#------------------------------------------------------------------------------ #$Date: 2014-07-11 17:35:18 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/00/40/1004003.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1004003 loop_ _publ_author_name 'Laurie I. Hill' 'Song Jin' 'Ran Zhou' 'D. Venkataraman' 'Francis J. DiSalvo' _publ_section_title ; Synthesis and Characterization of Oxidized W6S8L6 Clusters ; _journal_name_full 'Inorganic Chemistry' _journal_volume 40 _journal_page_first 2660 _journal_page_last 2665 _journal_year 2001 _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H90 F6 O2 P7 S8 W6' _chemical_formula_weight 2341.53 _chemical_melting_point ? _chemical_compound_source ? _space_group_IT_number 148 _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' 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' 'F' 'F' 0.0171 0.0103 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 13.91170(10) _cell_length_b 13.91170(10) _cell_length_c 32.4106(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5432.23(6) _cell_formula_units_Z 3 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_diffrn 2.147 _exptl_crystal_density_method ? _exptl_crystal_F_000 3303 _exptl_absorpt_coefficient_mu 9.922 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Insert the systematic name here ; _diffrn_ambient_temperature 163(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 'Bruker SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11328 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.09 _reflns_number_total 2723 _reflns_number_observed 2467 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0104P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2723 _refine_ls_number_parameters 104 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_obs 0.0451 _refine_ls_wR_factor_all 0.0774 _refine_ls_wR_factor_obs 0.0755 _refine_ls_goodness_of_fit_all 2.052 _refine_ls_goodness_of_fit_obs 2.105 _refine_ls_restrained_S_all 2.057 _refine_ls_restrained_S_obs 2.110 _refine_ls_shift/esd_max -0.034 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.28989(2) 0.54026(2) 0.132895(6) 0.02091(10) Uani 1 d D . S1 S 0.3333 0.6667 0.07405(6) 0.0219(5) Uani 1 d S . S2 S 0.4846(2) 0.5877(2) 0.13580(5) 0.0438(5) Uani 1 d . . P1 P 0.2390(2) 0.37547(15) 0.08644(5) 0.0474(6) Uani 1 d D . P2 P 0.6667 0.3333 0.3333 0.0268(8) Uani 1 d S . C1 C 0.3335(13) 0.4151(13) 0.0458(4) 0.044(4) Uiso 0.478(6) d PD 1 H1A H 0.3680(13) 0.3707(13) 0.0542(4) 0.052 Uiso 0.478(6) calc PR 1 H1B H 0.2796(13) 0.3688(13) 0.0243(4) 0.052 Uiso 0.478(6) calc PR 1 C2 C 0.4066(12) 0.4771(13) 0.0226(4) 0.041(4) Uiso 0.478(6) d PD 1 H2A H 0.4224(12) 0.4335(13) 0.0028(4) 0.061 Uiso 0.478(6) calc PR 1 H2B H 0.4738(12) 0.5251(13) 0.0385(4) 0.061 Uiso 0.478(6) calc PR 1 H2C H 0.3828(12) 0.5229(13) 0.0077(4) 0.061 Uiso 0.478(6) calc PR 1 C3 C 0.1005(10) 0.3415(11) 0.0531(3) 0.030(3) Uiso 0.478(6) d PD 1 H3A H 0.1054(10) 0.4125(11) 0.0451(3) 0.036 Uiso 0.478(6) calc PR 1 H3B H 0.0998(10) 0.3026(11) 0.0275(3) 0.036 Uiso 0.478(6) calc PR 1 C4 C -0.0105(12) 0.2697(12) 0.0762(4) 0.039(4) Uiso 0.478(6) d PD 1 H4A H -0.0725(12) 0.2571(12) 0.0583(4) 0.058 Uiso 0.478(6) calc PR 1 H4B H -0.0118(12) 0.3082(12) 0.1013(4) 0.058 Uiso 0.478(6) calc PR 1 H4C H -0.0174(12) 0.1982(12) 0.0836(4) 0.058 Uiso 0.478(6) calc PR 1 C5 C 0.1971(12) 0.2475(12) 0.1053(4) 0.039(3) Uiso 0.478(6) d PD 1 H5A H 0.1361(12) 0.2261(12) 0.1254(4) 0.046 Uiso 0.478(6) calc PR 1 H5B H 0.1702(12) 0.1923(12) 0.0827(4) 0.046 Uiso 0.478(6) calc PR 1 C6 C 0.2962(15) 0.2520(16) 0.1261(5) 0.061(5) Uiso 0.478(6) d PD 1 H6A H 0.2751(15) 0.1789(16) 0.1375(5) 0.092 Uiso 0.478(6) calc PR 1 H6B H 0.3220(15) 0.3069(16) 0.1484(5) 0.092 Uiso 0.478(6) calc PR 1 H6C H 0.3559(15) 0.2732(16) 0.1059(5) 0.092 Uiso 0.478(6) calc PR 1 C1' C 0.2803(11) 0.4025(10) 0.0339(3) 0.031(3) Uiso 0.522(6) d PD 2 H1'A H 0.2176(11) 0.3975(10) 0.0178(3) 0.037 Uiso 0.522(6) calc PR 2 H1'B H 0.3423(11) 0.4799(10) 0.0318(3) 0.037 Uiso 0.522(6) calc PR 2 C2' C 0.3178(14) 0.3251(13) 0.0131(5) 0.054(4) Uiso 0.522(6) d PD 2 H2'A H 0.3385(14) 0.3478(13) -0.0156(5) 0.081 Uiso 0.522(6) calc PR 2 H2'B H 0.2566(14) 0.2481(13) 0.0140(5) 0.081 Uiso 0.522(6) calc PR 2 H2'C H 0.3818(14) 0.3309(13) 0.0280(5) 0.081 Uiso 0.522(6) calc PR 2 C3' C 0.1071(10) 0.2632(11) 0.0900(3) 0.035(3) Uiso 0.522(6) d PD 2 H3'A H 0.0544(10) 0.2872(11) 0.0809(3) 0.042 Uiso 0.522(6) calc PR 2 H3'B H 0.1011(10) 0.2062(11) 0.0703(3) 0.042 Uiso 0.522(6) calc PR 2 C4' C 0.0694(13) 0.2089(13) 0.1315(4) 0.048(4) Uiso 0.522(6) d PD 2 H4'A H -0.0067(13) 0.1465(13) 0.1294(4) 0.072 Uiso 0.522(6) calc PR 2 H4'B H 0.0717(13) 0.2630(13) 0.1514(4) 0.072 Uiso 0.522(6) calc PR 2 H4'C H 0.1186(13) 0.1817(13) 0.1408(4) 0.072 Uiso 0.522(6) calc PR 2 C5' C 0.3293(12) 0.3017(11) 0.1040(4) 0.041(3) Uiso 0.522(6) d PD 2 H5'A H 0.4091(12) 0.3585(11) 0.1040(4) 0.049 Uiso 0.522(6) calc PR 2 H5'B H 0.3085(12) 0.2738(11) 0.1326(4) 0.049 Uiso 0.522(6) calc PR 2 C6' C 0.3119(13) 0.2052(12) 0.0761(4) 0.051(4) Uiso 0.522(6) d PD 2 H6'A H 0.3571(13) 0.1742(12) 0.0862(4) 0.076 Uiso 0.522(6) calc PR 2 H6'B H 0.3342(13) 0.2324(12) 0.0478(4) 0.076 Uiso 0.522(6) calc PR 2 H6'C H 0.2334(13) 0.1476(12) 0.0764(4) 0.076 Uiso 0.522(6) calc PR 2 F1 F 0.6667 0.3333 0.3825(2) 0.053(2) Uiso 1 d S . F2 F 0.7872(15) 0.4432(16) 0.3339(5) 0.050(3) Uiso 0.33 d P . F3 F 0.6087(22) 0.4076(20) 0.3391(4) 0.047(3) Uiso 0.33 d P . C1S C 0.6625(44) 0.3876(32) 0.1108(8) 0.199(14) Uiso 0.67 d PD . C2S C 0.6138(33) 0.3827(33) 0.0738(9) 0.203(15) Uiso 0.67 d PD . O1S O 0.7016(40) 0.3955(29) 0.0474(10) 0.178(16) Uiso 0.33 d PD . 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 0.0301(2) 0.01441(13) 0.01617(13) -0.00141(8) 0.00024(8) 0.00956(11) S1 0.0250(8) 0.0250(8) 0.0155(10) 0.000 0.000 0.0125(4) S2 0.0597(12) 0.0826(15) 0.0245(8) -0.0067(8) -0.0026(7) 0.0621(12) P1 0.0624(14) 0.0208(9) 0.0339(9) -0.0104(7) 0.0162(9) 0.0019(9) P2 0.0248(13) 0.0248(13) 0.031(2) 0.000 0.000 0.0124(6) 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 S2 2.446(2) 3_565 ? W1 S2 2.449(2) . ? W1 S2 2.4508(15) 14_455 ? W1 S1 2.456(2) . ? W1 P1 2.530(2) . ? W1 W1 2.6803(4) 2_665 ? W1 W1 2.6803(4) 3_565 ? W1 W1 2.6809(3) 15 ? W1 W1 2.6809(3) 14_455 ? S1 W1 2.456(2) 3_565 ? S1 W1 2.456(2) 2_665 ? S2 W1 2.446(2) 2_665 ? S2 W1 2.4509(15) 15 ? P1 C5 1.687(14) . ? P1 C3' 1.718(12) . ? P1 C1 1.744(14) . ? P1 C1' 1.775(11) . ? P1 C3 2.047(12) . ? P1 C5' 2.061(13) . ? P2 F1 1.593(7) 16_655 ? P2 F1 1.593(7) . ? P2 F2 1.608(14) 3_665 ? P2 F2 1.608(14) 17 ? P2 F2 1.608(14) . ? P2 F2 1.608(14) 16_655 ? P2 F2 1.608(14) 18_545 ? P2 F2 1.608(14) 2_655 ? P2 F3 1.608(14) 3_665 ? P2 F3 1.608(14) 2_655 ? P2 F3 1.608(14) 16_655 ? P2 F3 1.608(14) 17 ? C1 C2 1.21(2) . ? C3 C4 1.55(2) . ? C5 C6 1.51(2) . ? C1' C2' 1.56(2) . ? C3' C4' 1.503(15) . ? C5' C6' 1.53(2) . ? F2 F3 0.834(15) 3_665 ? F2 F3 0.867(15) 17 ? F2 F2 1.608(14) 18_545 ? F2 F2 1.608(14) 17 ? F3 F2 0.83(2) 2_655 ? F3 F2 0.867(15) 18_545 ? F3 F3 1.641(15) 18_545 ? F3 F3 1.641(15) 17 ? C1S C1S 1.36(5) 2_655 ? C1S C1S 1.36(5) 3_665 ? C1S C2S 1.36(3) . ? C1S C2S 1.91(5) 3_665 ? C2S O1S 1.32(5) 2_655 ? C2S O1S 1.43(4) . ? C2S C1S 1.91(5) 2_655 ? O1S O1S 1.30(6) 2_655 ? O1S O1S 1.30(6) 3_665 ? O1S C2S 1.32(5) 3_665 ? 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 S2 W1 S2 172.18(5) 3_565 . ? S2 W1 S2 89.81(4) 3_565 14_455 ? S2 W1 S2 89.76(4) . 14_455 ? S2 W1 S1 89.71(4) 3_565 . ? S2 W1 S1 89.65(4) . . ? S2 W1 S1 172.20(5) 14_455 . ? S2 W1 P1 95.64(7) 3_565 . ? S2 W1 P1 92.17(7) . . ? S2 W1 P1 95.28(6) 14_455 . ? S1 W1 P1 92.51(5) . . ? S2 W1 W1 116.79(5) 3_565 2_665 ? S2 W1 W1 56.76(5) . 2_665 ? S2 W1 W1 116.68(5) 14_455 2_665 ? S1 W1 W1 56.93(2) . 2_665 ? P1 W1 W1 132.84(4) . 2_665 ? S2 W1 W1 56.84(5) 3_565 3_565 ? S2 W1 W1 116.71(5) . 3_565 ? S2 W1 W1 116.73(4) 14_455 3_565 ? S1 W1 W1 56.93(2) . 3_565 ? P1 W1 W1 135.31(6) . 3_565 ? W1 W1 W1 60.0 2_665 3_565 ? S2 W1 W1 116.82(4) 3_565 15 ? S2 W1 W1 56.87(4) . 15 ? S2 W1 W1 56.72(5) 14_455 15 ? S1 W1 W1 116.89(3) . 15 ? P1 W1 W1 134.61(6) . 15 ? W1 W1 W1 60.007(5) 2_665 15 ? W1 W1 W1 90.0 3_565 15 ? S2 W1 W1 56.89(4) 3_565 14_455 ? S2 W1 W1 116.80(4) . 14_455 ? S2 W1 W1 56.78(4) 14_455 14_455 ? S1 W1 W1 116.89(3) . 14_455 ? P1 W1 W1 137.15(4) . 14_455 ? W1 W1 W1 90.0 2_665 14_455 ? W1 W1 W1 60.006(5) 3_565 14_455 ? W1 W1 W1 59.985(10) 15 14_455 ? W1 S1 W1 66.14(5) 3_565 2_665 ? W1 S1 W1 66.14(5) 3_565 . ? W1 S1 W1 66.14(5) 2_665 . ? W1 S2 W1 66.40(4) 2_665 . ? W1 S2 W1 66.38(4) 2_665 15 ? W1 S2 W1 66.35(4) . 15 ? C5 P1 C1 114.5(7) . . ? C3' P1 C1' 110.1(6) . . ? C5 P1 C3 99.2(6) . . ? C1 P1 C3 98.6(6) . . ? C3' P1 C5' 99.7(6) . . ? C1' P1 C5' 99.0(5) . . ? C5 P1 W1 122.2(5) . . ? C3' P1 W1 118.1(4) . . ? C1 P1 W1 109.7(5) . . ? C1' P1 W1 117.7(4) . . ? C3 P1 W1 109.2(4) . . ? C5' P1 W1 108.8(4) . . ? F1 P2 F1 180.0 16_655 . ? F1 P2 F2 90.7(5) 16_655 3_665 ? F1 P2 F2 89.3(5) . 3_665 ? F1 P2 F2 89.3(5) 16_655 17 ? F1 P2 F2 90.7(5) . 17 ? F2 P2 F2 60.01(3) 3_665 17 ? F1 P2 F2 90.7(5) 16_655 . ? F1 P2 F2 89.3(5) . . ? F2 P2 F2 119.99(2) 3_665 . ? F2 P2 F2 60.02(3) 17 . ? F1 P2 F2 89.3(5) 16_655 16_655 ? F1 P2 F2 90.7(5) . 16_655 ? F2 P2 F2 60.01(2) 3_665 16_655 ? F2 P2 F2 119.98(3) 17 16_655 ? F2 P2 F2 179.996(2) . 16_655 ? F1 P2 F2 89.3(5) 16_655 18_545 ? F1 P2 F2 90.7(5) . 18_545 ? F2 P2 F2 179.997(7) 3_665 18_545 ? F2 P2 F2 119.99(2) 17 18_545 ? F2 P2 F2 60.01(2) . 18_545 ? F2 P2 F2 119.99(2) 16_655 18_545 ? F1 P2 F2 90.7(5) 16_655 2_655 ? F1 P2 F2 89.3(5) . 2_655 ? F2 P2 F2 119.99(2) 3_665 2_655 ? F2 P2 F2 179.997(8) 17 2_655 ? F2 P2 F2 119.99(3) . 2_655 ? F2 P2 F2 60.02(3) 16_655 2_655 ? F2 P2 F2 60.02(3) 18_545 2_655 ? F1 P2 F3 96.7(4) 16_655 3_665 ? F1 P2 F3 83.3(4) . 3_665 ? F2 P2 F3 90.4(6) 3_665 3_665 ? F2 P2 F3 31.3(5) 17 3_665 ? F2 P2 F3 30.1(5) . 3_665 ? F2 P2 F3 149.9(5) 16_655 3_665 ? F2 P2 F3 89.6(6) 18_545 3_665 ? F2 P2 F3 148.7(5) 2_655 3_665 ? F1 P2 F3 96.7(4) 16_655 2_655 ? F1 P2 F3 83.3(4) . 2_655 ? F2 P2 F3 30.1(5) 3_665 2_655 ? F2 P2 F3 89.6(6) 17 2_655 ? F2 P2 F3 148.7(5) . 2_655 ? F2 P2 F3 31.3(5) 16_655 2_655 ? F2 P2 F3 149.9(5) 18_545 2_655 ? F2 P2 F3 90.4(6) 2_655 2_655 ? F3 P2 F3 118.7(2) 3_665 2_655 ? F1 P2 F3 83.3(4) 16_655 16_655 ? F1 P2 F3 96.7(4) . 16_655 ? F2 P2 F3 31.3(5) 3_665 16_655 ? F2 P2 F3 30.1(5) 17 16_655 ? F2 P2 F3 89.6(6) . 16_655 ? F2 P2 F3 90.4(6) 16_655 16_655 ? F2 P2 F3 148.7(5) 18_545 16_655 ? F2 P2 F3 149.9(5) 2_655 16_655 ? F3 P2 F3 61.3(2) 3_665 16_655 ? F3 P2 F3 61.3(2) 2_655 16_655 ? F1 P2 F3 83.3(4) 16_655 17 ? F1 P2 F3 96.7(4) . 17 ? F2 P2 F3 149.9(5) 3_665 17 ? F2 P2 F3 90.4(6) 17 17 ? F2 P2 F3 31.3(5) . 17 ? F2 P2 F3 148.7(5) 16_655 17 ? F2 P2 F3 30.1(5) 18_545 17 ? F2 P2 F3 89.6(6) 2_655 17 ? F3 P2 F3 61.3(2) 3_665 17 ? F3 P2 F3 179.996(5) 2_655 17 ? F3 P2 F3 118.7(2) 16_655 17 ? C2 C1 P1 157.8(14) . . ? C4 C3 P1 114.4(8) . . ? C6 C5 P1 107.0(11) . . ? C2' C1' P1 116.9(9) . . ? C4' C3' P1 117.6(9) . . ? C6' C5' P1 113.8(9) . . ? F3 F2 F3 149.3(32) 3_665 17 ? F3 F2 P2 75.0(16) 3_665 . ? F3 F2 P2 74.4(16) 17 . ? F3 F2 F2 133.7(16) 3_665 18_545 ? F3 F2 F2 18.7(13) 17 18_545 ? P2 F2 F2 59.992(14) . 18_545 ? F3 F2 F2 19.4(14) 3_665 17 ? F3 F2 F2 132.0(16) 17 17 ? P2 F2 F2 59.99(2) . 17 ? F2 F2 F2 119.94(10) 18_545 17 ? F2 F3 F2 141.9(27) 2_655 18_545 ? F2 F3 P2 74.9(16) 2_655 . ? F2 F3 P2 74.3(16) 18_545 . ? F2 F3 F3 15.7(16) 2_655 18_545 ? F2 F3 F3 128.3(16) 18_545 18_545 ? P2 F3 F3 59.33(9) . 18_545 ? F2 F3 F3 129.7(17) 2_655 17 ? F2 F3 F3 15.0(16) 18_545 17 ? P2 F3 F3 59.33(8) . 17 ? F3 F3 F3 114.9(6) 18_545 17 ? C1S C1S C1S 60.000(6) 2_655 3_665 ? C1S C1S C2S 89.2(37) 2_655 . ? C1S C1S C2S 113.8(20) 3_665 . ? C1S C1S C2S 86.6(25) 2_655 3_665 ? C1S C1S C2S 45.4(21) 3_665 3_665 ? C2S C1S C2S 79.3(27) . 3_665 ? O1S C2S C1S 117.2(37) 2_655 . ? O1S C2S O1S 56.4(32) 2_655 . ? C1S C2S O1S 98.5(32) . . ? O1S C2S C1S 79.3(25) 2_655 2_655 ? C1S C2S C1S 45.3(24) . 2_655 ? O1S C2S C1S 98.4(31) . 2_655 ? O1S O1S O1S 60.000(9) 2_655 3_665 ? O1S O1S C2S 110.8(29) 2_655 3_665 ? O1S O1S C2S 66.0(33) 3_665 3_665 ? O1S O1S C2S 57.7(32) 2_655 . ? O1S O1S C2S 104.4(29) 3_665 . ? C2S O1S C2S 101.8(35) 3_665 . ? _refine_diff_density_max 1.665 _refine_diff_density_min -1.526 _refine_diff_density_rms 0.218 _cod_database_code 1004003 _journal_paper_doi 10.1021/ic001099d