? ? yes Se(1) Os(1) Se(2) 80.59(1) ? ? ? yes Se(1) Os(1) O(1) 90.16(10) ? ? ? yes Se(1) Os(1) O(1) 89.84(10) ? ? ? yes Se(1) Os(1) Se(2) 80.59(1) ? ? ? yes Se(1) Os(1) Se(2) 99.41(1) ? ? ? yes Se(1) Os(1) O(1) 89.84(10) ? ? ? yes Se(1) Os(1) O(1) 90.16(10) ? ? ? yes Se(2) Os(1) Se(2) 180.0000(1) ? ? ? yes Se(2) Os(1) O(1) 92.75(9) ? ? ? yes Se(2) Os(1) O(1) 87.25(9) ? ? ? yes Se(2) Os(1) O(1) 87.25(9) ? ? ? yes Se(2) Os(1) O(1) 92.75(9) ? ? ? yes O(1) Os(1) O(1) 180.0000(1) ? ? ? yes Os(1) Se(1) P(1) 106.46(3) ? ? ? yes Os(1) Se(2) P(2) 101.88(3) ? ? ? yes Se(1) P(1) N(1) 117.1(1) ? ? ? yes Se(1) P(1) C(1) 111.1(1) ? ? ? yes Se(1) P(1) C(7) 105.2(1) ? ? ? yes N(1) P(1) C(1) 112.2(2) ? ? ? yes N(1) P(1) C(7) 105.7(2) ? ? ? yes C(1) P(1) C(7) 104.2(2) ? ? ? yes Se(2) P(2) N(1) 117.1(1) ? ? ? yes Se(2) P(2) C(13) 105.3(1) ? ? ? yes Se(2) P(2) C(19) 112.2(1) ? ? ? yes N(1) P(2) C(13) 109.8(2) ? ? ? yes N(1) P(2) C(19) 107.2(2) ? ? ? yes C(13) P(2) C(19) 104.5(2) ? ? ? yes P(1) N(1) P(2) 130.7(2) ? ? ? yes P(1) C(1) C(2) 123.1(3) ? ? ? yes P(1) C(1) C(6) 118.2(3) ? ? ? yes C(2) C(1) C(6) 118.6(4) ? ? ? yes C(1) C(2) C(3) 120.0(5) ? ? ? yes C(2) C(3) C(4) 121.0(6) ? ? ? yes C(3) C(4) C(5) 118.9(6) ? ? ? yes C(4) C(5) C(6) 121.6(5) ? ? ? yes C(1) C(6) C(5) 119.7(5) ? ? ? yes P(1) C(7) C(8) 121.2(3) ? ? ? yes P(1) C(7) C(12) 119.8(3) ? ? ? yes C(8) C(7) C(12) 119.0(4) ? ? ? yes C(7) C(8) C(9) 120.3(4) ? ? ? yes C(8) C(9) C(10) 120.5(5) ? ? ? yes C(9) C(10) C(11) 120.1(5) ? ? ? yes C(10) C(11) C(12) 120.0(4) ? ? ? yes C(7) C(12) C(11) 120.1(4) ? ? ? yes P(2) C(13) C(14) 119.4(4) ? ? ? yes P(2) C(13) C(18) 122.2(3) ? ? ? yes C(14) C(13) C(18) 118.4(4) ? ? ? yes C(13) C(14) C(15) 120.3(6) ? ? ? yes C(14) C(15) C(16) 120.5(6) ? ? ? yes C(15) C(16) C(17) 120.1(6) ? ? ? yes C(16) C(17) C(18) 120.0(6) ? ? ? yes C(13) C(18) C(17) 120.7(5) ? ? ? yes P(2) C(19) C(20) 120.4(4) ? ? ? yes P(2) C(19) C(24) 120.8(3) ? ? ? yes C(20) C(19) C(24) 118.6(4) ? ? ? yes C(19) C(20) C(21) 121.1(5) ? ? ? yes C(20) C(21) C(22) 120.2(5) ? ? ? yes C(21) C(22) C(23) 119.4(5) ? ? ? yes C(22) C(23) C(24) 120.7(5) ? ? ? yes C(19) C(24) C(23) 119.9(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #==========end of compound 3============ data_[Os{N(SPPh2)2}3] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 N3 Os P6 S6' _chemical_formula_weight 1535.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 '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 10.953(2) _cell_length_b 14.611(2) _cell_length_c 22.038(2) _cell_angle_alpha 82.640(10) _cell_angle_beta 86.660(10) _cell_angle_gamma 78.730(10) _cell_volume 3428.3(8) _cell_formula_units_Z 2 _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 1.2 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1550 _exptl_absorpt_coefficient_mu 2.227 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12301 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12044 _reflns_number_gt 9955 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.4922P] 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 12044 _refine_ls_number_parameters 746 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.264 _refine_ls_shift/su_mean 0.012 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 Os1 Os 0.274867(18) 0.330231(13) 0.228479(8) 0.02661(6) Uani 1 1 d . . . S1 S 0.37846(12) 0.34007(9) 0.31984(6) 0.0363(3) Uani 1 1 d . . . S2 S 0.16153(13) 0.21060(10) 0.27131(7) 0.0430(3) Uani 1 1 d . . . S3 S 0.09459(11) 0.44357(9) 0.25878(6) 0.0345(3) Uani 1 1 d . . . S4 S 0.36310(13) 0.45419(9) 0.17139(6) 0.0395(3) Uani 1 1 d . . . S5 S 0.14970(13) 0.34778(9) 0.13872(6) 0.0395(3) Uani 1 1 d . . . S6 S 0.44253(12) 0.20802(9) 0.20389(6) 0.0385(3) Uani 1 1 d . . . P1 P 0.45812(13) 0.21096(10) 0.35885(6) 0.0396(3) Uani 1 1 d . . . P2 P 0.24505(14) 0.12574(9) 0.34367(6) 0.0383(3) Uani 1 1 d . . . P3 P 0.15014(12) 0.54182(9) 0.30207(6) 0.0331(3) Uani 1 1 d . . . P4 P 0.37707(14) 0.55341(10) 0.22538(7) 0.0411(3) Uani 1 1 d . . . P5 P 0.22092(12) 0.25795(9) 0.07672(5) 0.0311(3) Uani 1 1 d . . . P6 P 0.47972(12) 0.21285(9) 0.11282(6) 0.0325(3) Uani 1 1 d . . . N1 N 0.3857(4) 0.1268(3) 0.3578(2) 0.0453(11) Uani 1 1 d . . . N2 N 0.2720(4) 0.5787(3) 0.2769(2) 0.0415(10) Uani 1 1 d . . . N3 N 0.3679(4) 0.2294(3) 0.06778(19) 0.0393(10) Uani 1 1 d . . . C11 C 0.6134(5) 0.1730(4) 0.3277(3) 0.0473(14) Uani 1 1 d . . . C12 C 0.6638(7) 0.0790(5) 0.3271(4) 0.072(2) Uani 1 1 d . . . H12 H 0.6174 0.0340 0.3429 0.086 Uiso 1 1 calc R . . C13 C 0.7841(8) 0.0508(6) 0.3029(5) 0.091(3) Uani 1 1 d . . . H13 H 0.8178 -0.0128 0.3031 0.109 Uiso 1 1 calc R . . C14 C 0.8521(7) 0.1165(8) 0.2791(4) 0.091(3) Uani 1 1 d . . . H14 H 0.9313 0.0977 0.2619 0.109 Uiso 1 1 calc R . . C15 C 0.8046(7) 0.2095(7) 0.2803(4) 0.080(2) Uani 1 1 d . . . H15 H 0.8523 0.2540 0.2652 0.096 Uiso 1 1 calc R . . C16 C 0.6854(6) 0.2380(5) 0.3038(3) 0.0601(17) Uani 1 1 d . . . H16 H 0.6532 0.3018 0.3037 0.072 Uiso 1 1 calc R . . C21 C 0.4846(6) 0.2257(5) 0.4381(3) 0.0544(15) Uani 1 1 d . . . C22 C 0.5199(13) 0.1465(7) 0.4782(4) 0.142(5) Uani 1 1 d . . . H22 H 0.5264 0.0872 0.4658 0.170 Uiso 1 1 calc R . . C23 C 0.5461(15) 0.1561(9) 0.5386(4) 0.159(6) Uani 1 1 d . . . H23 H 0.5709 0.1026 0.5659 0.191 Uiso 1 1 calc R . . C24 C 0.5361(11) 0.2400(9) 0.5571(4) 0.120(4) Uani 1 1 d . . . H24 H 0.5492 0.2448 0.5978 0.144 Uiso 1 1 calc R . . C25 C 0.5070(11) 0.3186(8) 0.5173(4) 0.115(4) Uani 1 1 d . . . H25 H 0.5044 0.3774 0.5299 0.138 Uiso 1 1 calc R . . C26 C 0.4806(9) 0.3109(6) 0.4568(3) 0.086(3) Uani 1 1 d . . . H26 H 0.4601 0.3649 0.4293 0.103 Uiso 1 1 calc R . . C31 C 0.1421(7) 0.1402(4) 0.4108(3) 0.0578(17) Uani 1 1 d . . . C32 C 0.1823(11) 0.0965(7) 0.4673(4) 0.111(4) Uani 1 1 d . . . H32 H 0.2625 0.0612 0.4711 0.133 Uiso 1 1 calc R . . C33 C 0.1011(17) 0.1057(11) 0.5190(5) 0.166(7) Uani 1 1 d . . . H33 H 0.1276 0.0768 0.5573 0.200 Uiso 1 1 calc R . . C34 C -0.0148(17) 0.1563(11) 0.5129(6) 0.155(7) Uani 1 1 d . . . H34 H -0.0672 0.1627 0.5475 0.186 Uiso 1 1 calc R . . C35 C -0.0567(11) 0.1974(9) 0.4587(6) 0.129(4) Uani 1 1 d . . . H35 H -0.1384 0.2299 0.4554 0.155 Uiso 1 1 calc R . . C36 C 0.0225(8) 0.1917(6) 0.4067(4) 0.081(2) Uani 1 1 d . . . H36 H -0.0056 0.2229 0.3692 0.097 Uiso 1 1 calc R . . C41 C 0.2474(6) 0.0070(4) 0.3281(2) 0.0437(13) Uani 1 1 d . . . C42 C 0.1429(7) -0.0345(5) 0.3387(3) 0.0621(17) Uani 1 1 d . . . H42 H 0.0709 -0.0029 0.3569 0.075 Uiso 1 1 calc R . . C43 C 0.1471(9) -0.1244(5) 0.3219(4) 0.078(2) Uani 1 1 d . . . H43 H 0.0767 -0.1516 0.3280 0.094 Uiso 1 1 calc R . . C44 C 0.2523(10) -0.1720(5) 0.2969(4) 0.083(3) Uani 1 1 d . . . H44 H 0.2553 -0.2325 0.2873 0.100 Uiso 1 1 calc R . . C45 C 0.3547(9) -0.1305(6) 0.2859(4) 0.081(2) Uani 1 1 d . . . H45 H 0.4264 -0.1627 0.2677 0.097 Uiso 1 1 calc R . . C46 C 0.3526(7) -0.0416(5) 0.3014(3) 0.0628(17) Uani 1 1 d . . . H46 H 0.4228 -0.0143 0.2936 0.075 Uiso 1 1 calc R . . C51 C 0.1637(5) 0.5064(4) 0.3834(2) 0.0397(12) Uani 1 1 d . . . C52 C 0.1242(6) 0.4275(4) 0.4121(3) 0.0499(14) Uani 1 1 d . . . H52 H 0.0904 0.3898 0.3893 0.060 Uiso 1 1 calc R . . C53 C 0.1346(7) 0.4037(6) 0.4750(3) 0.072(2) Uani 1 1 d . . . H53 H 0.1094 0.3495 0.4939 0.086 Uiso 1 1 calc R . . C54 C 0.1811(8) 0.4591(7) 0.5084(3) 0.081(2) Uani 1 1 d . . . H54 H 0.1865 0.4430 0.5505 0.097 Uiso 1 1 calc R . . C55 C 0.2207(7) 0.5389(7) 0.4817(3) 0.079(2) Uani 1 1 d . . . H55 H 0.2527 0.5762 0.5055 0.095 Uiso 1 1 calc R . . C56 C 0.2126(6) 0.5634(5) 0.4188(3) 0.0586(17) Uani 1 1 d . . . H56 H 0.2393 0.6172 0.4002 0.070 Uiso 1 1 calc R . . C61 C 0.0178(5) 0.6389(4) 0.2971(3) 0.0453(13) Uani 1 1 d . . . C62 C -0.0084(10) 0.6886(6) 0.2422(4) 0.101(3) Uani 1 1 d . . . H62 H 0.0439 0.6752 0.2084 0.121 Uiso 1 1 calc R . . C63 C -0.1137(12) 0.7602(7) 0.2355(5) 0.140(5) Uani 1 1 d . . . H63 H -0.1315 0.7937 0.1972 0.168 Uiso 1 1 calc R . . C64 C -0.1910(8) 0.7814(6) 0.2850(5) 0.101(3) Uani 1 1 d . . . H64 H -0.2617 0.8284 0.2805 0.121 Uiso 1 1 calc R . . C65 C -0.1632(8) 0.7330(6) 0.3405(5) 0.105(3) Uani 1 1 d . . . H65 H -0.2151 0.7463 0.3744 0.125 Uiso 1 1 calc R . . C66 C -0.0576(7) 0.6640(5) 0.3468(4) 0.081(2) Uani 1 1 d . . . H66 H -0.0368 0.6336 0.3855 0.098 Uiso 1 1 calc R . . C71 C 0.3569(14) 0.6600(9) 0.1633(7) 0.042(3) Uiso 0.50 1 d P . . C71A C 0.3972(11) 0.6562(7) 0.1791(5) 0.029(2) Uiso 0.50 1 d P . . C72 C 0.2552(17) 0.6803(12) 0.1275(7) 0.071(4) Uiso 0.50 1 d P . . H72 H 0.1975 0.6381 0.1311 0.085 Uiso 0.50 1 d PR . . C72A C 0.3110(15) 0.6890(10) 0.1341(7) 0.055(3) Uiso 0.50 1 d P . . H72A H 0.2541 0.6491 0.1277 0.066 Uiso 0.50 1 d PR . . C73 C 0.233(2) 0.7600(15) 0.0834(10) 0.102(6) Uiso 0.50 1 d P . . H73 H 0.1651 0.7778 0.0563 0.122 Uiso 0.50 1 d PR . . C73A C 0.306(2) 0.7760(15) 0.0999(10) 0.088(6) Uiso 0.50 1 d P . . H73A H 0.2384 0.8014 0.0730 0.105 Uiso 0.50 1 d PR . . C74 C 0.321(3) 0.813(2) 0.0799(12) 0.116(8) Uiso 0.50 1 d P . . H74 H 0.3160 0.8669 0.0496 0.139 Uiso 0.50 1 d PR . . C74A C 0.3852(18) 0.8217(12) 0.1031(8) 0.063(4) Uiso 0.50 1 d P . . H74A H 0.3906 0.8765 0.0746 0.075 Uiso 0.50 1 d PR . . C75 C 0.4309(19) 0.8083(12) 0.1172(8) 0.069(5) Uiso 0.50 1 d P . . H75 H 0.4871 0.8515 0.1157 0.083 Uiso 0.50 1 d PR . . C75A C 0.4865(13) 0.7944(10) 0.1502(7) 0.059(3) Uiso 0.50 1 d P . . H75A H 0.5439 0.8348 0.1550 0.071 Uiso 0.50 1 d PR . . C76 C 0.4407(14) 0.7184(10) 0.1590(7) 0.062(3) Uiso 0.50 1 d P . . H76 H 0.5088 0.7007 0.1863 0.075 Uiso 0.50 1 d PR . . C76A C 0.4876(11) 0.7093(8) 0.1862(6) 0.046(3) Uiso 0.50 1 d P . . H76A H 0.5507 0.6851 0.2157 0.055 Uiso 0.50 1 d PR . . C81 C 0.5259(6) 0.5284(4) 0.2614(3) 0.0547(15) Uiso 1 1 d . . . C82 C 0.5344(7) 0.5295(7) 0.3263(4) 0.058(2) Uiso 0.70 1 d P . . H82 H 0.4604 0.5496 0.3504 0.069 Uiso 0.70 1 d PR . . C82A C 0.5287(7) 0.5728(7) 0.3100(4) 0.048(5) Uiso 0.30 1 d PR . . H82A H 0.4575 0.6167 0.3227 0.058 Uiso 0.30 1 d PR . . C83 C 0.6515(9) 0.5026(9) 0.3539(5) 0.086(3) Uiso 0.70 1 d P . . H83 H 0.6560 0.5011 0.3974 0.104 Uiso 0.70 1 d PR . . C83A C 0.6397(9) 0.5531(9) 0.3411(5) 0.050(5) Uiso 0.30 1 d PR . . H83A H 0.6448 0.5593 0.3837 0.060 Uiso 0.30 1 d PR . . C84 C 0.7576(9) 0.4769(9) 0.3204(5) 0.079(3) Uiso 0.70 1 d P . . H84 H 0.8370 0.4615 0.3392 0.094 Uiso 0.70 1 d PR . . C84A C 0.7468(9) 0.5201(9) 0.3023(5) 0.070(7) Uiso 0.30 1 d PR . . H84A H 0.8245 0.5345 0.3123 0.084 Uiso 0.30 1 d PR . . C85 C 0.7481(8) 0.4765(6) 0.2554(4) 0.076(2) Uiso 1 1 d . . . H85 H 0.8222 0.4627 0.2302 0.091 Uiso 1 1 d R . . C86 C 0.6336(7) 0.4944(5) 0.2293(3) 0.0655(18) Uiso 1 1 d . . . H86 H 0.6281 0.4832 0.1890 0.079 Uiso 1 1 d R . . C91 C 0.1526(5) 0.1538(4) 0.0924(2) 0.0401(12) Uani 1 1 d . . . C92 C 0.2038(7) 0.0828(4) 0.1347(3) 0.0603(17) Uani 1 1 d . . . H92 H 0.2756 0.0876 0.1536 0.072 Uiso 1 1 calc R . . C93 C 0.1519(8) 0.0034(5) 0.1503(4) 0.076(2) Uani 1 1 d . . . H93 H 0.1892 -0.0443 0.1793 0.091 Uiso 1 1 calc R . . C94 C 0.0492(9) -0.0047(6) 0.1241(5) 0.112(4) Uani 1 1 d . . . H94 H 0.0127 -0.0571 0.1352 0.134 Uiso 1 1 calc R . . C95 C -0.0029(11) 0.0659(8) 0.0799(7) 0.158(6) Uani 1 1 d . . . H95 H -0.0740 0.0601 0.0608 0.190 Uiso 1 1 calc R . . C96 C 0.0486(9) 0.1447(6) 0.0638(5) 0.113(4) Uani 1 1 d . . . H96 H 0.0131 0.1914 0.0338 0.136 Uiso 1 1 calc R . . C101 C 0.1650(5) 0.3157(4) 0.0032(2) 0.0340(11) Uani 1 1 d . . . C102 C 0.2435(6) 0.3109(4) -0.0483(2) 0.0453(13) Uani 1 1 d . . . H102 H 0.3246 0.2770 -0.0455 0.054 Uiso 1 1 calc R . . C103 C 0.2009(7) 0.3567(5) -0.1040(3) 0.0622(18) Uani 1 1 d . . . H103 H 0.2540 0.3531 -0.1385 0.075 Uiso 1 1 calc R . . C104 C 0.0818(7) 0.4075(5) -0.1095(3) 0.0592(17) Uani 1 1 d . . . H104 H 0.0544 0.4373 -0.1475 0.071 Uiso 1 1 calc R . . C105 C 0.0040(6) 0.4140(5) -0.0592(3) 0.0575(16) Uani 1 1 d . . . H105 H -0.0765 0.4488 -0.0626 0.069 Uiso 1 1 calc R . . C106 C 0.0447(5) 0.3685(4) -0.0026(2) 0.0471(14) Uani 1 1 d . . . H106 H -0.0087 0.3734 0.0317 0.057 Uiso 1 1 calc R . . C111 C 0.5796(5) 0.2964(4) 0.0866(2) 0.0400(12) Uani 1 1 d . . . C112 C 0.6791(6) 0.3023(5) 0.1209(3) 0.0604(17) Uani 1 1 d . . . H112 H 0.6953 0.2630 0.1573 0.072 Uiso 1 1 calc R . . C113 C 0.7548(7) 0.3671(6) 0.1008(4) 0.072(2) Uani 1 1 d . . . H113 H 0.8219 0.3707 0.1238 0.087 Uiso 1 1 calc R . . C114 C 0.7315(6) 0.4247(5) 0.0480(4) 0.068(2) Uani 1 1 d . . . H114 H 0.7813 0.4689 0.0353 0.082 Uiso 1 1 calc R . . C115 C 0.6342(7) 0.4182(5) 0.0129(4) 0.071(2) Uani 1 1 d . . . H115 H 0.6204 0.4565 -0.0241 0.085 Uiso 1 1 calc R . . C116 C 0.5566(6) 0.3549(4) 0.0324(3) 0.0554(15) Uani 1 1 d . . . H116 H 0.4897 0.3518 0.0092 0.066 Uiso 1 1 calc R . . C121 C 0.5769(5) 0.0994(4) 0.1039(2) 0.0403(12) Uiso 1 1 d . . . C122 C 0.5703(10) 0.0553(7) 0.0526(5) 0.061(2) Uiso 0.70 1 d P . . H122 H 0.5106 0.0826 0.0221 0.073 Uiso 0.70 1 d PR . . C123 C 0.6509(11) -0.0295(8) 0.0452(6) 0.075(3) Uiso 0.70 1 d P . . H123 H 0.6510 -0.0568 0.0078 0.091 Uiso 0.70 1 d PR . . C124 C 0.7318(8) -0.0700(6) 0.0860(4) 0.075(2) Uiso 1 1 d . . . H124 H 0.7884 -0.1270 0.0789 0.090 Uiso 1 1 d R . . C125 C 0.7340(12) -0.0317(8) 0.1416(6) 0.078(3) Uiso 0.70 1 d P . . H125 H 0.7873 -0.0641 0.1737 0.094 Uiso 0.70 1 d PR . . C126 C 0.6569(10) 0.0530(7) 0.1487(5) 0.066(3) Uiso 0.70 1 d P . . H126 H 0.6566 0.0792 0.1865 0.079 Uiso 0.70 1 d PR . . C127 C 0.6354(19) 0.0840(14) 0.0472(9) 0.046(4) Uiso 0.30 1 d P . . H127 H 0.6304 0.1392 0.0180 0.055 Uiso 0.30 1 d PR . . C128 C 0.706(2) -0.0008(17) 0.0360(11) 0.064(6) Uiso 0.30 1 d P . . H128 H 0.7441 -0.0052 -0.0041 0.077 Uiso 0.30 1 d PR . . C129 C 0.588(2) 0.0238(17) 0.1480(11) 0.066(6) Uiso 0.30 1 d P . . H129 H 0.5456 0.0295 0.1872 0.079 Uiso 0.30 1 d PR . . C130 C 0.671(3) -0.063(2) 0.1346(14) 0.087(8) Uiso 0.30 1 d P . . H130 H 0.6632 -0.1196 0.1610 0.105 Uiso 0.30 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.02883(10) 0.02744(10) 0.02358(9) -0.00242(6) -0.00333(6) -0.00512(7) S1 0.0415(7) 0.0363(7) 0.0322(6) -0.0063(5) -0.0110(5) -0.0054(5) S2 0.0371(7) 0.0410(7) 0.0511(8) 0.0107(6) -0.0101(6) -0.0157(6) S3 0.0310(6) 0.0358(7) 0.0378(6) -0.0103(5) -0.0013(5) -0.0054(5) S4 0.0530(8) 0.0367(7) 0.0307(6) -0.0045(5) 0.0063(6) -0.0152(6) S5 0.0422(7) 0.0430(7) 0.0307(6) -0.0111(5) -0.0128(5) 0.0059(6) S6 0.0367(7) 0.0430(7) 0.0313(6) -0.0042(5) -0.0053(5) 0.0043(6) P1 0.0426(8) 0.0421(8) 0.0337(7) 0.0002(6) -0.0147(6) -0.0063(6) P2 0.0488(8) 0.0335(7) 0.0329(7) 0.0015(5) -0.0024(6) -0.0115(6) P3 0.0370(7) 0.0310(6) 0.0313(6) -0.0062(5) 0.0036(5) -0.0066(5) P4 0.0471(8) 0.0356(7) 0.0445(7) -0.0100(6) 0.0139(6) -0.0183(6) P5 0.0311(7) 0.0357(7) 0.0266(6) -0.0041(5) -0.0042(5) -0.0050(5) P6 0.0281(6) 0.0363(7) 0.0324(6) -0.0057(5) -0.0024(5) -0.0026(5) N1 0.046(3) 0.041(3) 0.049(3) 0.005(2) -0.019(2) -0.010(2) N2 0.046(3) 0.038(2) 0.044(2) -0.0127(19) 0.009(2) -0.016(2) N3 0.031(2) 0.055(3) 0.032(2) -0.0076(19) -0.0043(18) -0.003(2) C11 0.041(3) 0.052(3) 0.049(3) -0.009(3) -0.020(3) 0.000(3) C12 0.058(4) 0.060(4) 0.097(6) -0.019(4) -0.014(4) -0.001(3) C13 0.059(5) 0.080(6) 0.131(8) -0.043(5) -0.020(5) 0.017(4) C14 0.042(4) 0.130(8) 0.096(6) -0.034(6) -0.008(4) 0.010(5) C15 0.044(4) 0.107(7) 0.080(5) 0.005(5) -0.008(4) -0.003(4) C16 0.044(4) 0.071(4) 0.060(4) -0.001(3) -0.009(3) 0.000(3) C21 0.063(4) 0.066(4) 0.034(3) -0.005(3) -0.018(3) -0.007(3) C22 0.257(15) 0.099(7) 0.063(5) 0.007(5) -0.089(8) -0.003(8) C23 0.270(18) 0.132(10) 0.061(6) 0.002(6) -0.079(8) 0.012(11) C24 0.160(11) 0.151(10) 0.048(5) -0.017(6) -0.043(6) -0.009(8) C25 0.155(10) 0.135(9) 0.059(5) -0.036(6) -0.034(6) -0.016(8) C26 0.123(7) 0.086(6) 0.052(4) -0.013(4) -0.031(4) -0.016(5) C31 0.088(5) 0.050(4) 0.040(3) -0.011(3) 0.010(3) -0.025(3) C32 0.152(10) 0.116(8) 0.051(5) 0.006(5) 0.023(5) -0.009(7) C33 0.255(19) 0.166(14) 0.053(6) 0.010(7) 0.056(9) -0.012(13) C34 0.222(18) 0.162(14) 0.083(8) -0.038(9) 0.085(11) -0.056(12) C35 0.118(9) 0.148(11) 0.122(9) -0.044(8) 0.070(8) -0.031(8) C36 0.082(6) 0.084(5) 0.079(5) -0.025(4) 0.032(4) -0.021(5) C41 0.060(4) 0.034(3) 0.037(3) -0.002(2) -0.006(3) -0.009(3) C42 0.074(5) 0.048(4) 0.067(4) -0.009(3) 0.010(3) -0.021(3) C43 0.114(7) 0.050(4) 0.079(5) -0.005(4) -0.004(5) -0.039(4) C44 0.141(8) 0.039(4) 0.073(5) -0.008(3) -0.029(5) -0.015(5) C45 0.095(6) 0.064(5) 0.082(5) -0.030(4) -0.007(5) 0.007(4) C46 0.065(4) 0.065(4) 0.062(4) -0.018(3) 0.000(3) -0.015(3) C51 0.037(3) 0.046(3) 0.037(3) -0.006(2) 0.002(2) -0.011(2) C52 0.049(3) 0.057(4) 0.044(3) 0.000(3) 0.000(3) -0.015(3) C53 0.076(5) 0.095(6) 0.046(4) 0.014(4) -0.001(3) -0.033(4) C54 0.086(6) 0.124(7) 0.035(3) 0.004(4) 0.001(3) -0.037(5) C55 0.084(5) 0.126(7) 0.041(4) -0.029(4) 0.002(3) -0.042(5) C56 0.062(4) 0.081(5) 0.042(3) -0.022(3) 0.005(3) -0.030(4) C61 0.049(3) 0.036(3) 0.052(3) -0.013(2) -0.006(3) -0.003(2) C62 0.140(8) 0.083(6) 0.055(4) -0.008(4) -0.015(5) 0.042(6) C63 0.180(12) 0.108(8) 0.094(7) -0.008(6) -0.053(8) 0.079(8) C64 0.078(6) 0.070(5) 0.139(9) -0.028(6) -0.019(6) 0.041(5) C65 0.078(6) 0.084(6) 0.124(8) 0.007(6) 0.035(6) 0.028(5) C66 0.066(5) 0.071(5) 0.088(5) 0.009(4) 0.030(4) 0.012(4) C91 0.042(3) 0.037(3) 0.044(3) -0.004(2) -0.005(2) -0.014(2) C92 0.068(4) 0.051(4) 0.065(4) 0.005(3) -0.016(3) -0.023(3) C93 0.099(6) 0.045(4) 0.080(5) 0.013(3) -0.008(4) -0.016(4) C94 0.103(7) 0.070(6) 0.170(10) 0.025(6) -0.030(7) -0.055(5) C95 0.126(9) 0.122(9) 0.240(15) 0.071(10) -0.103(10) -0.086(8) C96 0.099(7) 0.082(6) 0.164(10) 0.052(6) -0.070(7) -0.058(5) C101 0.035(3) 0.042(3) 0.025(2) -0.003(2) -0.0081(19) -0.006(2) C102 0.049(3) 0.048(3) 0.036(3) -0.001(2) -0.001(2) -0.005(3) C103 0.075(5) 0.073(4) 0.032(3) 0.000(3) 0.001(3) -0.001(4) C104 0.076(5) 0.061(4) 0.034(3) 0.003(3) -0.013(3) 0.000(3) C105 0.056(4) 0.064(4) 0.045(3) -0.002(3) -0.016(3) 0.008(3) C106 0.036(3) 0.065(4) 0.034(3) -0.002(3) -0.006(2) 0.003(3) C111 0.033(3) 0.041(3) 0.046(3) -0.011(2) 0.006(2) -0.005(2) C112 0.047(4) 0.087(5) 0.054(4) -0.009(3) -0.003(3) -0.028(3) C113 0.059(4) 0.089(6) 0.084(5) -0.029(4) 0.008(4) -0.040(4) C114 0.042(4) 0.057(4) 0.108(6) -0.020(4) 0.026(4) -0.018(3) C115 0.064(5) 0.052(4) 0.089(5) 0.012(4) 0.014(4) -0.008(3) C116 0.050(4) 0.052(4) 0.060(4) 0.006(3) -0.004(3) -0.006(3) _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 Os1 S6 2.3884(13) . ? Os1 S4 2.3991(13) . ? Os1 S1 2.4013(12) . ? Os1 S2 2.4034(13) . ? Os1 S5 2.4305(12) . ? Os1 S3 2.4369(13) . ? S1 P1 2.0217(19) . ? S2 P2 2.0339(19) . ? S3 P3 2.0251(18) . ? S4 P4 2.0225(19) . ? S5 P5 2.0329(18) . ? S6 P6 2.0196(18) . ? P1 N1 1.591(5) . ? P1 C11 1.807(6) . ? P1 C21 1.832(6) . ? P2 N1 1.592(5) . ? P2 C41 1.807(5) . ? P2 C31 1.816(6) . ? P3 N2 1.580(4) . ? P3 C51 1.808(5) . ? P3 C61 1.817(6) . ? P4 N2 1.593(4) . ? P4 C71A 1.749(10) . ? P4 C81 1.806(7) . ? P4 C71 1.924(14) . ? P5 N3 1.590(4) . ? P5 C91 1.810(5) . ? P5 C101 1.809(5) . ? P6 N3 1.584(4) . ? P6 C121 1.813(5) . ? P6 C111 1.813(5) . ? C11 C12 1.378(9) . ? C11 C16 1.385(9) . ? C12 C13 1.397(11) . ? C13 C14 1.363(13) . ? C14 C15 1.360(12) . ? C15 C16 1.382(9) . ? C21 C26 1.352(10) . ? C21 C22 1.369(10) . ? C22 C23 1.407(12) . ? C23 C24 1.323(15) . ? C24 C25 1.350(14) . ? C25 C26 1.404(10) . ? C31 C36 1.379(11) . ? C31 C32 1.378(11) . ? C32 C33 1.409(14) . ? C33 C34 1.342(19) . ? C34 C35 1.331(18) . ? C35 C36 1.396(11) . ? C41 C46 1.374(9) . ? C41 C42 1.391(9) . ? C42 C43 1.401(9) . ? C43 C44 1.351(12) . ? C44 C45 1.371(12) . ? C45 C46 1.381(10) . ? C51 C52 1.377(8) . ? C51 C56 1.406(8) . ? C52 C53 1.389(8) . ? C53 C54 1.349(11) . ? C54 C55 1.372(11) . ? C55 C56 1.391(9) . ? C61 C62 1.345(9) . ? C61 C66 1.376(9) . ? C62 C63 1.399(12) . ? C63 C64 1.371(14) . ? C64 C65 1.351(13) . ? C65 C66 1.379(10) . ? C71 C71A 0.567(14) . ? C71 C72A 0.855(16) . ? C71 C76 1.362(19) . ? C71 C72 1.37(2) . ? C71 C76A 1.844(19) . ? C71A C76 1.135(17) . ? C71A C72A 1.382(18) . ? C71A C76A 1.398(17) . ? C71A C72 1.93(2) . ? C72 C72A 0.675(19) . ? C72 C73 1.41(3) . ? C72 C73A 1.64(3) . ? C72A C73A 1.39(3) . ? C72A C73 1.59(3) . ? C72A C76 1.70(2) . ? C73 C73A 0.97(3) . ? C73 C74 1.34(3) . ? C73A C74 0.69(3) . ? C73A C74A 1.21(3) . ? C73A C75 1.61(3) . ? C74 C74A 0.93(3) . ? C74 C75 1.48(3) . ? C74A C75 0.59(2) . ? C74A C75A 1.52(2) . ? C74A C76 1.85(2) . ? C75 C75A 0.951(19) . ? C75 C76 1.49(2) . ? C75 C76A 2.00(2) . ? C75A C76 1.295(19) . ? C75A C76A 1.386(18) . ? C76 C76A 0.793(16) . ? C81 C82A 1.327(10) . ? C81 C86 1.379(9) . ? C81 C82 1.442(10) . ? C82 C82A 0.6795 . ? C82 C83A 1.336(12) . ? C82 C83 1.415(12) . ? C82A C83A 1.393(12) . ? C82A C83 1.776(14) . ? C83 C83A 0.7450 . ? C83 C84 1.355(12) . ? C83 C84A 1.528(14) . ? C83A C84A 1.451(12) . ? C83A C84 1.617(14) . ? C84 C84A 0.6943 . ? C84 C85 1.442(12) . ? C84A C85 1.279(11) . ? C85 C86 1.375(10) . ? C91 C92 1.358(8) . ? C91 C96 1.369(9) . ? C92 C93 1.386(9) . ? C93 C94 1.327(12) . ? C94 C95 1.384(13) . ? C95 C96 1.377(11) . ? C101 C102 1.386(7) . ? C101 C106 1.394(7) . ? C102 C103 1.380(8) . ? C103 C104 1.372(9) . ? C104 C105 1.361(9) . ? C105 C106 1.389(8) . ? C111 C116 1.381(8) . ? C111 C112 1.384(8) . ? C112 C113 1.393(9) . ? C113 C114 1.352(11) . ? C114 C115 1.377(11) . ? C115 C116 1.388(9) . ? C121 C126 1.379(11) . ? C121 C122 1.383(11) . ? C121 C127 1.40(2) . ? C121 C129 1.37(2) . ? C122 C127 0.890(19) . ? C122 C123 1.396(15) . ? C122 C128 1.60(3) . ? C123 C128 0.80(2) . ? C123 C124 1.303(13) . ? C123 C127 1.64(2) . ? C123 C130 1.98(3) . ? C124 C130 1.23(3) . ? C124 C125 1.414(14) . ? C124 C128 1.40(3) . ? C125 C130 0.93(3) . ? C125 C126 1.377(15) . ? C125 C129 1.66(3) . ? C126 C129 0.94(2) . ? C126 C130 1.74(3) . ? C127 C128 1.37(3) . ? C129 C130 1.47(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S6 Os1 S4 94.69(5) . . ? S6 Os1 S1 88.99(5) . . ? S4 Os1 S1 92.72(5) . . ? S6 Os1 S2 88.19(5) . . ? S4 Os1 S2 169.96(4) . . ? S1 Os1 S2 96.95(5) . . ? S6 Os1 S5 100.59(4) . . ? S4 Os1 S5 83.30(5) . . ? S1 Os1 S5 169.87(4) . . ? S2 Os1 S5 86.72(5) . . ? S6 Os1 S3 174.68(5) . . ? S4 Os1 S3 90.63(5) . . ? S1 Os1 S3 90.92(4) . . ? S2 Os1 S3 86.54(5) . . ? S5 Os1 S3 79.84(4) . . ? P1 S1 Os1 111.06(7) . . ? P2 S2 Os1 113.55(7) . . ? P3 S3 Os1 110.09(6) . . ? P4 S4 Os1 110.54(7) . . ? P5 S5 Os1 113.81(6) . . ? P6 S6 Os1 112.16(6) . . ? N1 P1 C11 106.9(3) . . ? N1 P1 C21 110.0(3) . . ? C11 P1 C21 103.4(3) . . ? N1 P1 S1 118.17(17) . . ? C11 P1 S1 112.1(2) . . ? C21 P1 S1 105.4(2) . . ? N1 P2 C41 104.4(3) . . ? N1 P2 C31 112.2(3) . . ? C41 P2 C31 104.7(3) . . ? N1 P2 S2 120.18(18) . . ? C41 P2 S2 105.73(18) . . ? C31 P2 S2 108.3(2) . . ? N2 P3 C51 108.3(2) . . ? N2 P3 C61 109.6(3) . . ? C51 P3 C61 103.7(3) . . ? N2 P3 S3 118.21(17) . . ? C51 P3 S3 112.10(19) . . ? C61 P3 S3 103.87(19) . . ? N2 P4 C71A 109.4(4) . . ? N2 P4 C81 107.6(3) . . ? C71A P4 C81 97.7(5) . . ? N2 P4 C71 106.1(4) . . ? C71A P4 C71 16.9(4) . . ? C81 P4 C71 114.1(5) . . ? N2 P4 S4 119.62(17) . . ? C71A P4 S4 109.0(4) . . ? C81 P4 S4 111.3(2) . . ? C71 P4 S4 97.9(4) . . ? N3 P5 C91 110.2(3) . . ? N3 P5 C101 105.8(2) . . ? C91 P5 C101 106.2(2) . . ? N3 P5 S5 118.98(17) . . ? C91 P5 S5 108.82(19) . . ? C101 P5 S5 105.98(17) . . ? N3 P6 C121 108.3(2) . . ? N3 P6 C111 108.4(2) . . ? C121 P6 C111 104.1(2) . . ? N3 P6 S6 119.22(17) . . ? C121 P6 S6 104.07(18) . . ? C111 P6 S6 111.52(18) . . ? P1 N1 P2 131.7(3) . . ? P3 N2 P4 136.1(3) . . ? P6 N3 P5 133.5(3) . . ? C12 C11 C16 118.1(6) . . ? C12 C11 P1 121.3(5) . . ? C16 C11 P1 120.7(5) . . ? C11 C12 C13 120.6(8) . . ? C14 C13 C12 120.0(8) . . ? C15 C14 C13 120.1(8) . . ? C14 C15 C16 120.2(8) . . ? C11 C16 C15 121.0(7) . . ? C26 C21 C22 119.1(7) . . ? C26 C21 P1 122.7(5) . . ? C22 C21 P1 118.0(6) . . ? C21 C22 C23 119.0(10) . . ? C24 C23 C22 121.2(10) . . ? C23 C24 C25 120.4(8) . . ? C24 C25 C26 119.4(10) . . ? C21 C26 C25 120.8(8) . . ? C36 C31 C32 118.7(7) . . ? C36 C31 P2 121.7(5) . . ? C32 C31 P2 119.6(7) . . ? C31 C32 C33 119.5(11) . . ? C34 C33 C32 119.8(12) . . ? C35 C34 C33 121.8(11) . . ? C34 C35 C36 119.8(12) . . ? C31 C36 C35 120.4(10) . . ? C46 C41 C42 118.9(6) . . ? C46 C41 P2 119.1(5) . . ? C42 C41 P2 121.8(5) . . ? C41 C42 C43 119.5(7) . . ? C44 C43 C42 120.7(8) . . ? C43 C44 C45 119.6(7) . . ? C44 C45 C46 120.8(8) . . ? C41 C46 C45 120.4(7) . . ? C52 C51 C56 119.0(5) . . ? C52 C51 P3 122.3(4) . . ? C56 C51 P3 118.6(4) . . ? C51 C52 C53 120.4(6) . . ? C54 C53 C52 120.0(7) . . ? C53 C54 C55 121.4(6) . . ? C54 C55 C56 119.5(7) . . ? C51 C56 C55 119.6(7) . . ? C62 C61 C66 118.2(6) . . ? C62 C61 P3 118.5(5) . . ? C66 C61 P3 123.3(5) . . ? C61 C62 C63 120.5(9) . . ? C64 C63 C62 120.4(9) . . ? C65 C64 C63 119.2(7) . . ? C64 C65 C66 119.9(8) . . ? C61 C66 C65 121.7(8) . . ? C71A C71 C72A 152(3) . . ? C71A C71 C76 54.9(18) . . ? C72A C71 C76 97.6(17) . . ? C71A C71 C72 173(2) . . ? C72A C71 C72 23.6(14) . . ? C76 C71 C72 120.8(16) . . ? C71A C71 C76A 32.3(17) . . ? C72A C71 C76A 120.1(16) . . ? C76 C71 C76A 22.9(8) . . ? C72 C71 C76A 142.7(13) . . ? C71A C71 P4 63.8(19) . . ? C72A C71 P4 143.7(17) . . ? C76 C71 P4 118.7(13) . . ? C72 C71 P4 120.3(11) . . ? C76A C71 P4 96.0(8) . . ? C71 C71A C76 101(2) . . ? C71 C71A C72A 16.6(18) . . ? C76 C71A C72A 84.4(12) . . ? C71 C71A C76A 135(2) . . ? C76 C71A C76A 34.6(9) . . ? C72A C71A C76A 118.6(11) . . ? C71 C71A P4 99(2) . . ? C76 C71A P4 159.7(13) . . ? C72A C71A P4 115.9(10) . . ? C76A C71A P4 125.4(9) . . ? C71 C71A C72 5.2(17) . . ? C76 C71A C72 98.0(12) . . ? C72A C71A C72 14.0(9) . . ? C76A C71A C72 131.8(10) . . ? P4 C71A C72 102.3(7) . . ? C72A C72 C71 30.5(19) . . ? C72A C72 C73 92(3) . . ? C71 C72 C73 122.4(18) . . ? C72A C72 C73A 57(2) . . ? C71 C72 C73A 86.3(15) . . ? C73 C72 C73A 36.2(11) . . ? C72A C72 C71A 30(2) . . ? C71 C72 C71A 2.1(7) . . ? C73 C72 C71A 121.1(15) . . ? C73A C72 C71A 85.0(12) . . ? C72 C72A C71 126(3) . . ? C72 C72A C71A 136(3) . . ? C71 C72A C71A 10.9(12) . . ? C72 C72A C73A 99(3) . . ? C71 C72A C73A 133(2) . . ? C71A C72A C73A 121.7(16) . . ? C72 C72A C73 63(2) . . ? C71 C72A C73 169(2) . . ? C71A C72A C73 158.8(15) . . ? C73A C72A C73 37.3(11) . . ? C72 C72A C76 172(3) . . ? C71 C72A C76 52.5(14) . . ? C71A C72A C76 41.6(8) . . ? C73A C72A C76 80.7(13) . . ? C73 C72A C76 118.0(14) . . ? C73A C73 C74 29.8(19) . . ? C73A C73 C72 85(2) . . ? C74 C73 C72 114(2) . . ? C73A C73 C72A 60(2) . . ? C74 C73 C72A 89(2) . . ? C72 C73 C72A 25.2(9) . . ? C74 C73A C73 106(4) . . ? C74 C73A C74A 50(3) . . ? C73 C73A C74A 156(3) . . ? C74 C73A C72A 162(4) . . ? C73 C73A C72A 83(2) . . ? C74A C73A C72A 121(2) . . ? C74 C73A C72 162(4) . . ? C73 C73A C72 59.1(19) . . ? C74A C73A C72 145(2) . . ? C72A C73A C72 24.0(9) . . ? C74 C73A C75 66(3) . . ? C73 C73A C75 172(3) . . ? C74A C73A C75 17.7(12) . . ? C72A C73A C75 103.5(17) . . ? C72 C73A C75 127.5(17) . . ? C73A C74 C74A 95(4) . . ? C73A C74 C73 44(3) . . ? C74A C74 C73 139(3) . . ? C73A C74 C75 88(4) . . ? C74A C74 C75 10.4(17) . . ? C73 C74 C75 132(3) . . ? C75 C74A C74 153(4) . . ? C75 C74A C73A 124(4) . . ? C74 C74A C73A 35(2) . . ? C75 C74A C75A 11(2) . . ? C74 C74A C75A 156(3) . . ? C73A C74A C75A 122.6(19) . . ? C75 C74A C76 45(3) . . ? C74 C74A C76 113(2) . . ? C73A C74A C76 79.3(15) . . ? C75A C74A C76 43.8(9) . . ? C74A C75 C75A 162(4) . . ? C74A C75 C74 16(3) . . ? C75A C75 C74 162(2) . . ? C74A C75 C76 118(3) . . ? C75A C75 C76 59.1(14) . . ? C74 C75 C76 105.5(17) . . ? C74A C75 C73A 38(3) . . ? C75A C75 C73A 137(2) . . ? C74 C75 C73A 25.4(12) . . ? C76 C75 C73A 80.6(13) . . ? C74A C75 C76A 137(3) . . ? C75A C75 C76A 38.6(12) . . ? C74 C75 C76A 125.5(16) . . ? C76 C75 C76A 20.5(7) . . ? C73A C75 C76A 100.3(12) . . ? C75 C75A C76 81.8(17) . . ? C75 C75A C76A 116.0(18) . . ? C76 C75A C76A 34.2(8) . . ? C75 C75A C74A 7.1(15) . . ? C76 C75A C74A 81.6(12) . . ? C76A C75A C74A 115.5(13) . . ? C76A C76 C71A 91.2(19) . . ? C76A C76 C75A 79.2(17) . . ? C71A C76 C75A 165.5(16) . . ? C76A C76 C71 115(2) . . ? C71A C76 C71 24.1(8) . . ? C75A C76 C71 160.5(16) . . ? C76A C76 C75 118(2) . . ? C71A C76 C75 148.6(17) . . ? C75A C76 C75 39.1(9) . . ? C71 C76 C75 124.8(16) . . ? C76A C76 C72A 144(2) . . ? C71A C76 C72A 54.0(9) . . ? C75A C76 C72A 133.0(14) . . ? C71 C76 C72A 29.9(7) . . ? C75 C76 C72A 95.1(13) . . ? C76A C76 C74A 133.3(19) . . ? C71A C76 C74A 132.2(15) . . ? C75A C76 C74A 54.6(10) . . ? C71 C76 C74A 108.6(13) . . ? C75 C76 C74A 16.4(9) . . ? C72A C76 C74A 78.9(10) . . ? C76 C76A C71A 54.3(15) . . ? C76 C76A C75A 66.6(16) . . ? C71A C76A C75A 119.9(12) . . ? C76 C76A C71 42.0(15) . . ? C71A C76A C71 12.5(6) . . ? C75A C76A C71 107.4(11) . . ? C76 C76A C75 41.2(15) . . ? C71A C76A C75 94.9(10) . . ? C75A C76A C75 25.4(8) . . ? C71 C76A C75 82.4(9) . . ? C82A C81 C86 121.4(7) . . ? C82A C81 C82 28.0(2) . . ? C86 C81 C82 117.3(6) . . ? C82A C81 P4 114.3(6) . . ? C86 C81 P4 120.7(5) . . ? C82 C81 P4 121.3(5) . . ? C82A C82 C83A 80.3(7) . . ? C82A C82 C83 111.1(7) . . ? C83A C82 C83 31.3(3) . . ? C82A C82 C81 66.5(5) . . ? C83A C82 C81 113.0(8) . . ? C83 C82 C81 120.0(8) . . ? C82 C82A C81 85.5(5) . . ? C82 C82A C83A 70.9(7) . . ? C81 C82A C83A 116.8(8) . . ? C82 C82A C83 48.0(5) . . ? C81 C82A C83 104.8(7) . . ? C83A C82A C83 23.4(3) . . ? C83A C83 C84 96.4(8) . . ? C83A C83 C82 68.5(7) . . ? C84 C83 C82 121.4(10) . . ? C83A C83 C84A 69.9(7) . . ? C84 C83 C84A 27.0(3) . . ? C82 C83 C84A 105.0(9) . . ? C83A C83 C82A 48.0(5) . . ? C84 C83 C82A 113.5(10) . . ? C82 C83 C82A 20.9(2) . . ? C84A C83 C82A 91.1(8) . . ? C83 C83A C82 80.2(7) . . ? C83 C83A C82A 108.5(7) . . ? C82 C83A C82A 28.7(2) . . ? C83 C83A C84A 81.3(8) . . ? C82 C83A C84A 113.9(9) . . ? C82A C83A C84A 112.5(9) . . ? C83 C83A C84 56.4(6) . . ? C82 C83A C84 109.4(9) . . ? C82A C83A C84 121.5(9) . . ? C84A C83A C84 25.4(2) . . ? C84A C84 C83 90.6(8) . . ? C84A C84 C85 62.5(6) . . ? C83 C84 C85 118.1(10) . . ? C84A C84 C83A 63.8(6) . . ? C83 C84 C83A 27.2(3) . . ? C85 C84 C83A 106.1(9) . . ? C84 C84A C85 88.7(7) . . ? C84 C84A C83A 90.8(8) . . ? C85 C84A C83A 127.2(9) . . ? C84 C84A C83 62.4(7) . . ? C85 C84A C83 117.2(10) . . ? C83A C84A C83 28.8(3) . . ? C84A C85 C86 111.9(9) . . ? C84A C85 C84 28.8(3) . . ? C86 C85 C84 120.6(8) . . ? C81 C86 C85 121.7(7) . . ? C92 C91 C96 118.5(6) . . ? C92 C91 P5 119.4(4) . . ? C96 C91 P5 122.1(5) . . ? C91 C92 C93 121.7(6) . . ? C94 C93 C92 120.1(7) . . ? C93 C94 C95 119.0(8) . . ? C96 C95 C94 121.2(9) . . ? C91 C96 C95 119.5(8) . . ? C102 C101 C106 118.5(5) . . ? C102 C101 P5 120.1(4) . . ? C106 C101 P5 121.3(4) . . ? C103 C102 C101 119.7(6) . . ? C102 C103 C104 121.4(6) . . ? C105 C104 C103 119.7(6) . . ? C104 C105 C106 120.0(6) . . ? C105 C106 C101 120.6(5) . . ? C116 C111 C112 119.5(6) . . ? C116 C111 P6 120.3(4) . . ? C112 C111 P6 120.2(5) . . ? C111 C112 C113 119.9(7) . . ? C114 C113 C112 120.4(7) . . ? C113 C114 C115 120.2(6) . . ? C114 C115 C116 120.4(7) . . ? C111 C116 C115 119.5(6) . . ? C126 C121 C122 117.7(7) . . ? C126 C121 C127 107.9(10) . . ? C122 C121 C127 37.4(8) . . ? C126 C121 C129 40.1(10) . . ? C122 C121 C129 99.9(12) . . ? C127 C121 C129 116.7(14) . . ? C126 C121 P6 121.2(6) . . ? C122 C121 P6 121.0(5) . . ? C127 C121 P6 119.2(9) . . ? C129 C121 P6 123.8(11) . . ? C127 C122 C121 72.1(15) . . ? C127 C122 C123 88.8(16) . . ? C121 C122 C123 119.9(9) . . ? C127 C122 C128 58.9(16) . . ? C121 C122 C128 108.8(11) . . ? C123 C122 C128 30.1(9) . . ? C128 C123 C124 79(2) . . ? C128 C123 C122 89(2) . . ? C124 C123 C122 121.8(11) . . ? C128 C123 C127 56(2) . . ? C124 C123 C127 106.4(11) . . ? C122 C123 C127 32.9(7) . . ? C128 C123 C130 102(2) . . ? C124 C123 C130 37.2(10) . . ? C122 C123 C130 92.9(12) . . ? C127 C123 C130 95.0(13) . . ? C123 C124 C130 103.0(17) . . ? C123 C124 C125 120.1(10) . . ? C130 C124 C125 40.5(14) . . ? C123 C124 C128 34.3(10) . . ? C130 C124 C128 120.7(19) . . ? C125 C124 C128 112.6(13) . . ? C130 C125 C126 96(2) . . ? C130 C125 C124 59(2) . . ? C126 C125 C124 118.3(11) . . ? C130 C125 C129 62(2) . . ? C126 C125 C129 34.7(9) . . ? C124 C125 C129 100.8(12) . . ? C129 C126 C121 69.2(17) . . ? C129 C126 C125 89.1(18) . . ? C121 C126 C125 121.8(10) . . ? C129 C126 C130 57.4(19) . . ? C121 C126 C130 101.4(12) . . ? C125 C126 C130 32.1(10) . . ? C122 C127 C128 87(2) . . ? C122 C127 C121 70.6(15) . . ? C128 C127 C121 122.8(18) . . ? C122 C127 C123 58.4(14) . . ? C128 C127 C123 29.2(11) . . ? C121 C127 C123 104.6(13) . . ? C123 C128 C127 94(3) . . ? C123 C128 C124 66(2) . . ? C127 C128 C124 117(2) . . ? C123 C128 C122 61(2) . . ? C127 C128 C122 33.8(10) . . ? C124 C128 C122 103.7(17) . . ? C126 C129 C130 90(2) . . ? C126 C129 C121 70.6(17) . . ? C130 C129 C121 118(2) . . ? C126 C129 C125 56.2(15) . . ? C130 C129 C125 34.0(13) . . ? C121 C129 C125 105.2(17) . . ? C125 C130 C124 80(3) . . ? C125 C130 C129 84(3) . . ? C124 C130 C129 123(3) . . ? C125 C130 C126 51.8(18) . . ? C124 C130 C126 106(2) . . ? C129 C130 C126 32.7(12) . . ? C125 C130 C123 102(3) . . ? C124 C130 C123 39.8(11) . . ? C129 C130 C123 91.9(19) . . ? C126 C130 C123 93.7(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.007 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.092