# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2161 data_rxd10 _audit_creation_date 98-11-02 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ; 2000-05-19 acw edits default cif 2000-05-19 passes checkcif tests with minor warnings ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_moiety ' C22 H32 As4 Cl2 Co +, F6 P -, 0.3333(C4 H10 O), 0.3333(H2 O) ' _chemical_formula_structural ? _chemical_formula_sum ' C23.333 H36 As4 Cl2 Co F6 O0.666 P ' _chemical_formula_weight 901.70 _chemical_melting_point ? _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 21.231(2) _cell_length_b 21.231(2) _cell_length_c 18.627(3) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 120.000 _cell_volume 7271.3(18) _cell_formula_units_Z 9 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 47.34 _cell_measurement_theta_max 53.28 _cell_special_details ; ? ; _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M r_3:h _symmetry_space_group_name_Hall r_3 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -y,+x-y,+z -x+y,-x,+z 2/3+x,1/3+y,1/3+z 1/3+x,2/3+y,2/3+z 2/3-y,1/3+x-y,1/3+z 1/3-y,2/3+x-y,2/3+z 2/3-x+y,1/3-x,1/3+z 1/3-x+y,2/3-x,2/3+z _exptl_crystal_description 'needle' _exptl_crystal_preparation ? _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 3990 _exptl_absorpt_coefficient_mu 11.17 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min .222 _exptl_absorpt_correction_T_max .564 _exptl_special_details ; The scan width was (1.2+0.30tan\q)\% with an \w scan speed of 32\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0. loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 7345 _diffrn_reflns_av_R_equivalents .048 _diffrn_reflns_av_sigmaI/netI .047 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 60.01 _diffrn_reflns_reduction_process equatorial_monochr_Lp loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 210 .017 .009 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; H ? 0 324 0 0 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; As ? 0 36 -1.011 1.006 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; Cl ? 0 18 .348 .702 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; Co ? 0 9 -2.464 3.608 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; F ? 0 54 .069 .053 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; O ? 0 6 .047 .032 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; P ? 0 9 .283 .434 ;Int. Tables Vol_IV Tables_2.2B_and_2.3.1 ; 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 _atom_site_occupancy As1 .14775(6) .28465(6) .25000 .0462(6) Uani ? ? 1 As2 .24022(6) .25070(6) .33763(9) .0466(6) Uani ? ? 1 As3 .20639(6) .38683(6) .38973(9) .0453(5) Uani ? ? 1 As4 .37165(6) .44025(6) .35725(9) .0445(5) Uani ? ? 1 Co1 .26294(8) .36388(9) .29435(11) .0409(7) Uani ? ? 1 Cl1 .26771(17) .45938(16) .23657(17) .0607(15) Uani ? ? 1 Cl2 .33427(15) .35172(15) .21278(16) .0548(13) Uani ? ? 1 C1 .0999(7) .3146(8) .1823(7) .067(7) Uani ? ? 1 C2 .1564(5) .2058(6) .2117(6) .048(5) Uani ? ? 1 C3 .1235(7) .1654(7) .1519(6) .065(6) Uani ? ? 1 C4 .1342(8) .1073(8) .1341(8) .080(8) Uani ? ? 1 C5 .1820(9) .0940(7) .1754(8) .080(8) Uani ? ? 1 C6 .2126(8) .1312(7) .2338(7) .070(7) Uani ? ? 1 C7 .2015(6) .1895(5) .2527(6) .049(5) Uani ? ? 1 C8 .3094(7) .2258(7) .3767(7) .064(7) Uani ? ? 1 C9 .1544(7) .2002(7) .4009(6) .065(7) Uani ? ? 1 C10 .1007(6) .2294(6) .4007(6) .056(6) Uani ? ? 1 C11 .0751(6) .2344(6) .3251(6) .056(5) Uani ? ? 1 C12 .0345(8) .1754(8) .4458(7) .081(7) Uani ? ? 1 C13 .1339(7) .3031(7) .4428(6) .064(6) Uani ? ? 1 C14 .1563(7) .4387(8) .3703(7) .073(8) Uani ? ? 1 C15 .2768(6) .4474(6) .4613(5) .047(5) Uani ? ? 1 C16 .2551(6) .4672(7) .5213(7) .066(7) Uani ? ? 1 C17 .3089(8) .5091(8) .5715(7) .078(8) Uani ? ? 1 C18 .3808(8) .5365(8) .5581(7) .077(8) Uani ? ? 1 C19 .3998(7) .5157(7) .4957(6) .066(7) Uani ? ? 1 C20 .3490(5) .4715(6) .4472(6) .046(5) Uani ? ? 1 C21 .4385(7) .4072(8) .3863(7) .070(7) Uani ? ? 1 C22 .4356(6) .5288(7) .3082(7) .067(6) Uani ? ? 1 P1 .0666(2) .40847(18) .6466(2) .0686(18) Uani ? ? 1 F1 .0919(7) .4479(6) .5737(5) .124(7) Uani ? ? 1 F2 .1356(8) .4122(12) .6573(10) .239(17) Uani ? ? 1 F3 .0875(11) .4788(6) .6845(7) .207(12) Uani ? ? 1 F4 .0390(12) .3672(7) .7170(6) .214(12) Uani ? ? 1 F5 -.0071(9) .4020(13) .6344(14) .30(2) Uani ? ? 1 F6 .0356(10) .3355(5) .6094(6) .166(9) Uani ? ? 1 O1a .00000 .00000 .300(4) .153(15) Uiso ? ? .58(6) O1b .00000 .00000 .350(5) .153(15) Uiso ? ? .42(6) O2 -.042(3) .004(3) .5040(18) .18(2) Uiso ? ? .333 C23 .014(2) .023(3) .5580(18) .103(19) Uiso ? ? .333 C24 -.0228(19) .000(2) .6296(17) .086(15) Uiso ? ? .333 C25 .0364(16) .022(3) .688(2) .17(3) Uiso ? ? .333 C26 .00000 .00000 .761(2) .19(2) Uiso ? ? 1. H1 .12724 .32975 .13908 .10000 Uiso ? ? 1. H2 .05261 .27506 .17247 .10000 Uiso ? ? 1 H3 .09599 .35392 .20173 .10000 Uiso ? ? 1 H4 .09381 .17665 .12262 .10000 Uiso ? ? 1 H5 .10932 .07687 .09433 .10000 Uiso ? ? 1 H6 .19233 .05729 .16050 .10000 Uiso ? ? 1 H7 .24180 .11926 .26301 .10000 Uiso ? ? 1 H8 .28495 .17586 .38961 .10000 Uiso ? ? 1 H9 .34540 .23491 .34156 .10000 Uiso ? ? 1 H10 .33179 .25483 .41790 .10000 Uiso ? ? 1 H11 .12827 .15062 .38664 .10000 Uiso ? ? 1 H12 .17151 .20349 .44865 .10000 Uiso ? ? 1 H13 .04780 .25858 .32934 .10000 Uiso ? ? 1 H14 .04420 .18601 .30891 .10000 Uiso ? ? 1 H15 .01257 .12858 .42425 .10000 Uiso ? ? 1 H16 .05007 .17293 .49297 .10000 Uiso ? ? 1 H17 .00016 .19165 .44791 .10000 Uiso ? ? 1 H18 .15601 .29850 .48527 .10000 Uiso ? ? 1 H19 .09545 .31173 .45521 .10000 Uiso ? ? 1 H20 .13274 .44134 .41261 .10000 Uiso ? ? 1 H21 .19023 .48644 .35443 .10000 Uiso ? ? 1 H22 .12113 .41410 .33372 .10000 Uiso ? ? 1 H23 .20555 .45318 .52898 .10000 Uiso ? ? 1 H24 .29461 .51879 .61664 .10000 Uiso ? ? 1 H25 .41682 .56886 .59082 .10000 Uiso ? ? 1 H26 .44968 .53263 .48623 .10000 Uiso ? ? 1 H27 .48106 .44661 .40659 .10000 Uiso ? ? 1 H28 .41545 .36946 .42079 .10000 Uiso ? ? 1 H29 .45136 .38920 .34546 .10000 Uiso ? ? 1 H30 .41128 .55523 .29928 .10000 Uiso ? ? 1 H31 .47731 .55706 .33717 .10000 Uiso ? ? 1 H32 .45022 .51767 .26400 .10000 Uiso ? ? 1 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 As1 .0413(6) .0520(7) .0431(7) .0216(6) -.0052(5) -.0008(5) As2 .0506(7) .0461(6) .0448(7) .0254(5) -.0055(6) .0004(5) As3 .0389(6) .0505(7) .0463(7) .0223(5) .0008(5) -.0044(5) As4 .0366(6) .0489(7) .0449(6) .0190(5) .0014(5) -.0020(5) Co1 .0381(8) .0436(9) .0410(8) .0204(8) .0002(7) .0014(7) Cl1 .0636(17) .0574(17) .0632(18) .0318(15) .0065(14) .0174(14) Cl2 .0550(15) .0573(17) .0497(16) .0263(14) .0093(13) -.0025(12) C1 .054(7) .090(10) .055(7) .035(7) -.022(6) .008(7) C2 .036(5) .059(7) .042(6) .017(5) -.008(5) -.004(5) C3 .060(8) .063(8) .050(7) .014(6) .003(6) -.002(6) C4 .082(10) .062(8) .070(9) .017(8) -.006(8) -.033(7) C5 .086(10) .053(8) .071(9) .014(7) .002(8) -.011(7) C6 .078(9) .051(7) .068(8) .022(7) -.001(7) .003(6) C7 .052(6) .032(5) .059(7) .017(5) .001(5) .006(5) C8 .060(7) .069(8) .085(9) .049(7) -.018(6) .002(7) C9 .072(8) .068(8) .043(7) .027(7) .010(6) .016(6) C10 .042(6) .049(6) .059(7) .008(5) .015(5) .000(5) C11 .040(6) .052(7) .051(7) .005(5) -.005(5) .001(5) C12 .062(8) .076(9) .061(8) .002(7) .014(7) .013(7) C13 .064(8) .067(8) .042(6) .019(6) .017(6) .003(6) C14 .052(7) .109(11) .080(9) .055(8) -.016(7) -.012(8) C15 .055(6) .067(7) .024(5) .036(6) .012(5) .007(5) C16 .044(6) .069(8) .074(8) .019(6) .002(6) -.027(7) C17 .083(10) .095(11) .058(8) .046(9) .000(7) -.012(8) C18 .062(8) .100(11) .069(9) .041(8) -.023(7) -.041(8) C19 .060(7) .071(8) .062(8) .030(7) -.019(6) -.019(7) C20 .039(6) .054(6) .042(6) .023(5) -.000(5) -.009(5) C21 .049(7) .077(9) .083(9) .030(7) .001(6) -.004(7) C22 .039(6) .066(8) .074(8) .009(6) .019(6) .013(7) P1 .072(2) .0516(18) .082(2) .0312(17) .023(2) .0073(17) F1 .170(11) .094(7) .119(7) .073(7) .017(7) .023(6) F2 .135(12) .35(3) .27(2) .149(15) -.032(13) .050(19) F3 .37(2) .061(6) .151(10) .077(10) .125(13) .017(7) F4 .39(2) .100(8) .116(9) .094(13) .125(13) .045(7) F5 .109(11) .30(3) .54(4) .137(15) .044(17) .04(2) F6 .296(18) .074(7) .111(8) .080(10) -.037(10) -.023(6) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details ; Weights derived from sig(I) = [sig^2^(Icount) + 0.0009I^2^]^0.5^ The asymmetric unit is comprised of one cation, one PF6- anion, and a chain of disordered solvate molecules running close to or on (0,0,z). One series of peaks was interpretted to be a n-butanol molecule disordered along the 3-fold axis, and the other a water moilecule disordered over two closely adjacent axial sites. Restraints were imposed upon distances and angles of the n-butanol molecule. Hydrogen atoms for the cation were included at calculated positions, those on solvate molecules were omitted. ; _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 .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; Absolute structure determined by comparative refinement. Refinement of a model with coordinates transformed by (-x,-y,-z) yielded R = 0.041, wR = 0.042, S = 1.518. ; _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 2104 _refine_ls_number_parameters 346 _refine_ls_number_restraints 9 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .043 _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_all .04 _refine_ls_wR_factor_ref .036 _refine_ls_goodness_of_fit_all 1.332 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_shift/su_max .064 _refine_ls_shift/su_mean .004 _refine_diff_density_min -.481 _refine_diff_density_max .534 _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 As1 Co1 2.3192(18) . . ? As1 C1 1.918(16) . . ? As1 C2 1.912(14) . . ? As1 C11 1.956(11) . . ? As1 C28 2.1791(10) . 9_554 ? As2 Co1 2.345(2) . . ? As2 C7 1.950(10) . . ? As2 C8 1.933(17) . . ? As2 C9 1.976(12) . . ? As3 Co1 2.328(3) . . ? As3 C13 1.941(11) . . ? As3 C14 1.91(2) . . ? As3 C15 1.935(9) . . ? As3 C35 1.0563(16) . 9_554 ? As4 Co1 2.364(2) . . ? As4 C20 1.948(12) . . ? As4 C21 1.949(18) . . ? As4 C22 1.912(12) . . ? As4 C31 1.0329(17) . 2_665 ? Co1 Cl1 2.253(4) . . ? Co1 Cl2 2.249(4) . . ? Co1 C28 .951(2) . 9_554 ? Co1 C35 1.282(2) . 9_554 ? Cl2 C28 1.759(4) . 9_554 ? C1 H1 .950(12) . . ? C1 H2 .950(11) . . ? C1 H3 .950(18) . . ? C2 C3 1.366(15) . . ? C2 C7 1.40(2) . . ? C3 C4 1.40(3) . . ? C3 H4 .950(17) . . ? C4 C5 1.41(3) . . ? C4 H5 .950(13) . . ? C5 C6 1.31(2) . . ? C5 H6 .95(2) . . ? C6 C7 1.41(2) . . ? C6 H7 .950(17) . . ? C8 H8 .950(13) . . ? C8 H9 .950(14) . . ? C8 H10 .950(12) . . ? C9 C10 1.55(2) . . ? C9 H11 .950(13) . . ? C9 H12 .950(12) . . ? C10 C11 1.532(17) . . ? C10 C12 1.544(16) . . ? C10 C13 1.568(18) . . ? C11 H13 .950(15) . . ? C11 H14 .950(10) . . ? C12 H15 .950(15) . . ? C12 H16 .950(14) . . ? C12 H17 .95(2) . . ? C13 H18 .950(13) . . ? C13 H19 .950(17) . . ? C14 H20 .950(15) . . ? C14 H21 .950(13) . . ? C14 H22 .950(12) . . ? C15 C16 1.353(19) . . ? C15 C20 1.378(17) . . ? C16 C17 1.398(17) . . ? C16 H23 .950(13) . . ? C17 C18 1.36(2) . . ? C17 H24 .950(15) . . ? C18 C19 1.37(2) . . ? C18 H25 .950(13) . . ? C19 C20 1.360(15) . . ? C19 H26 .950(14) . . ? C20 C31 .999(13) . 2_665 ? C21 H27 .950(11) . . ? C21 H28 .950(13) . . ? C21 H29 .950(16) . . ? C22 H30 .950(17) . . ? C22 H31 .950(11) . . ? C22 H32 .950(14) . . ? P1 F1 1.544(11) . . ? P1 F2 1.44(2) . . ? P1 F3 1.503(13) . . ? P1 F4 1.522(12) . . ? P1 F5 1.52(2) . . ? P1 F6 1.514(11) . . ? P1 C32 1.354(5) . . ? P1 C33 1.452(3) . . ? P1 C29 1.551(5) . 9_554 ? F1 C33 1.575(10) . . ? F2 C33 1.52(3) . . ? F2 C29 1.227(18) . 9_554 ? F3 C32 1.092(18) . . ? F3 C33 1.13(2) . . ? F4 C30 1.390(17) . 9 ? F4 C36 .589(14) . 9 ? F5 C32 1.10(2) . . ? F6 C29 1.189(18) . 9_554 ? O1a O1b .95(12) . . ? O1a C34 1.36(6) . 4_445 ? O1a C34 1.36(6) . 6 ? O1a C34 1.36(6) . 8_455 ? O1b C34 .74(3) . 4_445 ? O1b C34 .74(3) . 6 ? O1b C34 .74(3) . 8_455 ? O2 C23 1.45(6) . . ? O2 O2 1.63(15) . 2 ? O2 C23 1.17(8) . 2 ? O2 O2 1.63(13) . 3 ? O2 C23 1.67(11) . 3 ? C23 C24 1.50(5) . . ? C23 C23 .75(6) . 2 ? C23 C24 1.60(7) . 2 ? C23 C23 .75(9) . 3 ? C23 C24 1.35(5) . 3 ? C23 C27 .94(4) . 4_445 ? C24 C25 1.54(5) . . ? C24 C24 .84(10) . 2 ? C24 C25 1.12(6) . 2 ? C24 C24 .84(8) . 3 ? C24 C25 1.39(7) . 3 ? C24 C27 .70(4) . 4_445 ? C25 C26 1.52(5) . . ? C25 C25 1.17(9) . 2 ? C25 C25 1.17(6) . 3 ? C25 C27 1.72(4) . 4_445 ? C30 C36 1.26968(11) . . ? C34 C34 1.22621(11) . 2_665 ? C34 C34 1.22621(12) . 3_565 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 Co1 As1 C1 122.4(4) . . . ? Co1 As1 C2 103.9(3) . . . ? Co1 As1 C11 113.5(3) . . . ? Co1 As1 C28 24.14(5) . . 9_554 ? C1 As1 C2 110.2(6) . . . ? C1 As1 C11 104.3(6) . . . ? C1 As1 C28 106.2(3) . . 9_554 ? C2 As1 C11 100.6(5) . . . ? C2 As1 C28 95.7(3) . . 9_554 ? C11 As1 C28 137.7(3) . . 9_554 ? Co1 As2 C7 101.9(4) . . . ? Co1 As2 C8 127.9(3) . . . ? Co1 As2 C9 115.0(5) . . . ? C7 As2 C8 104.3(6) . . . ? C7 As2 C9 98.9(4) . . . ? C8 As2 C9 104.3(6) . . . ? Co1 As3 C13 116.9(5) . . . ? Co1 As3 C14 118.0(4) . . . ? Co1 As3 C15 110.9(4) . . . ? Co1 As3 C35 5.88(6) . . 9_554 ? C13 As3 C14 102.1(6) . . . ? C13 As3 C15 104.7(4) . . . ? C13 As3 C35 111.1(5) . . 9_554 ? C14 As3 C15 102.4(6) . . . ? C14 As3 C35 121.9(4) . . 9_554 ? C15 As3 C35 112.8(4) . . 9_554 ? Co1 As4 C20 109.7(3) . . . ? Co1 As4 C21 121.9(4) . . . ? Co1 As4 C22 114.1(4) . . . ? Co1 As4 C31 117.16(9) . . 2_665 ? C20 As4 C21 103.4(6) . . . ? C20 As4 C22 104.5(5) . . . ? C20 As4 C31 16.3(4) . . 2_665 ? C21 As4 C22 101.5(6) . . . ? C21 As4 C31 87.5(4) . . 2_665 ? C22 As4 C31 111.4(4) . . 2_665 ? As1 Co1 As2 77.12(6) . . . ? As1 Co1 As3 87.51(7) . . . ? As1 Co1 As4 171.11(10) . . . ? As1 Co1 Cl1 92.25(11) . . . ? As1 Co1 Cl2 101.68(10) . . . ? As1 Co1 C28 69.64(9) . . 9_554 ? As1 Co1 C35 85.40(8) . . 9_554 ? As2 Co1 As3 95.09(8) . . . ? As2 Co1 As4 99.35(9) . . . ? As2 Co1 Cl1 168.62(11) . . . ? As2 Co1 Cl2 85.41(12) . . . ? As2 Co1 C28 111.09(14) . . 9_554 ? As2 Co1 C35 90.37(10) . . 9_554 ? As3 Co1 As4 84.67(8) . . . ? As3 Co1 Cl1 88.40(13) . . . ? As3 Co1 Cl2 170.65(11) . . . ? As3 Co1 C28 139.27(18) . . 9_554 ? As3 Co1 C35 4.84(5) . . 9_554 ? As4 Co1 Cl1 91.74(10) . . . ? As4 Co1 Cl2 86.04(10) . . . ? As4 Co1 C28 119.19(11) . . 9_554 ? As4 Co1 C35 86.48(10) . . 9_554 ? Cl1 Co1 Cl2 92.90(14) . . . ? Cl1 Co1 C28 60.51(14) . . 9_554 ? Cl1 Co1 C35 92.83(15) . . 9_554 ? Cl2 Co1 C28 47.84(13) . . 9_554 ? Cl2 Co1 C35 170.71(16) . . 9_554 ? C28 Co1 C35 141.4(2) 9_554 . 9_554 ? Co1 Cl2 C28 23.62(7) . . 9_554 ? As1 C1 H1 109.4(13) . . . ? As1 C1 H2 109.5(12) . . . ? As1 C1 H3 109.5(9) . . . ? H1 C1 H2 109.4(12) . . . ? H1 C1 H3 109.5(15) . . . ? H2 C1 H3 109.5(16) . . . ? As1 C2 C3 127.7(12) . . . ? As1 C2 C7 113.1(8) . . . ? C3 C2 C7 119.3(14) . . . ? C2 C3 C4 119.2(15) . . . ? C2 C3 H4 120.4(17) . . . ? C4 C3 H4 120.4(12) . . . ? C3 C4 C5 119.8(13) . . . ? C3 C4 H5 120.1(18) . . . ? C5 C4 H5 120.1(18) . . . ? C4 C5 C6 121.5(18) . . . ? C4 C5 H6 119.3(14) . . . ? C6 C5 H6 119(2) . . . ? C5 C6 C7 119.0(16) . . . ? C5 C6 H7 120.5(18) . . . ? C7 C6 H7 120.5(12) . . . ? As2 C7 C2 113.0(9) . . . ? As2 C7 C6 125.9(10) . . . ? C2 C7 C6 121.0(10) . . . ? As2 C8 H8 109.6(10) . . . ? As2 C8 H9 109.3(11) . . . ? As2 C8 H10 109.3(13) . . . ? H8 C8 H9 109.6(17) . . . ? H8 C8 H10 109.6(13) . . . ? H9 C8 H10 109.5(11) . . . ? As2 C9 C10 116.4(9) . . . ? As2 C9 H11 107.7(11) . . . ? As2 C9 H12 107.7(10) . . . ? C10 C9 H11 107.7(12) . . . ? C10 C9 H12 107.7(13) . . . ? H11 C9 H12 109.5(14) . . . ? C9 C10 C11 112.8(11) . . . ? C9 C10 C12 106.3(12) . . . ? C9 C10 C13 110.2(10) . . . ? C11 C10 C12 109.2(9) . . . ? C11 C10 C13 112.9(11) . . . ? C12 C10 C13 104.9(10) . . . ? As1 C11 C10 119.0(8) . . . ? As1 C11 H13 107.0(9) . . . ? As1 C11 H14 107.0(9) . . . ? C10 C11 H13 107.0(11) . . . ? C10 C11 H14 107.0(11) . . . ? H13 C11 H14 109.5(11) . . . ? C10 C12 H15 109.6(13) . . . ? C10 C12 H16 109.4(11) . . . ? C10 C12 H17 109.3(14) . . . ? H15 C12 H16 109.6(17) . . . ? H15 C12 H17 109.6(13) . . . ? H16 C12 H17 109.4(15) . . . ? As3 C13 C10 114.5(8) . . . ? As3 C13 H18 108.2(8) . . . ? As3 C13 H19 108.2(11) . . . ? C10 C13 H18 108.2(14) . . . ? C10 C13 H19 108.2(10) . . . ? H18 C13 H19 109.5(12) . . . ? As3 C14 H20 109.7(12) . . . ? As3 C14 H21 109.2(12) . . . ? As3 C14 H22 109.2(14) . . . ? H20 C14 H21 109.7(17) . . . ? H20 C14 H22 109.6(13) . . . ? H21 C14 H22 109.5(14) . . . ? As3 C15 C16 120.4(9) . . . ? As3 C15 C20 117.5(8) . . . ? C16 C15 C20 122.1(9) . . . ? C15 C16 C17 117.0(13) . . . ? C15 C16 H23 121.5(12) . . . ? C17 C16 H23 121.5(15) . . . ? C16 C17 C18 122.3(14) . . . ? C16 C17 H24 118.8(15) . . . ? C18 C17 H24 118.8(13) . . . ? C17 C18 C19 117.8(12) . . . ? C17 C18 H25 121.1(16) . . . ? C19 C18 H25 121.1(15) . . . ? C18 C19 C20 121.8(13) . . . ? C18 C19 H26 119.1(12) . . . ? C20 C19 H26 119.1(13) . . . ? As4 C20 C15 117.2(7) . . . ? As4 C20 C19 124.2(10) . . . ? As4 C20 C31 16.8(4) . . 2_665 ? C15 C20 C19 118.7(11) . . . ? C15 C20 C31 124.8(9) . . 2_665 ? C19 C20 C31 114.6(12) . . 2_665 ? As4 C21 H27 109.6(13) . . . ? As4 C21 H28 109.3(11) . . . ? As4 C21 H29 109.2(11) . . . ? H27 C21 H28 109.6(14) . . . ? H27 C21 H29 109.6(13) . . . ? H28 C21 H29 109.5(16) . . . ? As4 C22 H30 109.6(9) . . . ? As4 C22 H31 109.3(10) . . . ? As4 C22 H32 109.3(10) . . . ? H30 C22 H31 109.6(14) . . . ? H30 C22 H32 109.6(14) . . . ? H31 C22 H32 109.5(13) . . . ? F1 P1 F2 91.4(9) . . . ? F1 P1 F3 91.4(7) . . . ? F1 P1 F4 177.7(7) . . . ? F1 P1 F5 88.9(11) . . . ? F1 P1 F6 90.4(6) . . . ? F1 P1 C32 101.7(7) . . . ? F1 P1 C33 63.4(4) . . . ? F1 P1 C29 79.8(6) . . 9_554 ? F2 P1 F3 95.3(13) . . . ? F2 P1 F4 90.0(12) . . . ? F2 P1 F5 178.1(14) . . . ? F2 P1 F6 91.7(12) . . . ? F2 P1 C32 137.2(9) . . . ? F2 P1 C33 63.3(9) . . . ? F2 P1 C29 48.3(9) . . 9_554 ? F3 P1 F4 90.3(7) . . . ? F3 P1 F5 86.6(14) . . . ? F3 P1 F6 172.7(12) . . . ? F3 P1 C32 44.6(9) . . . ? F3 P1 C33 44.9(7) . . . ? F3 P1 C29 141.7(9) . . 9_554 ? F4 P1 F5 89.7(14) . . . ? F4 P1 F6 87.7(6) . . . ? F4 P1 C32 78.4(9) . . . ? F4 P1 C33 118.9(6) . . . ? F4 P1 C29 99.8(9) . . 9_554 ? F5 P1 F6 86.4(13) . . . ? F5 P1 C32 44.5(10) . . . ? F5 P1 C33 118.4(10) . . . ? F5 P1 C29 130.0(10) . . 9_554 ? F6 P1 C32 128.2(8) . . . ? F6 P1 C33 141.5(7) . . . ? F6 P1 C29 45.6(8) . . 9_554 ? C32 P1 C33 86.6(2) . . . ? C32 P1 C29 173.8(2) . . 9_554 ? C33 P1 C29 99.5(2) . . 9_554 ? P1 F1 C33 55.5(4) . . . ? P1 F2 C33 58.7(10) . . . ? P1 F2 C29 70.6(8) . . 9_554 ? C33 F2 C29 112.8(15) . . 9_554 ? P1 F3 C32 60.5(5) . . . ? P1 F3 C33 65.2(8) . . . ? C32 F3 C33 120.3(11) . . . ? P1 F4 C30 92.5(8) . . 9 ? P1 F4 C36 155(3) . . 9 ? C30 F4 C36 66.0(15) 9 . 9 ? P1 F5 C32 59.9(10) . . . ? P1 F6 C29 68.8(5) . . 9_554 ? O1b O1a C34 31.4(16) . . 4_445 ? O1b O1a C34 31.4(16) . . 6 ? O1b O1a C34 31.4(16) . . 8_455 ? C34 O1a C34 54(3) 4_445 . 6 ? C34 O1a C34 54(3) 4_445 . 8_455 ? C34 O1a C34 54(3) 6 . 8_455 ? O1a O1b C34 107(7) . . 4_445 ? O1a O1b C34 107(7) . . 6 ? O1a O1b C34 107(7) . . 8_455 ? C34 O1b C34 112(7) 4_445 . 6 ? C34 O1b C34 112(7) 4_445 . 8_455 ? C34 O1b C34 112(7) 6 . 8_455 ? C23 O2 O2 65(4) . . 2 ? C23 O2 C23 31(3) . . 2 ? C23 O2 O2 44(2) . . 3 ? C23 O2 C23 27(3) . . 3 ? O2 O2 C23 60(6) 2 . 2 ? O2 O2 O2 60(4) 2 . 3 ? O2 O2 C23 42(3) 2 . 3 ? C23 O2 O2 71(4) 2 . 3 ? C23 O2 C23 23(4) 2 . 3 ? O2 O2 C23 52(3) 3 . 3 ? O2 C23 C24 108(3) . . . ? O2 C23 O2 63(5) . . 2 ? O2 C23 C23 54(6) . . 2 ? O2 C23 C24 122(3) . . 2 ? O2 C23 O2 76(6) . . 3 ? O2 C23 C23 93(7) . . 3 ? O2 C23 C24 142(5) . . 3 ? O2 C23 C27 118(3) . . 4_445 ? C24 C23 O2 113(4) . . 2 ? C24 C23 C23 64(4) . . 2 ? C24 C23 C24 31(4) . . 2 ? C24 C23 O2 176(7) . . 3 ? C24 C23 C23 84(5) . . 3 ? C24 C23 C24 34(4) . . 3 ? C24 C23 C27 21(3) . . 4_445 ? O2 C23 C23 60(7) 2 . 2 ? O2 C23 C24 94(5) 2 . 2 ? O2 C23 O2 67(4) 2 . 3 ? O2 C23 C23 38(5) 2 . 3 ? O2 C23 C24 124(5) 2 . 3 ? O2 C23 C27 101(5) 2 . 4_445 ? C23 C23 C24 69(5) 2 . 2 ? C23 C23 O2 119(6) 2 . 3 ? C23 C23 C23 60(11) 2 . 3 ? C23 C23 C24 95(5) 2 . 3 ? C23 C23 C27 66(4) 2 . 4_445 ? C24 C23 O2 145(8) 2 . 3 ? C24 C23 C23 57(5) 2 . 3 ? C24 C23 C24 32(3) 2 . 3 ? C24 C23 C27 11(3) 2 . 4_445 ? O2 C23 C23 95(7) 3 . 3 ? O2 C23 C24 142(7) 3 . 3 ? O2 C23 C27 156(9) 3 . 4_445 ? C23 C23 C24 86(5) 3 . 3 ? C23 C23 C27 66(5) 3 . 4_445 ? C24 C23 C27 29(2) 3 . 4_445 ? C23 C24 C25 108(3) . . . ? C23 C24 C23 30(3) . . 2 ? C23 C24 C24 81(4) . . 2 ? C23 C24 C25 147(4) . . 2 ? C23 C24 C23 28(3) . . 3 ? C23 C24 C24 63(3) . . 3 ? C23 C24 C25 133(6) . . 3 ? C23 C24 C27 29(3) . . 4_445 ? C25 C24 C23 133(4) . . 2 ? C25 C24 C24 64(4) . . 2 ? C25 C24 C25 49(5) . . 2 ? C25 C24 C23 106(4) . . 3 ? C25 C24 C24 45(3) . . 3 ? C25 C24 C25 47(3) . . 3 ? C25 C24 C27 92(4) . . 4_445 ? C23 C24 C24 83(6) 2 . 2 ? C23 C24 C25 174(8) 2 . 2 ? C23 C24 C23 28(5) 2 . 3 ? C23 C24 C24 90(4) 2 . 3 ? C23 C24 C25 132(6) 2 . 3 ? C23 C24 C27 41(3) 2 . 4_445 ? C24 C24 C25 103(7) 2 . 2 ? C24 C24 C23 58(4) 2 . 3 ? C24 C24 C24 60(6) 2 . 3 ? C24 C24 C25 53(5) 2 . 3 ? C24 C24 C27 52(4) 2 . 4_445 ? C25 C24 C23 155(6) 2 . 3 ? C25 C24 C24 89(5) 2 . 3 ? C25 C24 C25 54(6) 2 . 3 ? C25 C24 C27 141(6) 2 . 4_445 ? C23 C24 C24 68(4) 3 . 3 ? C23 C24 C25 111(5) 3 . 3 ? C23 C24 C27 15(3) 3 . 4_445 ? C24 C24 C25 83(6) 3 . 3 ? C24 C24 C27 53(4) 3 . 4_445 ? C25 C24 C27 105(6) 3 . 4_445 ? C24 C25 C26 109(2) . . . ? C24 C25 C24 33(4) . . 2 ? C24 C25 C25 46(3) . . 2 ? C24 C25 C24 32(4) . . 3 ? C24 C25 C25 60(4) . . 3 ? C24 C25 C27 24.1(16) . . 4_445 ? C26 C25 C24 117(3) . . 2 ? C26 C25 C25 67(3) . . 2 ? C26 C25 C24 141(5) . . 3 ? C26 C25 C25 67(3) . . 3 ? C26 C25 C27 131(2) . . 4_445 ? C24 C25 C25 73(4) 2 . 2 ? C24 C25 C24 37(4) 2 . 3 ? C24 C25 C25 51(3) 2 . 3 ? C24 C25 C27 23(3) 2 . 4_445 ? C25 C25 C24 75(5) 2 . 3 ? C25 C25 C25 60(7) 2 . 3 ? C25 C25 C27 70(3) 2 . 4_445 ? C24 C25 C25 85(4) 3 . 3 ? C24 C25 C27 15(2) 3 . 4_445 ? C25 C25 C27 70(3) 3 . 4_445 ? C25 C26 C25 45(3) . . 2 ? C25 C26 C25 45(3) . . 3 ? C25 C26 C25 45(5) 2 . 3 ? C23 C27 C24 131(5) 5_554 . 5_554 ? C23 C27 C25 134(3) 5_554 . 5_554 ? C23 C27 C23 47(4) 5_554 . 7_554 ? C23 C27 C24 155(7) 5_554 . 7_554 ? C23 C27 C25 139(5) 5_554 . 7_554 ? C23 C27 C23 47(5) 5_554 . 9_554 ? C23 C27 C24 110(4) 5_554 . 9_554 ? C23 C27 C25 173(3) 5_554 . 9_554 ? C24 C27 C25 64(3) 5_554 . 5_554 ? C24 C27 C23 110(5) 5_554 . 7_554 ? C24 C27 C24 74(7) 5_554 . 7_554 ? C24 C27 C25 24(4) 5_554 . 7_554 ? C24 C27 C23 154(6) 5_554 . 9_554 ? C24 C27 C24 74(7) 5_554 . 9_554 ? C24 C27 C25 52(5) 5_554 . 9_554 ? C25 C27 C23 173(6) 5_554 . 7_554 ? C25 C27 C24 51(5) 5_554 . 7_554 ? C25 C27 C25 40(3) 5_554 . 7_554 ? C25 C27 C23 140(6) 5_554 . 9_554 ? C25 C27 C24 24(3) 5_554 . 9_554 ? C25 C27 C25 40(2) 5_554 . 9_554 ? C23 C27 C24 133(7) 7_554 . 7_554 ? C23 C27 C25 134(5) 7_554 . 7_554 ? C23 C27 C23 47(8) 7_554 . 9_554 ? C23 C27 C24 153(7) 7_554 . 9_554 ? C23 C27 C25 140(4) 7_554 . 9_554 ? C24 C27 C25 63(7) 7_554 . 7_554 ? C24 C27 C23 111(7) 7_554 . 9_554 ? C24 C27 C24 74(6) 7_554 . 9_554 ? C24 C27 C25 24(6) 7_554 . 9_554 ? C25 C27 C23 174(4) 7_554 . 9_554 ? C25 C27 C24 51(6) 7_554 . 9_554 ? C25 C27 C25 40(4) 7_554 . 9_554 ? C23 C27 C24 132(8) 9_554 . 9_554 ? C23 C27 C25 135(4) 9_554 . 9_554 ? C24 C27 C25 64(3) 9_554 . 9_554 ? As1 C28 Co1 86.2(2) 6 . 6 ? As1 C28 Cl2 127.91(12) 6 . 6 ? Co1 C28 Cl2 108.5(2) 6 . 6 ? P1 C29 F2 61(2) 6 . 6 ? P1 C29 F6 65.5(8) 6 . 6 ? F2 C29 F6 123(2) 6 . 6 ? C36 C30 F4 25.1(5) . . 6_554 ? As4 C31 C20 146.9(9) 3_565 . 3_565 ? P1 C32 F3 74.9(10) . . . ? P1 C32 F5 75.7(14) . . . ? F3 C32 F5 142.2(14) . . . ? P1 C33 F1 61.2(4) . . . ? P1 C33 F2 58.0(6) . . . ? P1 C33 F3 70.0(5) . . . ? F1 C33 F2 87.4(8) . . . ? F1 C33 F3 106.3(10) . . . ? F2 C33 F3 109.8(9) . . . ? C34 C34 C34 60.000(3) 2_665 . 3_565 ? C34 C34 O1a 63.2(13) 2_665 . 5_554 ? C34 C34 O1b 34(3) 2_665 . 5_554 ? C34 C34 O1a 63.2(13) 3_565 . 5_554 ? C34 C34 O1b 34(3) 3_565 . 5_554 ? O1a C34 O1b 42(7) 5_554 . 5_554 ? As3 C35 Co1 169.28(10) 6 . 6 ? C30 C36 F4 89(2) . . 6_554 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_number_total 2406 _reflns_number_gt 2105 _reflns_threshold_expression I>2.00\s(I) _reflns_d_resolution_high .89 _reflns_d_resolution_low 13.051 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 1.5667 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? _publ_requested_journal ' test ' _publ_contact_author_name ; Anthony C. Willis ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email 'willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Roy J. Doyle' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Nicole Habermehl' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Geoffrey Salem ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Synthesis of Chiral Multidentate Tertiary Arsines with As4 or As6 Donor Atoms ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #===END data_rxd11_from_pw1100/20 #- _audit_creation_date '1998-12-08' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 2000-05-19 acw edits cif 2000-05-19 passes checkcif tests with minor warnings ; #- _publ_requested_journal ' test ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ; Anthony C. Willis ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email 'willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Roy J. Doyle' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Nicole Habermehl' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Geoffrey Salem ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Synthesis of Chiral Multidentate Tertiary Arsines with As4 or As6 Donor Atoms ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Hall, S. R., King, G. S. D. & Stewart, J. M. (1995). Editors. Xtal3.4 Reference Manual. Univ. of Western Australia: Lamb, Perth, Australia. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #- _computing_data_collection ; Philips PW1100/20 software 1976 ; _computing_cell_refinement xtal_LATCON _computing_data_reduction xtal_DIFDAT_ABSORB_ADDREF _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #- _cell_length_a 9.284(3) _cell_length_b 13.369(5) _cell_length_c 13.437(4) _cell_angle_alpha 90 _cell_angle_beta 106.44(3) _cell_angle_gamma 90 _cell_volume 1599.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.2 _cell_measurement_theta_max 19.3 #- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 921.47 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H35 As4 Cl3 Co F6 P ' _chemical_formula_moiety ' C23 H35 As4 Cl3 Co +, F6 P - ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 904.00 _exptl_absorpt_coefficient_mu 4.994 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.506 _exptl_absorpt_correction_T_min 0.308 _exptl_special_details ; ? ; #- _diffrn_special_details ; The scan width was (1.2+0.34tan\q)\% with an \w scan speed of 1.5\% per minute. Stationary background counts were recorded for 15 sec at each end of the scan. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Philips PW1100/20' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5047 _reflns_number_total 4867 _reflns_number_gt 3848 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.07867 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 30.11 _diffrn_reflns_reduction_process 'Lp corrections applied' _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 C 0 46 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 70 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; As 0 8 -0.030 2.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 6 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 2 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom As(1) 0.3099(1) 0.5000 0.24607(7) 0.0355(2) 1.000 . Uani d ? As(2) 0.2468(1) 0.7123(1) 0.3264(1) 0.0495(3) 1.000 . Uani d ? As(3) 0.4887(1) 0.6782(1) 0.15632(8) 0.0376(2) 1.000 . Uani d ? As(4) 0.1896(1) 0.6071(1) -0.01096(8) 0.0432(3) 1.000 . Uani d ? Co(1) 0.2467(1) 0.6508(1) 0.1630(1) 0.0348(3) 1.000 . Uani d ? Cl(1) 0.2016(4) 0.8123(3) 0.1103(3) 0.076(1) 1.000 . Uani d ? Cl(2) 0.0017(2) 0.6073(3) 0.1433(2) 0.0556(8) 1.000 . Uani d ? Cl(3) 0.8056(5) 0.3186(4) 0.3240(4) 0.099(2) 1.000 . Uani d ? P(1) 0.7532(4) 0.5953(3) 0.5999(2) 0.0583(9) 1.000 . Uani d ? F(1) 0.924(1) 0.628(1) 0.6491(9) 0.164(6) 1.000 . Uani d ? F(2) 0.695(1) 0.6885(7) 0.6505(7) 0.100(4) 1.000 . Uani d ? F(3) 0.760(1) 0.531(1) 0.6992(8) 0.120(4) 1.000 . Uani d ? F(4) 0.588(1) 0.561(1) 0.5535(9) 0.132(5) 1.000 . Uani d ? F(5) 0.804(1) 0.4995(8) 0.5483(7) 0.094(3) 1.000 . Uani d ? F(6) 0.751(2) 0.6619(9) 0.5011(7) 0.138(5) 1.000 . Uani d ? C(1) 0.788(1) 0.443(1) 0.303(1) 0.069(4) 1.000 . Uani d ? C(2) 0.631(1) 0.4806(8) 0.2400(8) 0.041(3) 1.000 . Uani d ? C(3) 0.519(1) 0.4602(9) 0.3026(8) 0.046(3) 1.000 . Uani d ? C(4) 0.209(2) 0.381(1) 0.179(1) 0.068(4) 1.000 . Uani d ? C(5) 0.245(1) 0.508(1) 0.3732(8) 0.053(3) 1.000 . Uani d ? C(6) 0.235(2) 0.414(1) 0.424(1) 0.066(4) 1.000 . Uani d ? C(7) 0.193(2) 0.425(2) 0.517(1) 0.089(6) 1.000 . Uani d ? C(8) 0.163(2) 0.520(2) 0.551(1) 0.081(5) 1.000 . Uani d ? C(9) 0.186(2) 0.604(1) 0.500(1) 0.075(5) 1.000 . Uani d ? C(10) 0.224(1) 0.5964(9) 0.4100(8) 0.045(3) 1.000 . Uani d ? C(11) 0.411(2) 0.788(1) 0.413(1) 0.072(4) 1.000 . Uani d ? C(12) 0.076(2) 0.793(1) 0.325(1) 0.088(5) 1.000 . Uani d ? C(13) 0.6537(9) 0.595(1) 0.2377(7) 0.045(3) 1.000 . Uani d ? C(14) 0.577(2) 0.807(1) 0.191(1) 0.071(4) 1.000 . Uani d ? C(15) 0.493(1) 0.6542(8) 0.0140(8) 0.042(3) 1.000 . Uani d ? C(16) 0.627(1) 0.668(1) -0.0134(9) 0.052(3) 1.000 . Uani d ? C(17) 0.622(1) 0.644(1) -0.118(1) 0.071(4) 1.000 . Uani d ? C(18) 0.496(2) 0.613(1) -0.186(1) 0.070(4) 1.000 . Uani d ? C(19) 0.366(1) 0.605(1) -0.1602(9) 0.058(3) 1.000 . Uani d ? C(20) 0.3628(9) 0.6225(8) -0.0581(7) 0.037(2) 1.000 . Uani d ? C(21) 0.122(2) 0.476(2) -0.064(1) 0.101(6) 1.000 . Uani d ? C(22) 0.041(1) 0.690(2) -0.102(1) 0.086(5) 1.000 . Uani d ? C(23) 0.589(1) 0.435(1) 0.1361(8) 0.057(4) 1.000 . Uani d ? H(1) 0.8131 0.4756 0.3686 0.083 1.000 . Uiso c ? H(2) 0.8577 0.4626 0.2665 0.083 1.000 . Uiso c ? H(3) 0.5198 0.3900 0.3140 0.055 1.000 . Uiso c ? H(4) 0.5564 0.4936 0.3672 0.055 1.000 . Uiso c ? H(5) 0.2352 0.3694 0.1165 0.082 1.000 . Uiso c ? H(6) 0.2393 0.3250 0.2239 0.082 1.000 . Uiso c ? H(7) 0.1036 0.3895 0.1637 0.082 1.000 . Uiso c ? H(8) 0.2543 0.3514 0.3983 0.079 1.000 . Uiso c ? H(9) 0.1856 0.3680 0.5565 0.106 1.000 . Uiso c ? H(10) 0.1254 0.5255 0.6093 0.097 1.000 . Uiso c ? H(11) 0.1757 0.6684 0.5275 0.090 1.000 . Uiso c ? H(12) 0.4992 0.7485 0.4297 0.087 1.000 . Uiso c ? H(13) 0.3875 0.8067 0.4750 0.087 1.000 . Uiso c ? H(14) 0.4259 0.8466 0.3771 0.087 1.000 . Uiso c ? H(15) 0.0674 0.7988 0.3939 0.106 1.000 . Uiso c ? H(16) -0.0122 0.7633 0.2819 0.106 1.000 . Uiso c ? H(17) 0.0883 0.8580 0.2996 0.106 1.000 . Uiso c ? H(18) 0.6774 0.6179 0.3074 0.054 1.000 . Uiso c ? H(19) 0.7370 0.6061 0.2112 0.054 1.000 . Uiso c ? H(20) 0.6665 0.8110 0.1697 0.086 1.000 . Uiso c ? H(21) 0.6014 0.8164 0.2640 0.086 1.000 . Uiso c ? H(22) 0.5087 0.8569 0.1568 0.086 1.000 . Uiso c ? H(23) 0.7157 0.6917 0.0350 0.062 1.000 . Uiso c ? H(24) 0.7105 0.6514 -0.1394 0.085 1.000 . Uiso c ? H(25) 0.4974 0.5947 -0.2540 0.084 1.000 . Uiso c ? H(26) 0.2757 0.5886 -0.2118 0.070 1.000 . Uiso c ? H(27) 0.1215 0.4711 -0.1344 0.122 1.000 . Uiso c ? H(28) 0.1878 0.4265 -0.0243 0.122 1.000 . Uiso c ? H(29) 0.0233 0.4646 -0.0584 0.122 1.000 . Uiso c ? H(30) 0.0222 0.6669 -0.1708 0.103 1.000 . Uiso c ? H(31) 0.0773 0.7573 -0.0974 0.103 1.000 . Uiso c ? H(32) -0.0486 0.6883 -0.0814 0.103 1.000 . Uiso c ? H(33) 0.5765 0.3649 0.1422 0.068 1.000 . Uiso c ? H(34) 0.6659 0.4471 0.1037 0.068 1.000 . Uiso c ? H(35) 0.4974 0.4634 0.0954 0.068 1.000 . Uiso c ? 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 As(1) 0.0375(4) 0.0359(5) 0.0352(5) -0.0007(4) 0.0134(4) -0.0036(4) As(2) 0.0427(5) 0.0515(7) 0.0536(7) 0.0071(5) 0.0127(5) -0.0196(6) As(3) 0.0269(4) 0.0421(6) 0.0421(5) -0.0029(4) 0.0072(4) -0.0011(5) As(4) 0.0274(4) 0.0654(7) 0.0346(5) -0.0052(5) 0.0055(3) 0.0016(5) Co(1) 0.0256(5) 0.0388(7) 0.0391(7) 0.0042(5) 0.0077(5) -0.0030(6) Cl(1) 0.070(2) 0.054(2) 0.100(3) 0.019(2) 0.017(2) 0.019(2) Cl(2) 0.027(1) 0.086(2) 0.054(1) -0.001(1) 0.013(1) -0.003(2) Cl(3) 0.099(3) 0.095(3) 0.108(3) 0.038(3) 0.037(2) 0.032(3) P(1) 0.073(2) 0.060(2) 0.045(2) -0.001(2) 0.022(1) -0.011(2) F(1) 0.103(7) 0.27(2) 0.123(9) -0.06(1) 0.040(6) -0.08(1) F(2) 0.166(9) 0.068(6) 0.097(6) 0.003(6) 0.087(7) -0.014(5) F(3) 0.16(1) 0.126(9) 0.083(6) 0.044(8) 0.054(7) 0.025(7) F(4) 0.071(6) 0.19(1) 0.132(9) -0.028(7) 0.022(6) -0.062(9) F(5) 0.126(7) 0.086(6) 0.080(6) 0.029(6) 0.046(5) -0.014(5) F(6) 0.26(2) 0.103(9) 0.072(6) 0.018(9) 0.081(8) 0.016(6) C(1) 0.057(7) 0.09(1) 0.060(8) 0.032(7) 0.013(6) 0.009(7) C(2) 0.048(5) 0.043(6) 0.036(5) 0.013(4) 0.019(4) 0.003(4) C(3) 0.042(5) 0.058(7) 0.037(5) 0.006(5) 0.010(4) -0.002(5) C(4) 0.09(1) 0.044(7) 0.060(8) -0.019(7) 0.010(7) -0.007(6) C(5) 0.038(5) 0.085(9) 0.042(6) -0.006(6) 0.019(4) 0.015(7) C(6) 0.073(8) 0.069(9) 0.059(8) 0.004(7) 0.026(7) 0.024(7) C(7) 0.064(8) 0.15(2) 0.056(9) -0.02(1) 0.029(7) 0.00(1) C(8) 0.074(9) 0.13(2) 0.044(7) 0.00(1) 0.032(6) -0.003(9) C(9) 0.071(8) 0.10(1) 0.055(7) 0.016(9) 0.022(6) -0.023(9) C(10) 0.034(4) 0.063(7) 0.039(5) 0.000(5) 0.012(4) -0.017(6) C(11) 0.069(8) 0.068(9) 0.075(9) 0.005(7) 0.011(7) -0.023(8) C(12) 0.073(9) 0.10(1) 0.08(1) 0.043(9) 0.016(7) -0.02(1) C(13) 0.026(4) 0.071(8) 0.034(5) 0.008(5) 0.000(3) 0.000(5) C(14) 0.067(8) 0.056(8) 0.09(1) -0.025(7) 0.022(7) -0.018(8) C(15) 0.037(4) 0.045(6) 0.042(5) 0.004(4) 0.011(4) 0.019(5) C(16) 0.037(5) 0.058(7) 0.065(7) -0.003(5) 0.021(5) 0.009(6) C(17) 0.056(6) 0.11(1) 0.060(7) 0.009(7) 0.039(6) 0.019(8) C(18) 0.069(8) 0.10(1) 0.049(7) -0.002(8) 0.028(6) 0.008(8) C(19) 0.050(6) 0.080(9) 0.042(6) -0.003(7) 0.008(5) 0.005(7) C(20) 0.034(4) 0.045(6) 0.031(4) 0.000(4) 0.009(3) 0.005(4) C(21) 0.10(1) 0.16(2) 0.048(8) -0.09(1) 0.022(7) -0.03(1) C(22) 0.051(7) 0.13(2) 0.069(9) 0.033(9) 0.008(6) 0.03(1) C(23) 0.067(7) 0.067(8) 0.038(6) 0.014(6) 0.017(5) 0.002(6) #- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Absolute structure determined by comparative refinement. Refinement of a model with coordinates transformed by (-x,-y,-z) yielded R = 0.0531, wR = 0.0595, S = 2.270. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3848 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_all 0.0606 _refine_ls_wR_factor_ref 0.0584 _refine_ls_goodness_of_fit_all 2.048 _refine_ls_goodness_of_fit_ref 2.240 _refine_ls_shift/su_max 0.0124 _refine_ls_shift/su_mean 0.0022 _refine_diff_density_min -1.34 _refine_diff_density_max 1.21 #- _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 As(1) Co(1) 2.299(2) . . yes As(1) C(3) 1.95(1) . . yes As(1) C(4) 1.94(1) . . yes As(1) C(5) 1.97(1) . . yes As(2) Co(1) 2.343(2) . . yes As(2) C(10) 1.96(1) . . yes As(2) C(11) 1.92(1) . . yes As(2) C(12) 1.92(1) . . yes As(3) Co(1) 2.303(2) . . yes As(3) C(13) 1.96(1) . . yes As(3) C(14) 1.91(1) . . yes As(3) C(15) 1.95(1) . . yes As(4) Co(1) 2.321(2) . . yes As(4) C(20) 1.899(9) . . yes As(4) C(21) 1.93(2) . . yes As(4) C(22) 1.91(1) . . yes Co(1) Cl(1) 2.275(4) . . yes Co(1) Cl(2) 2.289(3) . . yes Cl(3) C(1) 1.69(2) . . yes P(1) F(1) 1.59(1) . . yes P(1) F(2) 1.585(9) . . yes P(1) F(3) 1.57(1) . . yes P(1) F(4) 1.55(1) . . yes P(1) F(5) 1.592(9) . . yes P(1) F(6) 1.59(1) . . yes C(1) C(2) 1.55(1) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) C(3) 1.53(1) . . yes C(2) C(13) 1.55(2) . . yes C(2) C(23) 1.47(2) . . yes C(3) H(3) 0.95 . . no C(3) H(4) 0.95 . . no C(4) H(5) 0.95 . . no C(4) H(6) 0.95 . . no C(4) H(7) 0.95 . . no C(5) C(6) 1.44(2) . . yes C(5) C(10) 1.32(2) . . yes C(6) C(7) 1.41(2) . . yes C(6) H(8) 0.95 . . no C(7) C(8) 1.40(3) . . yes C(7) H(9) 0.95 . . no C(8) C(9) 1.37(2) . . yes C(8) H(10) 0.95 . . no C(9) C(10) 1.35(2) . . yes C(9) H(11) 0.95 . . no C(11) H(12) 0.95 . . no C(11) H(13) 0.95 . . no C(11) H(14) 0.95 . . no C(12) H(15) 0.95 . . no C(12) H(16) 0.95 . . no C(12) H(17) 0.95 . . no C(13) H(18) 0.95 . . no C(13) H(19) 0.95 . . no C(14) H(20) 0.95 . . no C(14) H(21) 0.95 . . no C(14) H(22) 0.95 . . no C(15) C(16) 1.40(1) . . yes C(15) C(20) 1.39(1) . . yes C(16) C(17) 1.43(2) . . yes C(16) H(23) 0.95 . . no C(17) C(18) 1.34(2) . . yes C(17) H(24) 0.95 . . no C(18) C(19) 1.35(2) . . yes C(18) H(25) 0.95 . . no C(19) C(20) 1.40(1) . . yes C(19) H(26) 0.95 . . no C(21) H(27) 0.95 . . no C(21) H(28) 0.95 . . no C(21) H(29) 0.95 . . no C(22) H(30) 0.95 . . no C(22) H(31) 0.95 . . no C(22) H(32) 0.95 . . no C(23) H(33) 0.95 . . no C(23) H(34) 0.95 . . no C(23) H(35) 0.95 . . no #- 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 Co(1) As(1) C(3) 121.2(4) . . . yes Co(1) As(1) C(4) 118.2(4) . . . yes Co(1) As(1) C(5) 106.1(4) . . . yes C(3) As(1) C(4) 104.7(6) . . . yes C(3) As(1) C(5) 101.1(4) . . . yes C(4) As(1) C(5) 102.7(6) . . . yes Co(1) As(2) C(10) 106.8(3) . . . yes Co(1) As(2) C(11) 122.9(4) . . . yes Co(1) As(2) C(12) 114.2(5) . . . yes C(10) As(2) C(11) 105.3(6) . . . yes C(10) As(2) C(12) 103.2(7) . . . yes C(11) As(2) C(12) 102.5(7) . . . yes Co(1) As(3) C(13) 120.4(3) . . . yes Co(1) As(3) C(14) 119.5(4) . . . yes Co(1) As(3) C(15) 107.7(3) . . . yes C(13) As(3) C(14) 99.2(6) . . . yes C(13) As(3) C(15) 102.9(4) . . . yes C(14) As(3) C(15) 105.1(6) . . . yes Co(1) As(4) C(20) 109.6(3) . . . yes Co(1) As(4) C(21) 123.8(4) . . . yes Co(1) As(4) C(22) 114.3(5) . . . yes C(20) As(4) C(21) 101.2(6) . . . yes C(20) As(4) C(22) 104.4(5) . . . yes C(21) As(4) C(22) 101.3(8) . . . yes As(1) Co(1) As(2) 85.44(6) . . . yes As(1) Co(1) As(3) 92.32(5) . . . yes As(1) Co(1) As(4) 102.86(6) . . . yes As(1) Co(1) Cl(1) 169.5(1) . . . yes As(1) Co(1) Cl(2) 86.7(1) . . . yes As(2) Co(1) As(3) 103.82(6) . . . yes As(2) Co(1) As(4) 166.21(7) . . . yes As(2) Co(1) Cl(1) 84.8(1) . . . yes As(2) Co(1) Cl(2) 86.24(8) . . . yes As(3) Co(1) As(4) 87.02(5) . . . yes As(3) Co(1) Cl(1) 86.1(1) . . . yes As(3) Co(1) Cl(2) 169.8(1) . . . yes As(4) Co(1) Cl(1) 87.5(1) . . . yes As(4) Co(1) Cl(2) 83.30(8) . . . yes Cl(1) Co(1) Cl(2) 96.7(1) . . . yes F(1) P(1) F(2) 91.4(8) . . . yes F(1) P(1) F(3) 90.1(8) . . . yes F(1) P(1) F(4) 178(1) . . . yes F(1) P(1) F(5) 91.0(7) . . . yes F(1) P(1) F(6) 88.3(8) . . . yes F(2) P(1) F(3) 90.0(5) . . . yes F(2) P(1) F(4) 89.4(6) . . . yes F(2) P(1) F(5) 177.4(6) . . . yes F(2) P(1) F(6) 89.5(5) . . . yes F(3) P(1) F(4) 88.6(7) . . . yes F(3) P(1) F(5) 89.2(6) . . . yes F(3) P(1) F(6) 178.3(8) . . . yes F(4) P(1) F(5) 88.1(6) . . . yes F(4) P(1) F(6) 93.0(7) . . . yes F(5) P(1) F(6) 91.3(5) . . . yes Cl(3) C(1) C(2) 116(1) . . . yes Cl(3) C(1) H(1) 107.8 . . . no Cl(3) C(1) H(2) 107.8 . . . no C(2) C(1) H(1) 107.8 . . . no C(2) C(1) H(2) 107.8 . . . no H(1) C(1) H(2) 109.5 . . . no C(1) C(2) C(3) 108.8(9) . . . yes C(1) C(2) C(13) 102.4(9) . . . yes C(1) C(2) C(23) 109.8(9) . . . yes C(3) C(2) C(13) 107.8(8) . . . yes C(3) C(2) C(23) 114.1(9) . . . yes C(13) C(2) C(23) 113.1(9) . . . yes As(1) C(3) C(2) 119.4(7) . . . yes As(1) C(3) H(3) 106.9 . . . no As(1) C(3) H(4) 106.9 . . . no C(2) C(3) H(3) 106.9 . . . no C(2) C(3) H(4) 106.9 . . . no H(3) C(3) H(4) 109.4 . . . no As(1) C(4) H(5) 109.5 . . . no As(1) C(4) H(6) 109.5 . . . no As(1) C(4) H(7) 109.5 . . . no H(5) C(4) H(6) 109.5 . . . no H(5) C(4) H(7) 109.5 . . . no H(6) C(4) H(7) 109.5 . . . no As(1) C(5) C(6) 117(1) . . . yes As(1) C(5) C(10) 119.0(9) . . . yes C(6) C(5) C(10) 124(1) . . . yes C(5) C(6) C(7) 114(1) . . . yes C(5) C(6) H(8) 123.1 . . . no C(7) C(6) H(8) 123.1 . . . no C(6) C(7) C(8) 121(2) . . . yes C(6) C(7) H(9) 119.6 . . . no C(8) C(7) H(9) 119.6 . . . no C(7) C(8) C(9) 121(1) . . . yes C(7) C(8) H(10) 119.7 . . . no C(9) C(8) H(10) 119.7 . . . no C(8) C(9) C(10) 120(1) . . . yes C(8) C(9) H(11) 120.1 . . . no C(10) C(9) H(11) 120.1 . . . no As(2) C(10) C(5) 116.4(8) . . . yes As(2) C(10) C(9) 123(1) . . . yes C(5) C(10) C(9) 120(1) . . . yes As(2) C(11) H(12) 109.5 . . . no As(2) C(11) H(13) 109.5 . . . no As(2) C(11) H(14) 109.5 . . . no H(12) C(11) H(13) 109.5 . . . no H(12) C(11) H(14) 109.5 . . . no H(13) C(11) H(14) 109.5 . . . no As(2) C(12) H(15) 109.5 . . . no As(2) C(12) H(16) 109.5 . . . no As(2) C(12) H(17) 109.5 . . . no H(15) C(12) H(16) 109.5 . . . no H(15) C(12) H(17) 109.5 . . . no H(16) C(12) H(17) 109.5 . . . no As(3) C(13) C(2) 118.9(7) . . . yes As(3) C(13) H(18) 107.1 . . . no As(3) C(13) H(19) 107.1 . . . no C(2) C(13) H(18) 107.1 . . . no C(2) C(13) H(19) 107.1 . . . no H(18) C(13) H(19) 109.5 . . . no As(3) C(14) H(20) 109.5 . . . no As(3) C(14) H(21) 109.5 . . . no As(3) C(14) H(22) 109.5 . . . no H(20) C(14) H(21) 109.5 . . . no H(20) C(14) H(22) 109.5 . . . no H(21) C(14) H(22) 109.5 . . . no As(3) C(15) C(16) 120.2(8) . . . yes As(3) C(15) C(20) 118.5(7) . . . yes C(16) C(15) C(20) 121.3(9) . . . yes C(15) C(16) C(17) 117(1) . . . yes C(15) C(16) H(23) 121.7 . . . no C(17) C(16) H(23) 121.7 . . . no C(16) C(17) C(18) 121(1) . . . yes C(16) C(17) H(24) 119.3 . . . no C(18) C(17) H(24) 119.3 . . . no C(17) C(18) C(19) 122(1) . . . yes C(17) C(18) H(25) 119.2 . . . no C(19) C(18) H(25) 119.2 . . . no C(18) C(19) C(20) 120(1) . . . yes C(18) C(19) H(26) 119.8 . . . no C(20) C(19) H(26) 119.8 . . . no As(4) C(20) C(15) 117.1(7) . . . yes As(4) C(20) C(19) 124.3(7) . . . yes C(15) C(20) C(19) 118.6(9) . . . yes As(4) C(21) H(27) 109.5 . . . no As(4) C(21) H(28) 109.5 . . . no As(4) C(21) H(29) 109.5 . . . no H(27) C(21) H(28) 109.5 . . . no H(27) C(21) H(29) 109.5 . . . no H(28) C(21) H(29) 109.5 . . . no As(4) C(22) H(30) 109.5 . . . no As(4) C(22) H(31) 109.5 . . . no As(4) C(22) H(32) 109.5 . . . no H(30) C(22) H(31) 109.5 . . . no H(30) C(22) H(32) 109.5 . . . no H(31) C(22) H(32) 109.5 . . . no C(2) C(23) H(33) 109.5 . . . no C(2) C(23) H(34) 109.5 . . . no C(2) C(23) H(35) 109.5 . . . no H(33) C(23) H(34) 109.5 . . . no H(33) C(23) H(35) 109.5 . . . no H(34) C(23) H(35) 109.5 . . . no #- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(3) F(1) 3.53(2) . 2_746 no F(1) C(8) 3.23(2) . 1_655 no F(1) C(22) 3.32(2) . 1_656 no F(1) C(9) 3.58(2) . 1_655 no F(2) C(6) 3.31(2) . 2_656 no F(2) C(4) 3.39(2) . 2_656 no F(2) C(18) 3.40(1) . 1_556 no F(2) C(17) 3.42(1) . 1_556 no F(3) C(18) 3.42(2) . 1_556 no F(3) C(17) 3.43(2) . 1_556 no F(3) C(12) 3.58(2) . 2_646 no F(4) C(10) 3.42(1) . . no F(4) C(5) 3.49(1) . . no F(4) C(3) 3.52(1) . . no F(5) C(12) 3.26(2) . 2_646 no F(5) C(8) 3.33(2) . 1_655 no F(5) C(1) 3.34(2) . . no F(5) C(11) 3.58(2) . 2_646 no F(6) C(11) 3.48(2) . . no F(6) C(13) 3.51(1) . . no F(6) C(6) 3.51(2) . 2_656 no F(6) C(7) 3.58(3) . 2_656 no C(4) C(22) 3.41(2) . 2_545 no #- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag As(1) Co(1) As(2) C(10) . . . . -20.4(3) no As(1) Co(1) As(2) C(11) . . . . 101.2(6) no As(1) Co(1) As(2) C(12) . . . . -133.8(7) no As(1) Co(1) As(3) C(13) . . . . -12.3(4) no As(1) Co(1) As(3) C(14) . . . . -135.4(6) no As(1) Co(1) As(3) C(15) . . . . 105.0(3) no As(1) Co(1) As(4) C(20) . . . . -93.7(3) no As(1) Co(1) As(4) C(21) . . . . 25.4(7) no As(1) Co(1) As(4) C(22) . . . . 149.6(6) no As(1) C(3) C(2) C(1) . . . . 179.1(8) no As(1) C(3) C(2) C(13) . . . . 69(1) no As(1) C(3) C(2) C(23) . . . . -58(1) no As(1) C(5) C(6) C(7) . . . . 178(1) no As(1) C(5) C(10) As(2) . . . . 5(1) no As(1) C(5) C(10) C(9) . . . . -177.0(9) no As(2) Co(1) As(1) C(3) . . . . -92.4(4) no As(2) Co(1) As(1) C(4) . . . . 136.2(5) no As(2) Co(1) As(1) C(5) . . . . 21.7(3) no As(2) Co(1) As(3) C(13) . . . . 73.5(4) no As(2) Co(1) As(3) C(14) . . . . -49.5(6) no As(2) Co(1) As(3) C(15) . . . . -169.1(3) no As(2) Co(1) As(4) C(20) . . . . 140.3(4) no As(2) Co(1) As(4) C(21) . . . . -100.6(8) no As(2) Co(1) As(4) C(22) . . . . 23.6(7) no As(2) C(10) C(5) C(6) . . . . 179(1) no As(2) C(10) C(9) C(8) . . . . 176(1) no As(3) Co(1) As(1) C(3) . . . . 11.3(4) no As(3) Co(1) As(1) C(4) . . . . -120.1(5) no As(3) Co(1) As(1) C(5) . . . . 125.4(3) no As(3) Co(1) As(2) C(10) . . . . -111.6(3) no As(3) Co(1) As(2) C(11) . . . . 9.9(6) no As(3) Co(1) As(2) C(12) . . . . 134.9(7) no As(3) Co(1) As(4) C(20) . . . . -2.0(3) no As(3) Co(1) As(4) C(21) . . . . 117.1(7) no As(3) Co(1) As(4) C(22) . . . . -118.7(6) no As(3) C(13) C(2) C(1) . . . . 175.2(7) no As(3) C(13) C(2) C(3) . . . . -70(1) no As(3) C(13) C(2) C(23) . . . . 57(1) no As(3) C(15) C(16) C(17) . . . . 177(1) no As(3) C(15) C(20) As(4) . . . . 1(1) no As(3) C(15) C(20) C(19) . . . . 179.9(9) no As(4) Co(1) As(1) C(3) . . . . 98.7(4) no As(4) Co(1) As(1) C(4) . . . . -32.6(5) no As(4) Co(1) As(1) C(5) . . . . -147.1(3) no As(4) Co(1) As(2) C(10) . . . . 107.3(4) no As(4) Co(1) As(2) C(11) . . . . -131.1(6) no As(4) Co(1) As(2) C(12) . . . . -6.1(8) no As(4) Co(1) As(3) C(13) . . . . -115.1(4) no As(4) Co(1) As(3) C(14) . . . . 121.9(6) no As(4) Co(1) As(3) C(15) . . . . 2.2(3) no As(4) C(20) C(15) C(16) . . . . -179.9(9) no As(4) C(20) C(19) C(18) . . . . -176(1) no Co(1) As(1) C(3) C(2) . . . . -41(1) no Co(1) As(1) C(5) C(6) . . . . 163.8(9) no Co(1) As(1) C(5) C(10) . . . . -21.1(9) no Co(1) As(2) C(10) C(5) . . . . 13.7(9) no Co(1) As(2) C(10) C(9) . . . . -165(1) no Co(1) As(3) C(13) C(2) . . . . 43.9(8) no Co(1) As(3) C(15) C(16) . . . . 178.3(8) no Co(1) As(3) C(15) C(20) . . . . -2.3(9) no Co(1) As(4) C(20) C(15) . . . . 1.1(9) no Co(1) As(4) C(20) C(19) . . . . -178(1) no Cl(1) Co(1) As(1) C(3) . . . . -69.9(7) no Cl(1) Co(1) As(1) C(4) . . . . 158.8(8) no Cl(1) Co(1) As(1) C(5) . . . . 44.3(7) no Cl(1) Co(1) As(2) C(10) . . . . 163.7(3) no Cl(1) Co(1) As(2) C(11) . . . . -74.8(6) no Cl(1) Co(1) As(2) C(12) . . . . 50.3(7) no Cl(1) Co(1) As(3) C(13) . . . . 157.2(4) no Cl(1) Co(1) As(3) C(14) . . . . 34.2(6) no Cl(1) Co(1) As(3) C(15) . . . . -85.4(3) no Cl(1) Co(1) As(4) C(20) . . . . 84.3(3) no Cl(1) Co(1) As(4) C(21) . . . . -156.6(7) no Cl(1) Co(1) As(4) C(22) . . . . -32.5(6) no Cl(2) Co(1) As(1) C(3) . . . . -178.9(4) no Cl(2) Co(1) As(1) C(4) . . . . 49.7(5) no Cl(2) Co(1) As(1) C(5) . . . . -64.7(3) no Cl(2) Co(1) As(2) C(10) . . . . 66.6(3) no Cl(2) Co(1) As(2) C(11) . . . . -171.8(6) no Cl(2) Co(1) As(2) C(12) . . . . -46.8(7) no Cl(2) Co(1) As(3) C(13) . . . . -96.7(7) no Cl(2) Co(1) As(3) C(14) . . . . 140.3(8) no Cl(2) Co(1) As(3) C(15) . . . . 20.6(7) no Cl(2) Co(1) As(4) C(20) . . . . -178.7(3) no Cl(2) Co(1) As(4) C(21) . . . . -59.6(7) no Cl(2) Co(1) As(4) C(22) . . . . 64.5(6) no Cl(3) C(1) C(2) C(3) . . . . 65(1) no Cl(3) C(1) C(2) C(13) . . . . 178.8(8) no Cl(3) C(1) C(2) C(23) . . . . -61(1) no C(2) C(3) As(1) C(4) . . . . 95(1) no C(2) C(3) As(1) C(5) . . . . -158.1(9) no C(2) C(13) As(3) C(14) . . . . 176.3(8) no C(2) C(13) As(3) C(15) . . . . -75.8(8) no C(3) As(1) C(5) C(6) . . . . -69(1) no C(3) As(1) C(5) C(10) . . . . 106.2(9) no C(4) As(1) C(5) C(6) . . . . 39(1) no C(4) As(1) C(5) C(10) . . . . -145.8(9) no C(5) C(6) C(7) C(8) . . . . 1(2) no C(5) C(10) As(2) C(11) . . . . -118.4(9) no C(5) C(10) As(2) C(12) . . . . 134.5(9) no C(5) C(10) C(9) C(8) . . . . -3(2) no C(6) C(5) C(10) C(9) . . . . -2(2) no C(6) C(7) C(8) C(9) . . . . -6(2) no C(7) C(6) C(5) C(10) . . . . 3(2) no C(7) C(8) C(9) C(10) . . . . 7(2) no C(9) C(10) As(2) C(11) . . . . 63(1) no C(9) C(10) As(2) C(12) . . . . -44(1) no C(13) As(3) C(15) C(16) . . . . -54(1) no C(13) As(3) C(15) C(20) . . . . 125.8(9) no C(14) As(3) C(15) C(16) . . . . 50(1) no C(14) As(3) C(15) C(20) . . . . -130.8(9) no C(15) C(16) C(17) C(18) . . . . 1(2) no C(15) C(20) As(4) C(21) . . . . -131.1(9) no C(15) C(20) As(4) C(22) . . . . 124(1) no C(15) C(20) C(19) C(18) . . . . 5(2) no C(16) C(15) C(20) C(19) . . . . -1(2) no C(16) C(17) C(18) C(19) . . . . 3(3) no C(17) C(16) C(15) C(20) . . . . -2(2) no C(17) C(18) C(19) C(20) . . . . -6(3) no C(19) C(20) As(4) C(21) . . . . 50(1) no C(19) C(20) As(4) C(22) . . . . -55(1) no #- #===END data_rxd12 #- _audit_creation_date '1999-03-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 2000-05-19 acw edits cif 2000-05-19 passes checkcif tests with minor warnings ; #- _publ_requested_journal ' test ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ; Anthony C. Willis ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email 'willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Roy J. Doyle' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Nicole Habermehl' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Geoffrey Salem ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Synthesis of Chiral Multidentate Tertiary Arsines with As4 or As6 Donor Atoms ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #- _cell_length_a 13.080(3) _cell_length_b 24.057(4) _cell_length_c 31.300(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9849(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 53.1 _cell_measurement_theta_max 54.8 #- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'octahedron' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1439.75 _chemical_formula_analytical ? _chemical_formula_sum 'C35 H54.62 As6 Co F18 O1.31 P3 ' _chemical_formula_moiety 'C32 H48 As6 Co 3+, (F6 P -)3, C3 H6 O, 0.31(H2 O)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 5656.80 _exptl_absorpt_coefficient_mu 9.047 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.344 _exptl_absorpt_correction_T_min 0.232 _exptl_special_details ; The scan width was (1.00+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. Mass attenuation coefficients for absorption from International Tables for X-ray Crystallography, Vol IV (1974) Table 2.1C. ; #- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_method \w-2\q _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.47 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 0 0 0 4 0 0 0 12 _diffrn_reflns_number 8059 _reflns_number_total 7312 _reflns_number_gt 5385 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 60.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00796 _diffrn_orient_matrix_UB_12 0.03899 _diffrn_orient_matrix_UB_13 -0.01057 _diffrn_orient_matrix_UB_21 -0.04967 _diffrn_orient_matrix_UB_22 0.01314 _diffrn_orient_matrix_UB_23 0.02209 _diffrn_orient_matrix_UB_31 0.05758 _diffrn_orient_matrix_UB_32 0.00594 _diffrn_orient_matrix_UB_33 0.02052 #- 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 C 0 280 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 436.96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; As 0 48 -1.011 1.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 8 -2.464 3.608 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 144 0.069 0.053 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 10.48 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 24 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom As(1) 0.30385(7) 0.16164(4) 0.56234(3) 0.0235(3) 1.000 . Uani d ? As(2) 0.24809(8) 0.03308(4) 0.57922(3) 0.0276(3) 1.000 . Uani d ? As(3) 0.48954(7) 0.08751(4) 0.59536(3) 0.0245(3) 1.000 . Uani d ? As(4) 0.36521(7) 0.04058(4) 0.67680(3) 0.0258(3) 1.000 . Uani d ? As(5) 0.39257(7) 0.18221(4) 0.65540(3) 0.0232(2) 1.000 . Uani d ? As(6) 0.16628(7) 0.13029(4) 0.65138(3) 0.0244(3) 1.000 . Uani d ? Co(1) 0.3241(1) 0.10333(5) 0.62128(4) 0.0218(4) 1.000 . Uani d ? P(1) -0.0206(2) -0.0980(1) 0.68755(9) 0.0387(7) 1.000 . Uani d ? P(2) 0.2926(2) 0.1969(1) 0.81632(9) 0.0414(8) 1.000 . Uani d ? P(3) 0.3599(2) 0.1442(1) 0.9889(1) 0.0475(9) 1.000 . Uani d ? F(1) 0.0056(9) -0.0345(3) 0.6887(3) 0.150(4) 1.000 . Uani d ? F(2) 0.0666(7) -0.1104(3) 0.6542(3) 0.118(3) 1.000 . Uani d ? F(3) -0.0939(8) -0.0884(5) 0.6519(3) 0.184(5) 1.000 . Uani d ? F(4) -0.0375(6) -0.1616(3) 0.6899(3) 0.094(3) 1.000 . Uani d ? F(5) -0.1015(5) -0.0831(3) 0.7223(2) 0.088(3) 1.000 . Uani d ? F(6) 0.0603(7) -0.1059(4) 0.7236(3) 0.142(4) 1.000 . Uani d ? F(7) 0.3497(5) 0.2476(3) 0.7950(2) 0.083(3) 1.000 . Uani d ? F(8) 0.3880(4) 0.1579(2) 0.8055(2) 0.054(2) 1.000 . Uani d ? F(9) 0.2439(5) 0.1819(3) 0.7714(2) 0.079(2) 1.000 . Uani d ? F(10) 0.2372(6) 0.1455(3) 0.8360(2) 0.092(3) 1.000 . Uani d ? F(11) 0.1968(4) 0.2346(3) 0.8274(2) 0.075(2) 1.000 . Uani d ? F(12) 0.3449(6) 0.2129(3) 0.8595(2) 0.089(3) 1.000 . Uani d ? F(13) 0.3529(7) 0.1209(4) 0.9443(2) 0.142(4) 1.000 . Uani d ? F(14) 0.2495(6) 0.1209(4) 0.9969(3) 0.119(3) 1.000 . Uani d ? F(15) 0.4026(7) 0.0911(3) 1.0095(4) 0.151(4) 1.000 . Uani d ? F(16) 0.3663(6) 0.1708(3) 1.0361(2) 0.098(3) 1.000 . Uani d ? F(17) 0.4698(5) 0.1675(3) 0.9814(2) 0.084(3) 1.000 . Uani d ? F(18) 0.3121(6) 0.2006(3) 0.9750(3) 0.112(3) 1.000 . Uani d ? O(1) 0.4661(8) 0.3957(5) 0.9416(4) 0.135(5) 1.000 . Uani d ? O(2) 0.227(3) -0.147(2) 0.609(1) 0.177 0.31(2) . Uiso d ? C(1) 0.5874(7) 0.2490(4) 0.5584(3) 0.037(3) 1.000 . Uani d ? C(2) 0.5124(6) 0.2068(3) 0.5765(3) 0.027(2) 1.000 . Uani d ? C(3) 0.4313(6) 0.1939(3) 0.5420(3) 0.028(2) 1.000 . Uani d ? C(4) 0.2135(7) 0.2248(4) 0.5642(3) 0.036(3) 1.000 . Uani d ? C(5) 0.2511(7) 0.1187(4) 0.5152(3) 0.029(2) 1.000 . Uani d ? C(6) 0.2348(7) 0.1424(4) 0.4753(3) 0.033(3) 1.000 . Uani d ? C(7) 0.1931(8) 0.1111(4) 0.4433(3) 0.043(3) 1.000 . Uani d ? C(8) 0.1683(8) 0.0554(4) 0.4503(3) 0.049(3) 1.000 . Uani d ? C(9) 0.1867(8) 0.0316(4) 0.4898(3) 0.044(3) 1.000 . Uani d ? C(10) 0.2276(6) 0.0624(4) 0.5226(3) 0.028(2) 1.000 . Uani d ? C(11) 0.3232(9) -0.0355(4) 0.5701(3) 0.047(3) 1.000 . Uani d ? C(12) 0.1144(8) 0.0037(4) 0.5919(3) 0.048(3) 1.000 . Uani d ? C(13) 0.5710(6) 0.1541(4) 0.5876(3) 0.030(3) 1.000 . Uani d ? C(14) 0.5151(7) 0.0495(4) 0.5416(3) 0.040(3) 1.000 . Uani d ? C(15) 0.5623(6) 0.0429(3) 0.6363(3) 0.026(2) 1.000 . Uani d ? C(16) 0.6660(7) 0.0327(4) 0.6319(3) 0.037(3) 1.000 . Uani d ? C(17) 0.7154(7) 0.0008(4) 0.6626(3) 0.043(3) 1.000 . Uani d ? C(18) 0.6610(8) -0.0215(4) 0.6964(3) 0.043(3) 1.000 . Uani d ? C(19) 0.5601(7) -0.0101(4) 0.7008(3) 0.034(3) 1.000 . Uani d ? C(20) 0.5112(7) 0.0234(3) 0.6713(3) 0.027(2) 1.000 . Uani d ? C(21) 0.3519(8) 0.0614(4) 0.7365(3) 0.042(3) 1.000 . Uani d ? C(22) 0.3034(8) -0.0324(4) 0.6802(3) 0.042(3) 1.000 . Uani d ? C(23) 0.4632(6) 0.2330(3) 0.6162(3) 0.030(3) 1.000 . Uani d ? C(24) 0.4883(7) 0.1765(4) 0.7026(3) 0.037(3) 1.000 . Uani d ? C(25) 0.2794(6) 0.2257(4) 0.6776(3) 0.025(2) 1.000 . Uani d ? C(26) 0.2965(7) 0.2773(4) 0.6963(3) 0.033(3) 1.000 . Uani d ? C(27) 0.2155(8) 0.3062(4) 0.7127(3) 0.043(3) 1.000 . Uani d ? C(28) 0.1181(7) 0.2848(4) 0.7097(3) 0.041(3) 1.000 . Uani d ? C(29) 0.1008(7) 0.2338(4) 0.6909(3) 0.037(3) 1.000 . Uani d ? C(30) 0.1834(6) 0.2040(3) 0.6748(3) 0.026(2) 1.000 . Uani d ? C(31) 0.0464(7) 0.1359(4) 0.6148(3) 0.033(3) 1.000 . Uani d ? C(32) 0.1080(7) 0.0906(4) 0.6989(3) 0.037(3) 1.000 . Uani d ? C(33) 0.4619(9) 0.3602(5) 0.9136(5) 0.067(4) 1.000 . Uani d ? C(34) 0.416(2) 0.3700(7) 0.8721(5) 0.167(9) 1.000 . Uani d ? C(35) 0.497(2) 0.3048(8) 0.9196(5) 0.167(9) 1.000 . Uani d ? H(1) 0.6379 0.2574 0.5792 0.045 1.000 . Uiso c ? H(2) 0.6194 0.2340 0.5337 0.045 1.000 . Uiso c ? H(3) 0.5518 0.2821 0.5509 0.045 1.000 . Uiso c ? H(4) 0.4608 0.1686 0.5222 0.034 1.000 . Uiso c ? H(5) 0.4153 0.2277 0.5278 0.034 1.000 . Uiso c ? H(6) 0.2337 0.2489 0.5867 0.043 1.000 . Uiso c ? H(7) 0.2169 0.2442 0.5378 0.043 1.000 . Uiso c ? H(8) 0.1455 0.2125 0.5690 0.043 1.000 . Uiso c ? H(9) 0.2525 0.1801 0.4703 0.040 1.000 . Uiso c ? H(10) 0.1810 0.1274 0.4161 0.052 1.000 . Uiso c ? H(11) 0.1390 0.0339 0.4280 0.058 1.000 . Uiso c ? H(12) 0.1707 -0.0064 0.4944 0.053 1.000 . Uiso c ? H(13) 0.3212 -0.0573 0.5954 0.057 1.000 . Uiso c ? H(14) 0.2930 -0.0556 0.5473 0.057 1.000 . Uiso c ? H(15) 0.3922 -0.0271 0.5632 0.057 1.000 . Uiso c ? H(16) 0.0654 0.0328 0.5906 0.058 1.000 . Uiso c ? H(17) 0.0974 -0.0242 0.5716 0.058 1.000 . Uiso c ? H(18) 0.1145 -0.0120 0.6198 0.058 1.000 . Uiso c ? H(19) 0.6072 0.1607 0.6134 0.036 1.000 . Uiso c ? H(20) 0.6183 0.1472 0.5652 0.036 1.000 . Uiso c ? H(21) 0.4783 0.0155 0.5410 0.048 1.000 . Uiso c ? H(22) 0.4934 0.0723 0.5185 0.048 1.000 . Uiso c ? H(23) 0.5862 0.0421 0.5389 0.048 1.000 . Uiso c ? H(24) 0.7028 0.0473 0.6083 0.045 1.000 . Uiso c ? H(25) 0.7869 -0.0058 0.6604 0.052 1.000 . Uiso c ? H(26) 0.6944 -0.0449 0.7165 0.052 1.000 . Uiso c ? H(27) 0.5230 -0.0251 0.7242 0.041 1.000 . Uiso c ? H(28) 0.3874 0.0353 0.7538 0.050 1.000 . Uiso c ? H(29) 0.3801 0.0974 0.7407 0.050 1.000 . Uiso c ? H(30) 0.2816 0.0617 0.7442 0.050 1.000 . Uiso c ? H(31) 0.2350 -0.0290 0.6900 0.050 1.000 . Uiso c ? H(32) 0.3036 -0.0492 0.6527 0.050 1.000 . Uiso c ? H(33) 0.3412 -0.0549 0.6995 0.050 1.000 . Uiso c ? H(34) 0.4148 0.2597 0.6067 0.036 1.000 . Uiso c ? H(35) 0.5157 0.2511 0.6319 0.036 1.000 . Uiso c ? H(36) 0.4615 0.1521 0.7237 0.044 1.000 . Uiso c ? H(37) 0.5517 0.1624 0.6925 0.044 1.000 . Uiso c ? H(38) 0.4987 0.2122 0.7148 0.044 1.000 . Uiso c ? H(39) 0.3637 0.2922 0.6978 0.040 1.000 . Uiso c ? H(40) 0.2264 0.3411 0.7261 0.052 1.000 . Uiso c ? H(41) 0.0621 0.3054 0.7208 0.050 1.000 . Uiso c ? H(42) 0.0334 0.2193 0.6890 0.044 1.000 . Uiso c ? H(43) -0.0062 0.1553 0.6295 0.040 1.000 . Uiso c ? H(44) 0.0638 0.1554 0.5895 0.040 1.000 . Uiso c ? H(45) 0.0231 0.0997 0.6077 0.040 1.000 . Uiso c ? H(46) 0.0537 0.1118 0.7108 0.044 1.000 . Uiso c ? H(47) 0.0824 0.0558 0.6893 0.044 1.000 . Uiso c ? H(48) 0.1590 0.0847 0.7200 0.044 1.000 . Uiso c ? H(49) 0.4490 0.4002 0.8585 0.200 1.000 . Uiso c ? H(50) 0.4222 0.3375 0.8550 0.200 1.000 . Uiso c ? H(51) 0.3452 0.3785 0.8757 0.200 1.000 . Uiso c ? H(52) 0.4595 0.2878 0.9420 0.201 1.000 . Uiso c ? H(53) 0.4878 0.2843 0.8939 0.201 1.000 . Uiso c ? H(54) 0.5677 0.3053 0.9268 0.201 1.000 . Uiso c ? 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 As(1) 0.0218(5) 0.0247(5) 0.0239(5) 0.0007(4) -0.0012(4) 0.0030(4) As(2) 0.0325(5) 0.0252(5) 0.0251(5) -0.0022(5) -0.0027(5) -0.0002(4) As(3) 0.0212(5) 0.0288(5) 0.0233(5) 0.0035(4) 0.0014(4) 0.0024(4) As(4) 0.0272(5) 0.0272(5) 0.0229(5) -0.0013(4) -0.0007(4) 0.0035(4) As(5) 0.0176(5) 0.0265(5) 0.0253(5) -0.0031(4) 0.0006(4) -0.0015(4) As(6) 0.0169(5) 0.0292(5) 0.0272(5) -0.0024(4) 0.0008(4) -0.0006(4) Co(1) 0.0192(7) 0.0234(7) 0.0229(7) -0.0004(6) 0.0004(6) 0.0023(6) P(1) 0.043(2) 0.032(1) 0.041(2) 0.003(1) 0.006(1) -0.002(1) P(2) 0.025(1) 0.054(2) 0.045(2) 0.001(1) 0.002(1) -0.002(1) P(3) 0.043(2) 0.042(2) 0.057(2) -0.005(1) -0.002(1) 0.005(1) F(1) 0.25(1) 0.047(5) 0.158(9) -0.042(6) 0.104(9) -0.005(5) F(2) 0.148(8) 0.082(6) 0.123(7) 0.031(6) 0.092(6) 0.022(5) F(3) 0.21(1) 0.24(1) 0.099(7) 0.17(1) -0.112(7) -0.098(7) F(4) 0.090(6) 0.046(4) 0.146(7) -0.008(4) 0.028(5) -0.004(4) F(5) 0.073(5) 0.104(6) 0.088(5) 0.010(5) 0.043(4) -0.015(5) F(6) 0.117(7) 0.158(9) 0.150(9) 0.074(7) -0.067(7) -0.079(7) F(7) 0.058(4) 0.081(5) 0.110(6) -0.012(4) 0.010(4) 0.027(5) F(8) 0.033(3) 0.067(4) 0.062(4) 0.013(3) 0.002(3) -0.009(3) F(9) 0.071(5) 0.098(5) 0.067(5) 0.010(4) -0.025(4) -0.015(4) F(10) 0.083(5) 0.065(5) 0.127(7) -0.004(4) 0.051(5) 0.021(5) F(11) 0.041(4) 0.069(5) 0.115(6) 0.014(3) -0.003(4) -0.018(4) F(12) 0.103(6) 0.103(6) 0.062(5) 0.034(5) -0.034(4) -0.030(4) F(13) 0.129(8) 0.22(1) 0.077(6) -0.085(8) 0.027(6) -0.084(7) F(14) 0.073(5) 0.157(8) 0.126(7) -0.056(6) -0.010(5) 0.061(6) F(15) 0.154(9) 0.048(5) 0.25(1) 0.003(5) -0.115(9) 0.022(6) F(16) 0.113(7) 0.103(6) 0.079(5) -0.024(5) 0.025(5) -0.015(5) F(17) 0.055(4) 0.121(6) 0.078(5) -0.026(4) 0.017(4) -0.026(5) F(18) 0.108(7) 0.081(6) 0.145(8) 0.021(5) -0.034(6) 0.022(6) O(1) 0.106(9) 0.128(9) 0.17(1) -0.065(8) 0.050(8) -0.095(9) C(1) 0.029(5) 0.043(6) 0.040(6) -0.012(5) 0.004(5) 0.012(5) C(2) 0.025(5) 0.028(5) 0.029(5) -0.004(4) 0.000(4) 0.009(4) C(3) 0.024(5) 0.025(5) 0.036(5) 0.002(4) 0.007(4) 0.006(4) C(4) 0.027(5) 0.033(5) 0.047(6) 0.007(4) 0.003(5) 0.007(5) C(5) 0.021(5) 0.037(5) 0.027(5) 0.002(4) -0.001(4) 0.002(4) C(6) 0.036(6) 0.033(5) 0.032(5) 0.002(5) 0.000(5) 0.001(4) C(7) 0.058(7) 0.048(6) 0.024(5) 0.008(6) -0.012(5) 0.000(5) C(8) 0.059(7) 0.056(7) 0.031(6) 0.004(6) -0.015(5) -0.013(5) C(9) 0.048(7) 0.041(6) 0.042(6) -0.013(5) -0.012(5) -0.006(5) C(10) 0.026(5) 0.032(5) 0.025(5) 0.001(4) -0.008(4) 0.000(4) C(11) 0.071(8) 0.029(5) 0.042(6) 0.005(5) -0.001(6) -0.007(5) C(12) 0.059(7) 0.042(6) 0.043(6) -0.017(6) 0.001(6) -0.004(5) C(13) 0.020(5) 0.037(5) 0.032(5) 0.001(4) 0.007(4) 0.004(4) C(14) 0.041(6) 0.047(6) 0.031(5) 0.003(5) 0.004(5) -0.006(5) C(15) 0.025(5) 0.022(5) 0.031(5) 0.005(4) -0.007(4) 0.003(4) C(16) 0.030(5) 0.043(6) 0.038(6) 0.006(5) -0.001(5) 0.000(5) C(17) 0.031(6) 0.046(6) 0.053(7) 0.010(5) -0.009(5) -0.006(5) C(18) 0.042(6) 0.041(6) 0.047(7) 0.012(5) -0.013(5) 0.000(5) C(19) 0.035(6) 0.037(6) 0.031(5) 0.006(5) -0.006(5) 0.008(4) C(20) 0.029(5) 0.022(5) 0.030(5) 0.001(4) -0.009(4) 0.001(4) C(21) 0.055(7) 0.053(6) 0.018(5) 0.005(5) -0.002(5) -0.006(4) C(22) 0.046(6) 0.034(6) 0.046(6) -0.011(5) -0.001(5) 0.012(5) C(23) 0.027(5) 0.030(5) 0.032(5) -0.013(4) -0.003(4) 0.004(4) C(24) 0.032(5) 0.049(6) 0.030(5) -0.004(5) -0.005(4) 0.004(5) C(25) 0.019(5) 0.033(5) 0.022(5) -0.001(4) 0.003(4) 0.001(4) C(26) 0.029(5) 0.028(5) 0.043(6) -0.002(4) 0.003(5) -0.003(4) C(27) 0.055(7) 0.030(6) 0.044(6) 0.004(5) -0.005(5) -0.011(5) C(28) 0.034(6) 0.041(6) 0.049(6) 0.009(5) 0.003(5) -0.008(5) C(29) 0.023(5) 0.044(6) 0.044(6) 0.003(4) 0.002(5) -0.002(5) C(30) 0.026(5) 0.027(5) 0.025(5) 0.002(4) -0.001(4) -0.003(4) C(31) 0.020(5) 0.036(5) 0.042(6) 0.001(4) -0.006(4) -0.005(5) C(32) 0.033(6) 0.032(5) 0.045(6) -0.002(4) 0.006(5) 0.004(5) C(33) 0.050(8) 0.054(8) 0.10(1) -0.005(6) 0.014(8) -0.005(8) C(34) 0.29(3) 0.14(2) 0.07(1) 0.14(2) 0.03(1) 0.04(1) C(35) 0.27(3) 0.17(2) 0.07(1) 0.16(2) 0.01(1) 0.00(1) #- _refine_special_details ; Asymmetric unit comprised of cation, three PF6- anions, acetone molecule and water molecule of occupancy 0.31(2). Hydrogen atoms included at calculated positions, those on water not being located. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _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 5385 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_all 0.0574 _refine_ls_wR_factor_ref 0.0542 _refine_ls_goodness_of_fit_all 1.908 _refine_ls_goodness_of_fit_ref 2.133 _refine_ls_shift/su_max 0.0590 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_min -0.92 _refine_diff_density_max 1.15 #- _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 As(1) Co(1) 2.332(2) . . yes As(1) C(3) 1.946(8) . . yes As(1) C(4) 1.926(9) . . yes As(1) C(5) 1.929(9) . . yes As(2) Co(1) 2.362(2) . . yes As(2) C(10) 1.926(8) . . yes As(2) C(11) 1.94(1) . . yes As(2) C(12) 1.93(1) . . yes As(3) Co(1) 2.342(2) . . yes As(3) C(13) 1.940(9) . . yes As(3) C(14) 1.945(9) . . yes As(3) C(15) 1.924(8) . . yes As(4) Co(1) 2.364(2) . . yes As(4) C(20) 1.961(9) . . yes As(4) C(21) 1.941(8) . . yes As(4) C(22) 1.936(9) . . yes As(5) Co(1) 2.355(2) . . yes As(5) C(23) 1.962(8) . . yes As(5) C(24) 1.942(9) . . yes As(5) C(25) 1.941(8) . . yes As(6) Co(1) 2.360(2) . . yes As(6) C(30) 1.930(8) . . yes As(6) C(31) 1.946(9) . . yes As(6) C(32) 1.923(9) . . yes P(1) F(1) 1.567(7) . . yes P(1) F(2) 1.575(7) . . yes P(1) F(3) 1.489(7) . . yes P(1) F(4) 1.547(7) . . yes P(1) F(5) 1.559(6) . . yes P(1) F(6) 1.559(8) . . yes P(2) F(7) 1.578(7) . . yes P(2) F(8) 1.599(6) . . yes P(2) F(9) 1.585(6) . . yes P(2) F(10) 1.561(7) . . yes P(2) F(11) 1.584(6) . . yes P(2) F(12) 1.563(7) . . yes P(3) F(13) 1.509(7) . . yes P(3) F(14) 1.569(7) . . yes P(3) F(15) 1.537(7) . . yes P(3) F(16) 1.610(8) . . yes P(3) F(17) 1.561(7) . . yes P(3) F(18) 1.557(7) . . yes O(1) C(33) 1.23(1) . . yes C(1) C(2) 1.52(1) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) C(3) 1.55(1) . . yes C(2) C(13) 1.52(1) . . yes C(2) C(23) 1.53(1) . . yes C(3) H(4) 0.95 . . no C(3) H(5) 0.95 . . no C(4) H(6) 0.95 . . no C(4) H(7) 0.95 . . no C(4) H(8) 0.95 . . no C(5) C(6) 1.39(1) . . yes C(5) C(10) 1.41(1) . . yes C(6) C(7) 1.37(1) . . yes C(6) H(9) 0.95 . . no C(7) C(8) 1.39(1) . . yes C(7) H(10) 0.95 . . no C(8) C(9) 1.39(1) . . yes C(8) H(11) 0.95 . . no C(9) C(10) 1.37(1) . . yes C(9) H(12) 0.95 . . no C(11) H(13) 0.95 . . no C(11) H(14) 0.95 . . no C(11) H(15) 0.95 . . no C(12) H(16) 0.95 . . no C(12) H(17) 0.95 . . no C(12) H(18) 0.95 . . no C(13) H(19) 0.95 . . no C(13) H(20) 0.95 . . no C(14) H(21) 0.95 . . no C(14) H(22) 0.95 . . no C(14) H(23) 0.95 . . no C(15) C(16) 1.39(1) . . yes C(15) C(20) 1.36(1) . . yes C(16) C(17) 1.39(1) . . yes C(16) H(24) 0.95 . . no C(17) C(18) 1.38(1) . . yes C(17) H(25) 0.95 . . no C(18) C(19) 1.36(1) . . yes C(18) H(26) 0.95 . . no C(19) C(20) 1.39(1) . . yes C(19) H(27) 0.95 . . no C(21) H(28) 0.95 . . no C(21) H(29) 0.95 . . no C(21) H(30) 0.95 . . no C(22) H(31) 0.95 . . no C(22) H(32) 0.95 . . no C(22) H(33) 0.95 . . no C(23) H(34) 0.95 . . no C(23) H(35) 0.95 . . no C(24) H(36) 0.95 . . no C(24) H(37) 0.95 . . no C(24) H(38) 0.95 . . no C(25) C(26) 1.39(1) . . yes C(25) C(30) 1.36(1) . . yes C(26) C(27) 1.37(1) . . yes C(26) H(39) 0.95 . . no C(27) C(28) 1.38(1) . . yes C(27) H(40) 0.95 . . no C(28) C(29) 1.38(1) . . yes C(28) H(41) 0.95 . . no C(29) C(30) 1.39(1) . . yes C(29) H(42) 0.95 . . no C(31) H(43) 0.95 . . no C(31) H(44) 0.95 . . no C(31) H(45) 0.95 . . no C(32) H(46) 0.95 . . no C(32) H(47) 0.95 . . no C(32) H(48) 0.95 . . no C(33) C(34) 1.45(2) . . yes C(33) C(35) 1.42(2) . . yes C(34) H(49) 0.95 . . no C(34) H(50) 0.95 . . no C(34) H(51) 0.95 . . no C(35) H(52) 0.95 . . no C(35) H(53) 0.95 . . no C(35) H(54) 0.95 . . no #- 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 Co(1) As(1) C(3) 113.7(3) . . . yes Co(1) As(1) C(4) 121.4(3) . . . yes Co(1) As(1) C(5) 108.9(3) . . . yes C(3) As(1) C(4) 102.7(4) . . . yes C(3) As(1) C(5) 105.6(4) . . . yes C(4) As(1) C(5) 103.1(4) . . . yes Co(1) As(2) C(10) 108.0(3) . . . yes Co(1) As(2) C(11) 118.5(3) . . . yes Co(1) As(2) C(12) 122.0(3) . . . yes C(10) As(2) C(11) 104.3(4) . . . yes C(10) As(2) C(12) 101.4(4) . . . yes C(11) As(2) C(12) 100.2(4) . . . yes Co(1) As(3) C(13) 114.6(3) . . . yes Co(1) As(3) C(14) 122.4(3) . . . yes Co(1) As(3) C(15) 108.5(3) . . . yes C(13) As(3) C(14) 100.7(4) . . . yes C(13) As(3) C(15) 105.8(4) . . . yes C(14) As(3) C(15) 103.3(4) . . . yes Co(1) As(4) C(20) 106.9(3) . . . yes Co(1) As(4) C(21) 121.5(3) . . . yes Co(1) As(4) C(22) 121.6(3) . . . yes C(20) As(4) C(21) 103.1(4) . . . yes C(20) As(4) C(22) 102.8(4) . . . yes C(21) As(4) C(22) 98.3(4) . . . yes Co(1) As(5) C(23) 113.4(3) . . . yes Co(1) As(5) C(24) 122.2(3) . . . yes Co(1) As(5) C(25) 107.9(3) . . . yes C(23) As(5) C(24) 102.5(4) . . . yes C(23) As(5) C(25) 104.3(4) . . . yes C(24) As(5) C(25) 104.9(4) . . . yes Co(1) As(6) C(30) 107.6(3) . . . yes Co(1) As(6) C(31) 119.3(3) . . . yes Co(1) As(6) C(32) 121.3(3) . . . yes C(30) As(6) C(31) 104.6(4) . . . yes C(30) As(6) C(32) 102.0(4) . . . yes C(31) As(6) C(32) 99.7(4) . . . yes As(1) Co(1) As(2) 86.67(5) . . . yes As(1) Co(1) As(3) 85.91(5) . . . yes As(1) Co(1) As(4) 172.42(7) . . . yes As(1) Co(1) As(5) 85.25(5) . . . yes As(1) Co(1) As(6) 92.94(6) . . . yes As(2) Co(1) As(3) 94.56(6) . . . yes As(2) Co(1) As(4) 92.78(6) . . . yes As(2) Co(1) As(5) 171.77(7) . . . yes As(2) Co(1) As(6) 92.93(6) . . . yes As(3) Co(1) As(4) 86.59(5) . . . yes As(3) Co(1) As(5) 86.36(6) . . . yes As(3) Co(1) As(6) 172.34(7) . . . yes As(4) Co(1) As(5) 95.43(6) . . . yes As(4) Co(1) As(6) 94.64(6) . . . yes As(5) Co(1) As(6) 86.00(5) . . . yes F(1) P(1) F(2) 92.4(5) . . . yes F(1) P(1) F(3) 90.4(6) . . . yes F(1) P(1) F(4) 174.0(6) . . . yes F(1) P(1) F(5) 84.7(4) . . . yes F(1) P(1) F(6) 87.3(6) . . . yes F(2) P(1) F(3) 90.0(5) . . . yes F(2) P(1) F(4) 87.0(4) . . . yes F(2) P(1) F(5) 176.0(5) . . . yes F(2) P(1) F(6) 88.0(5) . . . yes F(3) P(1) F(4) 95.5(6) . . . yes F(3) P(1) F(5) 92.8(5) . . . yes F(3) P(1) F(6) 176.9(7) . . . yes F(4) P(1) F(5) 95.7(4) . . . yes F(4) P(1) F(6) 86.7(5) . . . yes F(5) P(1) F(6) 89.1(5) . . . yes F(7) P(2) F(8) 89.7(4) . . . yes F(7) P(2) F(9) 89.5(4) . . . yes F(7) P(2) F(10) 177.9(4) . . . yes F(7) P(2) F(11) 91.4(4) . . . yes F(7) P(2) F(12) 88.3(4) . . . yes F(8) P(2) F(9) 89.5(4) . . . yes F(8) P(2) F(10) 88.9(4) . . . yes F(8) P(2) F(11) 178.9(4) . . . yes F(8) P(2) F(12) 89.2(3) . . . yes F(9) P(2) F(10) 89.1(4) . . . yes F(9) P(2) F(11) 90.4(4) . . . yes F(9) P(2) F(12) 177.4(4) . . . yes F(10) P(2) F(11) 90.0(4) . . . yes F(10) P(2) F(12) 93.2(5) . . . yes F(11) P(2) F(12) 90.9(4) . . . yes F(13) P(3) F(14) 87.6(5) . . . yes F(13) P(3) F(15) 95.8(6) . . . yes F(13) P(3) F(16) 178.4(6) . . . yes F(13) P(3) F(17) 92.8(4) . . . yes F(13) P(3) F(18) 92.3(6) . . . yes F(14) P(3) F(15) 88.3(5) . . . yes F(14) P(3) F(16) 92.6(5) . . . yes F(14) P(3) F(17) 179.6(5) . . . yes F(14) P(3) F(18) 89.2(5) . . . yes F(15) P(3) F(16) 85.8(5) . . . yes F(15) P(3) F(17) 91.6(5) . . . yes F(15) P(3) F(18) 171.4(6) . . . yes F(16) P(3) F(17) 87.1(4) . . . yes F(16) P(3) F(18) 86.1(5) . . . yes F(17) P(3) F(18) 90.8(5) . . . yes C(2) C(1) H(1) 109.5 . . . no C(2) C(1) H(2) 109.5 . . . no C(2) C(1) H(3) 109.5 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 109.5 . . . no H(2) C(1) H(3) 109.5 . . . no C(1) C(2) C(3) 108.4(7) . . . yes C(1) C(2) C(13) 108.4(7) . . . yes C(1) C(2) C(23) 107.4(7) . . . yes C(3) C(2) C(13) 109.7(7) . . . yes C(3) C(2) C(23) 111.2(7) . . . yes C(13) C(2) C(23) 111.7(7) . . . yes As(1) C(3) C(2) 116.0(6) . . . yes As(1) C(3) H(4) 107.8 . . . no As(1) C(3) H(5) 107.8 . . . no C(2) C(3) H(4) 107.8 . . . no C(2) C(3) H(5) 107.8 . . . no H(4) C(3) H(5) 109.4 . . . no As(1) C(4) H(6) 109.5 . . . no As(1) C(4) H(7) 109.5 . . . no As(1) C(4) H(8) 109.5 . . . no H(6) C(4) H(7) 109.5 . . . no H(6) C(4) H(8) 109.5 . . . no H(7) C(4) H(8) 109.5 . . . no As(1) C(5) C(6) 121.5(7) . . . yes As(1) C(5) C(10) 117.8(6) . . . yes C(6) C(5) C(10) 120.6(8) . . . yes C(5) C(6) C(7) 119.6(9) . . . yes C(5) C(6) H(9) 120.2 . . . no C(7) C(6) H(9) 120.2 . . . no C(6) C(7) C(8) 120.5(9) . . . yes C(6) C(7) H(10) 119.8 . . . no C(8) C(7) H(10) 119.8 . . . no C(7) C(8) C(9) 119.8(9) . . . yes C(7) C(8) H(11) 120.1 . . . no C(9) C(8) H(11) 120.1 . . . no C(8) C(9) C(10) 120.8(9) . . . yes C(8) C(9) H(12) 119.6 . . . no C(10) C(9) H(12) 119.6 . . . no As(2) C(10) C(5) 118.3(6) . . . yes As(2) C(10) C(9) 123.0(7) . . . yes C(5) C(10) C(9) 118.7(8) . . . yes As(2) C(11) H(13) 109.5 . . . no As(2) C(11) H(14) 109.5 . . . no As(2) C(11) H(15) 109.5 . . . no H(13) C(11) H(14) 109.5 . . . no H(13) C(11) H(15) 109.5 . . . no H(14) C(11) H(15) 109.5 . . . no As(2) C(12) H(16) 109.5 . . . no As(2) C(12) H(17) 109.5 . . . no As(2) C(12) H(18) 109.5 . . . no H(16) C(12) H(17) 109.5 . . . no H(16) C(12) H(18) 109.5 . . . no H(17) C(12) H(18) 109.5 . . . no As(3) C(13) C(2) 116.1(6) . . . yes As(3) C(13) H(19) 107.8 . . . no As(3) C(13) H(20) 107.8 . . . no C(2) C(13) H(19) 107.8 . . . no C(2) C(13) H(20) 107.8 . . . no H(19) C(13) H(20) 109.5 . . . no As(3) C(14) H(21) 109.5 . . . no As(3) C(14) H(22) 109.5 . . . no As(3) C(14) H(23) 109.5 . . . no H(21) C(14) H(22) 109.5 . . . no H(21) C(14) H(23) 109.5 . . . no H(22) C(14) H(23) 109.5 . . . no As(3) C(15) C(16) 121.1(7) . . . yes As(3) C(15) C(20) 118.9(6) . . . yes C(16) C(15) C(20) 119.9(8) . . . yes C(15) C(16) C(17) 118.9(9) . . . yes C(15) C(16) H(24) 120.5 . . . no C(17) C(16) H(24) 120.5 . . . no C(16) C(17) C(18) 120.3(9) . . . yes C(16) C(17) H(25) 119.9 . . . no C(18) C(17) H(25) 119.9 . . . no C(17) C(18) C(19) 120.0(9) . . . yes C(17) C(18) H(26) 120.0 . . . no C(19) C(18) H(26) 120.0 . . . no C(18) C(19) C(20) 120.0(9) . . . yes C(18) C(19) H(27) 120.0 . . . no C(20) C(19) H(27) 120.0 . . . no As(4) C(20) C(15) 118.4(6) . . . yes As(4) C(20) C(19) 120.9(7) . . . yes C(15) C(20) C(19) 120.6(8) . . . yes As(4) C(21) H(28) 109.5 . . . no As(4) C(21) H(29) 109.5 . . . no As(4) C(21) H(30) 109.5 . . . no H(28) C(21) H(29) 109.5 . . . no H(28) C(21) H(30) 109.5 . . . no H(29) C(21) H(30) 109.5 . . . no As(4) C(22) H(31) 109.5 . . . no As(4) C(22) H(32) 109.5 . . . no As(4) C(22) H(33) 109.5 . . . no H(31) C(22) H(32) 109.5 . . . no H(31) C(22) H(33) 109.5 . . . no H(32) C(22) H(33) 109.5 . . . no As(5) C(23) C(2) 116.6(6) . . . yes As(5) C(23) H(34) 107.6 . . . no As(5) C(23) H(35) 107.6 . . . no C(2) C(23) H(34) 107.7 . . . no C(2) C(23) H(35) 107.7 . . . no H(34) C(23) H(35) 109.5 . . . no As(5) C(24) H(36) 109.5 . . . no As(5) C(24) H(37) 109.5 . . . no As(5) C(24) H(38) 109.5 . . . no H(36) C(24) H(37) 109.5 . . . no H(36) C(24) H(38) 109.5 . . . no H(37) C(24) H(38) 109.5 . . . no As(5) C(25) C(26) 120.6(6) . . . yes As(5) C(25) C(30) 118.2(6) . . . yes C(26) C(25) C(30) 121.2(8) . . . yes C(25) C(26) C(27) 119.2(9) . . . yes C(25) C(26) H(39) 120.4 . . . no C(27) C(26) H(39) 120.4 . . . no C(26) C(27) C(28) 120.0(9) . . . yes C(26) C(27) H(40) 120.0 . . . no C(28) C(27) H(40) 120.0 . . . no C(27) C(28) C(29) 120.9(9) . . . yes C(27) C(28) H(41) 119.5 . . . no C(29) C(28) H(41) 119.6 . . . no C(28) C(29) C(30) 119.1(9) . . . yes C(28) C(29) H(42) 120.5 . . . no C(30) C(29) H(42) 120.5 . . . no As(6) C(30) C(25) 118.9(6) . . . yes As(6) C(30) C(29) 121.4(7) . . . yes C(25) C(30) C(29) 119.6(8) . . . yes As(6) C(31) H(43) 109.5 . . . no As(6) C(31) H(44) 109.5 . . . no As(6) C(31) H(45) 109.5 . . . no H(43) C(31) H(44) 109.5 . . . no H(43) C(31) H(45) 109.5 . . . no H(44) C(31) H(45) 109.5 . . . no As(6) C(32) H(46) 109.5 . . . no As(6) C(32) H(47) 109.5 . . . no As(6) C(32) H(48) 109.5 . . . no H(46) C(32) H(47) 109.5 . . . no H(46) C(32) H(48) 109.5 . . . no H(47) C(32) H(48) 109.5 . . . no O(1) C(33) C(34) 123(1) . . . yes O(1) C(33) C(35) 123(2) . . . yes C(34) C(33) C(35) 114(1) . . . yes C(33) C(34) H(49) 109.5 . . . no C(33) C(34) H(50) 109.5 . . . no C(33) C(34) H(51) 109.5 . . . no H(49) C(34) H(50) 109.5 . . . no H(49) C(34) H(51) 109.5 . . . no H(50) C(34) H(51) 109.4 . . . no C(33) C(35) H(52) 109.5 . . . no C(33) C(35) H(53) 109.5 . . . no C(33) C(35) H(54) 109.5 . . . no H(52) C(35) H(53) 109.4 . . . no H(52) C(35) H(54) 109.5 . . . no H(53) C(35) H(54) 109.5 . . . no #- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(32) 3.31(1) . . no F(1) C(12) 3.47(1) . . no F(1) C(19) 3.58(1) . 8_456 no F(2) O(2) 2.68(4) . . no F(2) C(12) 3.42(1) . . no F(2) C(26) 3.50(1) . 6_545 no F(3) C(7) 3.30(1) . 5_556 no F(3) C(17) 3.31(1) . 1_455 no F(3) C(8) 3.44(1) . 5_556 no F(4) F(11) 3.297(9) . 3_546 no F(4) C(26) 3.48(1) . 6_545 no F(4) C(28) 3.56(1) . 3_546 no F(4) C(23) 3.56(1) . 6_545 no F(5) C(22) 3.52(1) . 8_456 no F(5) C(18) 3.53(1) . 1_455 no F(6) C(19) 3.30(1) . 8_456 no F(6) C(18) 3.48(1) . 8_456 no F(6) C(26) 3.48(1) . 6_545 no F(7) C(26) 3.24(1) . . no F(7) C(29) 3.33(1) . 8_556 no F(7) C(27) 3.42(1) . . no F(8) C(21) 3.21(1) . . no F(8) C(31) 3.29(1) . 8_556 no F(8) C(32) 3.30(1) . 8_556 no F(8) C(29) 3.33(1) . 8_556 no F(8) C(24) 3.50(1) . . no F(9) C(25) 3.16(1) . . no F(9) C(30) 3.17(1) . . no F(9) C(26) 3.36(1) . . no F(9) C(29) 3.38(1) . . no F(9) C(21) 3.41(1) . . no F(9) C(24) 3.44(1) . 8_456 no F(9) C(27) 3.53(1) . . no F(9) C(28) 3.54(1) . . no F(10) C(16) 3.04(1) . 8_456 no F(10) C(13) 3.24(1) . 8_456 no F(10) C(15) 3.47(1) . 8_456 no F(10) C(17) 3.49(1) . 8_456 no F(10) C(24) 3.55(1) . 8_456 no F(11) C(24) 3.21(1) . 8_456 no F(11) C(23) 3.53(1) . 8_456 no F(12) C(31) 3.32(1) . 8_556 no F(12) F(13) 3.46(1) . . no F(12) C(35) 3.52(2) . . no F(13) C(31) 3.16(1) . 8_556 no F(14) C(11) 3.22(1) . 4 no F(14) O(2) 3.57(4) . 4 no F(15) C(9) 3.23(1) . 4 no F(15) C(12) 3.45(1) . 4 no F(16) O(2) 2.65(4) . 4 no F(16) C(4) 3.33(1) . 7 no F(16) C(3) 3.37(1) . 7 no F(16) C(1) 3.55(1) . 7 no F(17) C(31) 3.26(1) . 8_556 no F(17) C(1) 3.49(1) . 7 no F(18) C(1) 3.33(1) . 8_456 no F(18) C(4) 3.56(1) . 7 no O(1) C(11) 3.24(1) . 3_656 no O(1) C(6) 3.33(1) . 7 no O(1) C(14) 3.45(1) . 7 no O(1) C(7) 3.57(2) . 7 no O(2) C(11) 3.20(5) . . no O(2) C(26) 3.30(4) . 6_545 no O(2) C(4) 3.47(5) . 6_545 no O(2) C(27) 3.52(4) . 6_545 no C(1) C(6) 3.41(1) . 2_556 no C(4) C(35) 3.46(2) . 8_456 no C(6) C(33) 3.54(2) . 7_554 no C(14) C(14) 3.55(2) . 5_656 no C(18) C(34) 3.52(2) . 3_646 no #- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag As(1) Co(1) As(2) C(10) . . . . 5.1(3) no As(1) Co(1) As(2) C(11) . . . . 123.2(3) no As(1) Co(1) As(2) C(12) . . . . -111.6(4) no As(1) Co(1) As(3) C(13) . . . . 56.2(3) no As(1) Co(1) As(3) C(14) . . . . -65.9(3) no As(1) Co(1) As(3) C(15) . . . . 174.2(3) no As(1) Co(1) As(4) C(20) . . . . 16.2(6) no As(1) Co(1) As(4) C(21) . . . . 133.8(6) no As(1) Co(1) As(4) C(22) . . . . -101.1(6) no As(1) Co(1) As(5) C(23) . . . . -31.2(3) no As(1) Co(1) As(5) C(24) . . . . -154.7(3) no As(1) Co(1) As(5) C(25) . . . . 83.8(3) no As(1) Co(1) As(6) C(30) . . . . -74.5(3) no As(1) Co(1) As(6) C(31) . . . . 44.3(3) no As(1) Co(1) As(6) C(32) . . . . 168.9(3) no As(1) C(3) C(2) C(1) . . . . -160.2(6) no As(1) C(3) C(2) C(13) . . . . 81.6(8) no As(1) C(3) C(2) C(23) . . . . -42.4(8) no As(1) C(5) C(6) C(7) . . . . -177.1(7) no As(1) C(5) C(10) As(2) . . . . 1(1) no As(1) C(5) C(10) C(9) . . . . 177.7(7) no As(2) Co(1) As(1) C(3) . . . . -122.2(3) no As(2) Co(1) As(1) C(4) . . . . 114.5(3) no As(2) Co(1) As(1) C(5) . . . . -4.7(3) no As(2) Co(1) As(3) C(13) . . . . 142.6(3) no As(2) Co(1) As(3) C(14) . . . . 20.4(3) no As(2) Co(1) As(3) C(15) . . . . -99.5(3) no As(2) Co(1) As(4) C(20) . . . . 101.8(3) no As(2) Co(1) As(4) C(21) . . . . -140.5(4) no As(2) Co(1) As(4) C(22) . . . . -15.4(4) no As(2) Co(1) As(5) C(23) . . . . -41.7(6) no As(2) Co(1) As(5) C(24) . . . . -165.2(6) no As(2) Co(1) As(5) C(25) . . . . 73.2(6) no As(2) Co(1) As(6) C(30) . . . . -161.3(3) no As(2) Co(1) As(6) C(31) . . . . -42.5(3) no As(2) Co(1) As(6) C(32) . . . . 82.1(3) no As(2) C(10) C(5) C(6) . . . . -178.0(7) no As(2) C(10) C(9) C(8) . . . . 176.5(8) no As(3) Co(1) As(1) C(3) . . . . -27.3(3) no As(3) Co(1) As(1) C(4) . . . . -150.7(3) no As(3) Co(1) As(1) C(5) . . . . 90.1(3) no As(3) Co(1) As(2) C(10) . . . . -80.6(3) no As(3) Co(1) As(2) C(11) . . . . 37.6(3) no As(3) Co(1) As(2) C(12) . . . . 162.8(4) no As(3) Co(1) As(4) C(20) . . . . 7.4(3) no As(3) Co(1) As(4) C(21) . . . . 125.1(4) no As(3) Co(1) As(4) C(22) . . . . -109.8(4) no As(3) Co(1) As(5) C(23) . . . . 55.0(3) no As(3) Co(1) As(5) C(24) . . . . -68.5(3) no As(3) Co(1) As(5) C(25) . . . . 170.0(3) no As(3) Co(1) As(6) C(30) . . . . 6.7(6) no As(3) Co(1) As(6) C(31) . . . . 125.5(6) no As(3) Co(1) As(6) C(32) . . . . -110.0(6) no As(3) C(13) C(2) C(1) . . . . -162.6(6) no As(3) C(13) C(2) C(3) . . . . -44.4(9) no As(3) C(13) C(2) C(23) . . . . 79.3(8) no As(3) C(15) C(16) C(17) . . . . 179.3(7) no As(3) C(15) C(20) As(4) . . . . 1.6(9) no As(3) C(15) C(20) C(19) . . . . 178.1(7) no As(4) Co(1) As(1) C(3) . . . . -36.1(6) no As(4) Co(1) As(1) C(4) . . . . -159.4(6) no As(4) Co(1) As(1) C(5) . . . . 81.3(6) no As(4) Co(1) As(2) C(10) . . . . -167.4(3) no As(4) Co(1) As(2) C(11) . . . . -49.2(3) no As(4) Co(1) As(2) C(12) . . . . 76.0(4) no As(4) Co(1) As(3) C(13) . . . . -124.9(3) no As(4) Co(1) As(3) C(14) . . . . 112.9(3) no As(4) Co(1) As(3) C(15) . . . . -6.9(3) no As(4) Co(1) As(5) C(23) . . . . 141.2(3) no As(4) Co(1) As(5) C(24) . . . . 17.8(3) no As(4) Co(1) As(5) C(25) . . . . -103.8(3) no As(4) Co(1) As(6) C(30) . . . . 105.7(3) no As(4) Co(1) As(6) C(31) . . . . -135.5(3) no As(4) Co(1) As(6) C(32) . . . . -11.0(3) no As(4) C(20) C(15) C(16) . . . . 178.4(7) no As(4) C(20) C(19) C(18) . . . . 179.9(7) no As(5) Co(1) As(1) C(3) . . . . 59.3(3) no As(5) Co(1) As(1) C(4) . . . . -64.0(3) no As(5) Co(1) As(1) C(5) . . . . 176.8(3) no As(5) Co(1) As(2) C(10) . . . . 15.6(6) no As(5) Co(1) As(2) C(11) . . . . 133.7(6) no As(5) Co(1) As(2) C(12) . . . . -101.0(6) no As(5) Co(1) As(3) C(13) . . . . -29.2(3) no As(5) Co(1) As(3) C(14) . . . . -151.4(3) no As(5) Co(1) As(3) C(15) . . . . 88.7(3) no As(5) Co(1) As(4) C(20) . . . . -78.6(3) no As(5) Co(1) As(4) C(21) . . . . 39.0(4) no As(5) Co(1) As(4) C(22) . . . . 164.1(4) no As(5) Co(1) As(6) C(30) . . . . 10.5(3) no As(5) Co(1) As(6) C(31) . . . . 129.3(3) no As(5) Co(1) As(6) C(32) . . . . -106.1(3) no As(5) C(23) C(2) C(1) . . . . -163.6(6) no As(5) C(23) C(2) C(3) . . . . 78.1(8) no As(5) C(23) C(2) C(13) . . . . -44.8(9) no As(5) C(25) C(26) C(27) . . . . -178.2(7) no As(5) C(25) C(30) As(6) . . . . 3(1) no As(5) C(25) C(30) C(29) . . . . 179.1(7) no As(6) Co(1) As(1) C(3) . . . . 145.1(3) no As(6) Co(1) As(1) C(4) . . . . 21.8(3) no As(6) Co(1) As(1) C(5) . . . . -97.5(3) no As(6) Co(1) As(2) C(10) . . . . 97.8(3) no As(6) Co(1) As(2) C(11) . . . . -144.0(3) no As(6) Co(1) As(2) C(12) . . . . -18.8(4) no As(6) Co(1) As(3) C(13) . . . . -25.4(6) no As(6) Co(1) As(3) C(14) . . . . -147.5(6) no As(6) Co(1) As(3) C(15) . . . . 92.6(6) no As(6) Co(1) As(4) C(20) . . . . -165.0(3) no As(6) Co(1) As(4) C(21) . . . . -47.4(4) no As(6) Co(1) As(4) C(22) . . . . 77.7(4) no As(6) Co(1) As(5) C(23) . . . . -124.5(3) no As(6) Co(1) As(5) C(24) . . . . 112.0(3) no As(6) Co(1) As(5) C(25) . . . . -9.5(3) no As(6) C(30) C(25) C(26) . . . . -176.3(6) no As(6) C(30) C(29) C(28) . . . . 175.9(7) no Co(1) As(1) C(3) C(2) . . . . -33.5(7) no Co(1) As(1) C(5) C(6) . . . . -177.8(7) no Co(1) As(1) C(5) C(10) . . . . 3.4(7) no Co(1) As(2) C(10) C(5) . . . . -4.7(7) no Co(1) As(2) C(10) C(9) . . . . 178.6(7) no Co(1) As(3) C(13) C(2) . . . . -30.2(7) no Co(1) As(3) C(15) C(16) . . . . -172.0(7) no Co(1) As(3) C(15) C(20) . . . . 4.8(7) no Co(1) As(4) C(20) C(15) . . . . -7.1(7) no Co(1) As(4) C(20) C(19) . . . . 176.3(7) no Co(1) As(5) C(23) C(2) . . . . -29.1(7) no Co(1) As(5) C(25) C(26) . . . . -174.7(6) no Co(1) As(5) C(25) C(30) . . . . 6.3(7) no Co(1) As(6) C(30) C(25) . . . . -10.4(8) no Co(1) As(6) C(30) C(29) . . . . 173.2(7) no C(2) C(3) As(1) C(4) . . . . 99.5(6) no C(2) C(3) As(1) C(5) . . . . -152.8(6) no C(2) C(13) As(3) C(14) . . . . 103.1(7) no C(2) C(13) As(3) C(15) . . . . -149.7(6) no C(2) C(23) As(5) C(24) . . . . 104.6(7) no C(2) C(23) As(5) C(25) . . . . -146.2(6) no C(3) As(1) C(5) C(6) . . . . -55.3(8) no C(3) As(1) C(5) C(10) . . . . 125.9(7) no C(4) As(1) C(5) C(6) . . . . 52.1(8) no C(4) As(1) C(5) C(10) . . . . -126.7(7) no C(5) C(6) C(7) C(8) . . . . -1(2) no C(5) C(10) As(2) C(11) . . . . -131.5(7) no C(5) C(10) As(2) C(12) . . . . 124.7(7) no C(5) C(10) C(9) C(8) . . . . 0(2) no C(6) C(5) C(10) C(9) . . . . -1(1) no C(6) C(7) C(8) C(9) . . . . 0(2) no C(7) C(6) C(5) C(10) . . . . 2(1) no C(7) C(8) C(9) C(10) . . . . 1(2) no C(9) C(10) As(2) C(11) . . . . 51.7(9) no C(9) C(10) As(2) C(12) . . . . -52.1(9) no C(13) As(3) C(15) C(16) . . . . -48.6(8) no C(13) As(3) C(15) C(20) . . . . 128.2(7) no C(14) As(3) C(15) C(16) . . . . 56.8(8) no C(14) As(3) C(15) C(20) . . . . -126.4(7) no C(15) C(16) C(17) C(18) . . . . 2(2) no C(15) C(20) As(4) C(21) . . . . -136.2(7) no C(15) C(20) As(4) C(22) . . . . 122.0(7) no C(15) C(20) C(19) C(18) . . . . 3(1) no C(16) C(15) C(20) C(19) . . . . -5(1) no C(16) C(17) C(18) C(19) . . . . -3(2) no C(17) C(16) C(15) C(20) . . . . 2(1) no C(17) C(18) C(19) C(20) . . . . 1(2) no C(19) C(20) As(4) C(21) . . . . 47.2(8) no C(19) C(20) As(4) C(22) . . . . -54.6(8) no C(23) As(5) C(25) C(26) . . . . -53.8(8) no C(23) As(5) C(25) C(30) . . . . 127.2(7) no C(24) As(5) C(25) C(26) . . . . 53.6(8) no C(24) As(5) C(25) C(30) . . . . -125.4(7) no C(25) C(26) C(27) C(28) . . . . -1(2) no C(25) C(30) As(6) C(31) . . . . -138.2(7) no C(25) C(30) As(6) C(32) . . . . 118.2(7) no C(25) C(30) C(29) C(28) . . . . 0(1) no C(26) C(25) C(30) C(29) . . . . 0(1) no C(26) C(27) C(28) C(29) . . . . 1(2) no C(27) C(26) C(25) C(30) . . . . 1(1) no C(27) C(28) C(29) C(30) . . . . 0(2) no C(29) C(30) As(6) C(31) . . . . 45.4(8) no C(29) C(30) As(6) C(32) . . . . -58.2(8) no #- #===END