# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1a _database_code_depnum_ccdc_archive 'CCDC 873509' #TrackingRef '10373_web_deposit_cif_file_0_JoseGoicoechea_1332849746.1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)][P3C2H2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C18 H36 K N2 O6, C2 H2 P3' _chemical_formula_sum 'C20 H38 K N2 O6 P3' _chemical_formula_weight 534.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9714(3) _cell_length_b 10.8313(2) _cell_length_c 25.5105(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.071(3) _cell_angle_gamma 90.00 _cell_volume 2734.26(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7564 _cell_measurement_theta_min 3.4887 _cell_measurement_theta_max 76.2371 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 3.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4063 _exptl_absorpt_correction_T_max 0.5279 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.5035 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 14287 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 76.43 _reflns_number_total 5677 _reflns_number_gt 5088 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.9868P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5677 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.36394(5) 0.94471(4) 0.17687(2) 0.04001(12) Uani 1 1 d . . . P2 P 0.51234(5) 1.08005(4) 0.177652(19) 0.04027(12) Uani 1 1 d . . . P3 P 0.50644(7) 1.11098(5) 0.09639(2) 0.05553(15) Uani 1 1 d . . . C1 C 0.3774(2) 1.0036(2) 0.07315(8) 0.0529(5) Uani 1 1 d . . . H1 H 0.3492 0.9951 0.0364 0.063 Uiso 1 1 calc R . . C2 C 0.3183(2) 0.9323(2) 0.10953(8) 0.0470(5) Uani 1 1 d . . . H2 H 0.2503 0.8745 0.0968 0.056 Uiso 1 1 calc R . . K101 K 0.86482(3) 0.47343(3) 0.116481(12) 0.02349(8) Uani 1 1 d . . . N101 N 1.01303(14) 0.23849(13) 0.15050(6) 0.0337(3) Uani 1 1 d . . . N102 N 0.72505(17) 0.71186(15) 0.08151(7) 0.0434(4) Uani 1 1 d . . . O101 O 1.11826(11) 0.48175(12) 0.17406(5) 0.0376(3) Uani 1 1 d . . . O102 O 1.00730(14) 0.70324(11) 0.13112(5) 0.0388(3) Uani 1 1 d . . . O103 O 0.92113(13) 0.29863(12) 0.03838(5) 0.0403(3) Uani 1 1 d . . . O104 O 0.74585(15) 0.50226(16) 0.01014(5) 0.0494(3) Uani 1 1 d . . . O105 O 0.76321(12) 0.32062(10) 0.18838(4) 0.0299(2) Uani 1 1 d . . . O106 O 0.64922(11) 0.55713(10) 0.16756(5) 0.0299(2) Uani 1 1 d . . . C101 C 1.13372(18) 0.26468(19) 0.18796(8) 0.0441(4) Uani 1 1 d . . . H10A H 1.1960 0.1934 0.1887 0.053 Uiso 1 1 calc R . . H10B H 1.1064 0.2738 0.2238 0.053 Uiso 1 1 calc R . . C102 C 1.20792(17) 0.3794(2) 0.17469(9) 0.0464(5) Uani 1 1 d . . . H10C H 1.2874 0.3929 0.2014 0.056 Uiso 1 1 calc R . . H10D H 1.2400 0.3701 0.1397 0.056 Uiso 1 1 calc R . . C103 C 1.18781(19) 0.5954(2) 0.18097(7) 0.0446(5) Uani 1 1 d . . . H10E H 1.2435 0.6081 0.1519 0.053 Uiso 1 1 calc R . . H10F H 1.2486 0.5947 0.2147 0.053 Uiso 1 1 calc R . . C104 C 1.0883(2) 0.69695(18) 0.18132(7) 0.0462(5) Uani 1 1 d . . . H10G H 1.0299 0.6821 0.2094 0.055 Uiso 1 1 calc R . . H10H H 1.1361 0.7763 0.1889 0.055 Uiso 1 1 calc R . . C105 C 0.9316(3) 0.81460(17) 0.12586(11) 0.0566(6) Uani 1 1 d . . . H10I H 0.9929 0.8852 0.1223 0.068 Uiso 1 1 calc R . . H10J H 0.8863 0.8280 0.1578 0.068 Uiso 1 1 calc R . . C106 C 0.8276(3) 0.80748(19) 0.07809(11) 0.0599(6) Uani 1 1 d . . . H10K H 0.7820 0.8885 0.0730 0.072 Uiso 1 1 calc R . . H10L H 0.8740 0.7913 0.0466 0.072 Uiso 1 1 calc R . . C107 C 1.0522(2) 0.17610(17) 0.10354(9) 0.0485(5) Uani 1 1 d . . . H10M H 1.0768 0.0896 0.1129 0.058 Uiso 1 1 calc R . . H10N H 1.1337 0.2171 0.0932 0.058 Uiso 1 1 calc R . . C108 C 0.9450(3) 0.17573(18) 0.05713(9) 0.0545(6) Uani 1 1 d . . . H10O H 0.9739 0.1237 0.0287 0.065 Uiso 1 1 calc R . . H10P H 0.8605 0.1406 0.0676 0.065 Uiso 1 1 calc R . . C109 C 0.8233(2) 0.3017(3) -0.00727(9) 0.0609(6) Uani 1 1 d . . . H10Q H 0.7360 0.2694 0.0017 0.073 Uiso 1 1 calc R . . H10R H 0.8533 0.2485 -0.0352 0.073 Uiso 1 1 calc R . . C110 C 0.8052(2) 0.4306(3) -0.02712(7) 0.0590(6) Uani 1 1 d . . . H11A H 0.8939 0.4660 -0.0327 0.071 Uiso 1 1 calc R . . H11B H 0.7464 0.4311 -0.0614 0.071 Uiso 1 1 calc R . . C111 C 0.7184(3) 0.6242(3) -0.00914(8) 0.0667(7) Uani 1 1 d . . . H11C H 0.6623 0.6209 -0.0439 0.080 Uiso 1 1 calc R . . H11D H 0.8041 0.6668 -0.0136 0.080 Uiso 1 1 calc R . . C112 C 0.6448(3) 0.6938(3) 0.02964(9) 0.0648(7) Uani 1 1 d . . . H11E H 0.6179 0.7756 0.0145 0.078 Uiso 1 1 calc R . . H11F H 0.5612 0.6483 0.0347 0.078 Uiso 1 1 calc R . . C113 C 0.9193(2) 0.16045(15) 0.17602(8) 0.0397(4) Uani 1 1 d . . . H11G H 0.9703 0.0909 0.1940 0.048 Uiso 1 1 calc R . . H11H H 0.8512 0.1254 0.1485 0.048 Uiso 1 1 calc R . . C114 C 0.84734(18) 0.22948(15) 0.21574(7) 0.0349(4) Uani 1 1 d . . . H11I H 0.7920 0.1716 0.2341 0.042 Uiso 1 1 calc R . . H11J H 0.9141 0.2692 0.2425 0.042 Uiso 1 1 calc R . . C115 C 0.68082(18) 0.37967(15) 0.22259(7) 0.0332(3) Uani 1 1 d . . . H11K H 0.7375 0.4305 0.2489 0.040 Uiso 1 1 calc R . . H11L H 0.6334 0.3170 0.2417 0.040 Uiso 1 1 calc R . . C116 C 0.58045(17) 0.45944(16) 0.19016(7) 0.0346(4) Uani 1 1 d . . . H11M H 0.5295 0.4097 0.1618 0.042 Uiso 1 1 calc R . . H11N H 0.5154 0.4938 0.2127 0.042 Uiso 1 1 calc R . . C117 C 0.55761(18) 0.64103(19) 0.13945(8) 0.0419(4) Uani 1 1 d . . . H11O H 0.4922 0.6711 0.1627 0.050 Uiso 1 1 calc R . . H11P H 0.5066 0.5987 0.1089 0.050 Uiso 1 1 calc R . . C118 C 0.6346(2) 0.74811(19) 0.12062(9) 0.0483(5) Uani 1 1 d . . . H11Q H 0.5695 0.8106 0.1046 0.058 Uiso 1 1 calc R . . H11R H 0.6890 0.7868 0.1513 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0349(2) 0.0342(2) 0.0513(3) -0.00774(19) 0.00697(19) -0.00011(17) P2 0.0415(2) 0.0393(2) 0.0385(2) -0.00381(18) -0.00133(19) -0.00793(19) P3 0.0750(4) 0.0471(3) 0.0446(3) 0.0130(2) 0.0077(3) 0.0040(3) C1 0.0621(13) 0.0529(12) 0.0395(10) -0.0086(9) -0.0103(9) 0.0246(10) C2 0.0361(9) 0.0486(11) 0.0527(11) -0.0226(9) -0.0091(8) 0.0104(8) K101 0.02277(15) 0.02310(15) 0.02512(15) 0.00041(11) 0.00505(11) 0.00078(10) N101 0.0352(7) 0.0257(6) 0.0423(8) 0.0060(6) 0.0129(6) 0.0076(5) N102 0.0462(9) 0.0416(8) 0.0446(9) 0.0162(7) 0.0145(7) 0.0194(7) O101 0.0234(5) 0.0420(7) 0.0465(7) 0.0035(5) 0.0007(5) -0.0067(5) O102 0.0513(7) 0.0260(5) 0.0412(7) -0.0065(5) 0.0145(6) -0.0058(5) O103 0.0462(7) 0.0393(6) 0.0354(6) -0.0144(5) 0.0052(5) -0.0053(6) O104 0.0471(8) 0.0760(10) 0.0249(6) 0.0033(6) 0.0038(5) 0.0111(7) O105 0.0370(6) 0.0253(5) 0.0296(5) 0.0027(4) 0.0134(5) 0.0005(4) O106 0.0220(5) 0.0292(5) 0.0399(6) 0.0006(5) 0.0090(4) 0.0013(4) C101 0.0313(8) 0.0477(10) 0.0533(11) 0.0174(9) 0.0054(8) 0.0150(8) C102 0.0214(7) 0.0625(12) 0.0549(11) 0.0126(10) 0.0035(7) 0.0044(8) C103 0.0382(9) 0.0623(12) 0.0324(9) -0.0040(8) 0.0014(7) -0.0251(9) C104 0.0629(12) 0.0431(10) 0.0350(9) -0.0135(8) 0.0153(8) -0.0258(9) C105 0.0693(14) 0.0216(8) 0.0857(17) -0.0032(9) 0.0369(13) -0.0051(9) C106 0.0740(15) 0.0340(10) 0.0781(16) 0.0272(10) 0.0346(13) 0.0177(10) C107 0.0631(13) 0.0283(8) 0.0598(12) 0.0005(8) 0.0299(10) 0.0152(8) C108 0.0818(16) 0.0318(9) 0.0550(12) -0.0194(9) 0.0287(11) -0.0084(10) C109 0.0509(12) 0.0853(17) 0.0444(11) -0.0373(12) -0.0019(9) -0.0073(12) C110 0.0493(12) 0.104(2) 0.0222(8) -0.0107(10) -0.0012(8) 0.0099(12) C111 0.0728(15) 0.0953(19) 0.0318(10) 0.0237(11) 0.0055(10) 0.0280(14) C112 0.0627(14) 0.0849(17) 0.0456(12) 0.0274(12) 0.0020(10) 0.0378(13) C113 0.0490(10) 0.0213(7) 0.0509(10) 0.0074(7) 0.0151(8) 0.0032(7) C114 0.0396(9) 0.0297(8) 0.0367(9) 0.0091(7) 0.0097(7) -0.0016(7) C115 0.0413(9) 0.0292(8) 0.0327(8) -0.0031(6) 0.0187(7) -0.0069(7) C116 0.0273(7) 0.0354(8) 0.0440(9) -0.0082(7) 0.0156(7) -0.0070(6) C117 0.0277(8) 0.0491(10) 0.0496(10) 0.0039(8) 0.0075(7) 0.0145(7) C118 0.0498(11) 0.0397(10) 0.0587(12) 0.0129(9) 0.0200(9) 0.0255(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C2 1.727(2) . ? P1 P2 2.0812(7) . ? P2 P3 2.0936(8) . ? P3 C1 1.781(3) . ? C1 C2 1.393(3) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? K101 O105 2.7545(11) . ? K101 O101 2.7637(12) . ? K101 O106 2.7984(11) . ? K101 O104 2.8410(13) . ? K101 O103 2.8540(12) . ? K101 O102 2.8675(12) . ? K101 N101 3.0162(14) . ? K101 N102 3.0169(15) . ? N101 C101 1.469(3) . ? N101 C107 1.470(2) . ? N101 C113 1.470(2) . ? N102 C106 1.465(3) . ? N102 C112 1.473(3) . ? N102 C118 1.478(2) . ? O101 C103 1.414(2) . ? O101 C102 1.423(2) . ? O102 C105 1.421(2) . ? O102 C104 1.429(2) . ? O103 C108 1.425(3) . ? O103 C109 1.425(3) . ? O104 C110 1.413(3) . ? O104 C111 1.424(3) . ? O105 C114 1.422(2) . ? O105 C115 1.4220(18) . ? O106 C117 1.419(2) . ? O106 C116 1.421(2) . ? C101 C102 1.506(3) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.482(3) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.502(4) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.495(3) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.488(4) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.505(3) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.510(2) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.493(3) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.502(3) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 P2 99.46(8) . . ? P1 P2 P3 99.78(3) . . ? C1 P3 P2 98.98(8) . . ? C2 C1 P3 119.21(15) . . ? C2 C1 H1 120.4 . . ? P3 C1 H1 120.4 . . ? C1 C2 P1 122.56(16) . . ? C1 C2 H2 118.7 . . ? P1 C2 H2 118.7 . . ? O105 K101 O101 93.04(4) . . ? O105 K101 O106 61.18(3) . . ? O101 K101 O106 116.53(4) . . ? O105 K101 O104 123.86(4) . . ? O101 K101 O104 138.67(4) . . ? O106 K101 O104 98.89(4) . . ? O105 K101 O103 100.74(4) . . ? O101 K101 O103 98.46(4) . . ? O106 K101 O103 140.21(4) . . ? O104 K101 O103 60.08(4) . . ? O105 K101 O102 130.68(4) . . ? O101 K101 O102 59.77(4) . . ? O106 K101 O102 93.14(3) . . ? O104 K101 O102 99.84(4) . . ? O103 K101 O102 122.00(4) . . ? O105 K101 N101 60.58(4) . . ? O101 K101 N101 59.40(4) . . ? O106 K101 N101 121.10(4) . . ? O104 K101 N101 119.98(5) . . ? O103 K101 N101 60.64(4) . . ? O102 K101 N101 118.52(4) . . ? O105 K101 N102 121.12(4) . . ? O101 K101 N102 119.22(5) . . ? O106 K101 N102 60.46(4) . . ? O104 K101 N102 60.01(5) . . ? O103 K101 N102 119.00(4) . . ? O102 K101 N102 59.93(5) . . ? N101 K101 N102 178.14(4) . . ? C101 N101 C107 109.88(15) . . ? C101 N101 C113 109.73(15) . . ? C107 N101 C113 110.12(15) . . ? C101 N101 K101 110.93(10) . . ? C107 N101 K101 108.87(11) . . ? C113 N101 K101 107.26(9) . . ? C106 N102 C112 110.27(18) . . ? C106 N102 C118 109.92(17) . . ? C112 N102 C118 109.39(17) . . ? C106 N102 K101 108.80(11) . . ? C112 N102 K101 109.41(13) . . ? C118 N102 K101 109.02(10) . . ? C103 O101 C102 112.29(14) . . ? C103 O101 K101 119.82(11) . . ? C102 O101 K101 120.84(11) . . ? C105 O102 C104 111.11(16) . . ? C105 O102 K101 118.40(12) . . ? C104 O102 K101 106.95(10) . . ? C108 O103 C109 111.43(17) . . ? C108 O103 K101 115.11(10) . . ? C109 O103 K101 112.42(12) . . ? C110 O104 C111 110.85(17) . . ? C110 O104 K101 114.95(12) . . ? C111 O104 K101 118.15(14) . . ? C114 O105 C115 111.19(12) . . ? C114 O105 K101 120.06(9) . . ? C115 O105 K101 115.22(9) . . ? C117 O106 C116 111.66(13) . . ? C117 O106 K101 117.12(10) . . ? C116 O106 K101 112.61(9) . . ? N101 C101 C102 113.51(15) . . ? N101 C101 H10A 108.9 . . ? C102 C101 H10A 108.9 . . ? N101 C101 H10B 108.9 . . ? C102 C101 H10B 108.9 . . ? H10A C101 H10B 107.7 . . ? O101 C102 C101 108.66(14) . . ? O101 C102 H10C 110.0 . . ? C101 C102 H10C 110.0 . . ? O101 C102 H10D 110.0 . . ? C101 C102 H10D 110.0 . . ? H10C C102 H10D 108.3 . . ? O101 C103 C104 109.16(15) . . ? O101 C103 H10E 109.8 . . ? C104 C103 H10E 109.8 . . ? O101 C103 H10F 109.8 . . ? C104 C103 H10F 109.8 . . ? H10E C103 H10F 108.3 . . ? O102 C104 C103 109.57(14) . . ? O102 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O102 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O102 C105 C106 109.81(17) . . ? O102 C105 H10I 109.7 . . ? C106 C105 H10I 109.7 . . ? O102 C105 H10J 109.7 . . ? C106 C105 H10J 109.7 . . ? H10I C105 H10J 108.2 . . ? N102 C106 C105 113.89(17) . . ? N102 C106 H10K 108.8 . . ? C105 C106 H10K 108.8 . . ? N102 C106 H10L 108.8 . . ? C105 C106 H10L 108.8 . . ? H10K C106 H10L 107.7 . . ? N101 C107 C108 114.24(16) . . ? N101 C107 H10M 108.7 . . ? C108 C107 H10M 108.7 . . ? N101 C107 H10N 108.7 . . ? C108 C107 H10N 108.7 . . ? H10M C107 H10N 107.6 . . ? O103 C108 C107 109.69(16) . . ? O103 C108 H10O 109.7 . . ? C107 C108 H10O 109.7 . . ? O103 C108 H10P 109.7 . . ? C107 C108 H10P 109.7 . . ? H10O C108 H10P 108.2 . . ? O103 C109 C110 109.99(18) . . ? O103 C109 H10Q 109.7 . . ? C110 C109 H10Q 109.7 . . ? O103 C109 H10R 109.7 . . ? C110 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O104 C110 C109 109.26(18) . . ? O104 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O104 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.3 . . ? O104 C111 C112 109.03(18) . . ? O104 C111 H11C 109.9 . . ? C112 C111 H11C 109.9 . . ? O104 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? H11C C111 H11D 108.3 . . ? N102 C112 C111 113.70(18) . . ? N102 C112 H11E 108.8 . . ? C111 C112 H11E 108.8 . . ? N102 C112 H11F 108.8 . . ? C111 C112 H11F 108.8 . . ? H11E C112 H11F 107.7 . . ? N101 C113 C114 113.13(14) . . ? N101 C113 H11G 109.0 . . ? C114 C113 H11G 109.0 . . ? N101 C113 H11H 109.0 . . ? C114 C113 H11H 109.0 . . ? H11G C113 H11H 107.8 . . ? O105 C114 C113 108.35(14) . . ? O105 C114 H11I 110.0 . . ? C113 C114 H11I 110.0 . . ? O105 C114 H11J 110.0 . . ? C113 C114 H11J 110.0 . . ? H11I C114 H11J 108.4 . . ? O105 C115 C116 108.59(13) . . ? O105 C115 H11K 110.0 . . ? C116 C115 H11K 110.0 . . ? O105 C115 H11L 110.0 . . ? C116 C115 H11L 110.0 . . ? H11K C115 H11L 108.4 . . ? O106 C116 C115 109.37(13) . . ? O106 C116 H11M 109.8 . . ? C115 C116 H11M 109.8 . . ? O106 C116 H11N 109.8 . . ? C115 C116 H11N 109.8 . . ? H11M C116 H11N 108.2 . . ? O106 C117 C118 109.50(15) . . ? O106 C117 H11O 109.8 . . ? C118 C117 H11O 109.8 . . ? O106 C117 H11P 109.8 . . ? C118 C117 H11P 109.8 . . ? H11O C117 H11P 108.2 . . ? N102 C118 C117 112.90(17) . . ? N102 C118 H11Q 109.0 . . ? C117 C118 H11Q 109.0 . . ? N102 C118 H11R 109.0 . . ? C117 C118 H11R 109.0 . . ? H11Q C118 H11R 107.8 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 76.43 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.630 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.047 _iucr_refine_instructions_details ; TITL 1a CELL 1.54184 9.9714 10.8313 25.5105 90.000 97.071 90.000 ZERR 4.00 0.0003 0.0002 0.0007 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P K UNIT 80 152 8 24 12 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.200 0.280 0.300 TEMP -123 ACTA BOND $H L.S. 4 WGHT 0.047200 0.986800 FVAR 0.12040 P1 5 0.363945 0.944709 0.176866 11.00000 0.03494 0.03422 = 0.05130 -0.00774 0.00697 -0.00011 P2 5 0.512338 1.080053 0.177652 11.00000 0.04147 0.03928 = 0.03851 -0.00381 -0.00133 -0.00793 P3 5 0.506444 1.110980 0.096389 11.00000 0.07503 0.04707 = 0.04457 0.01299 0.00767 0.00396 C1 1 0.377403 1.003628 0.073153 11.00000 0.06210 0.05291 = 0.03950 -0.00860 -0.01026 0.02457 AFIX 43 H1 2 0.349197 0.995121 0.036384 11.00000 -1.20000 AFIX 0 C2 1 0.318318 0.932284 0.109531 11.00000 0.03611 0.04858 = 0.05266 -0.02258 -0.00906 0.01037 AFIX 43 H2 2 0.250278 0.874544 0.096812 11.00000 -1.20000 AFIX 0 K101 6 0.864819 0.473431 0.116481 11.00000 0.02277 0.02310 = 0.02512 0.00041 0.00505 0.00078 N101 3 1.013025 0.238486 0.150503 11.00000 0.03520 0.02572 = 0.04233 0.00605 0.01290 0.00761 N102 3 0.725055 0.711864 0.081511 11.00000 0.04618 0.04158 = 0.04464 0.01620 0.01451 0.01938 O101 4 1.118262 0.481754 0.174058 11.00000 0.02344 0.04197 = 0.04646 0.00347 0.00071 -0.00670 O102 4 1.007295 0.703235 0.131121 11.00000 0.05128 0.02602 = 0.04120 -0.00651 0.01453 -0.00584 O103 4 0.921134 0.298633 0.038376 11.00000 0.04620 0.03928 = 0.03539 -0.01444 0.00523 -0.00531 O104 4 0.745846 0.502264 0.010145 11.00000 0.04709 0.07603 = 0.02486 0.00333 0.00376 0.01106 O105 4 0.763206 0.320621 0.188375 11.00000 0.03699 0.02528 = 0.02963 0.00269 0.01338 0.00053 O106 4 0.649219 0.557127 0.167559 11.00000 0.02199 0.02924 = 0.03992 0.00062 0.00901 0.00133 C101 1 1.133718 0.264682 0.187959 11.00000 0.03128 0.04773 = 0.05335 0.01744 0.00535 0.01499 AFIX 23 H10A 2 1.196024 0.193370 0.188682 11.00000 -1.20000 H10B 2 1.106422 0.273844 0.223778 11.00000 -1.20000 AFIX 0 C102 1 1.207920 0.379398 0.174685 11.00000 0.02135 0.06255 = 0.05485 0.01257 0.00349 0.00445 AFIX 23 H10C 2 1.287413 0.392906 0.201364 11.00000 -1.20000 H10D 2 1.240012 0.370116 0.139685 11.00000 -1.20000 AFIX 0 C103 1 1.187813 0.595439 0.180973 11.00000 0.03822 0.06234 = 0.03236 -0.00403 0.00138 -0.02513 AFIX 23 H10E 2 1.243533 0.608143 0.151877 11.00000 -1.20000 H10F 2 1.248556 0.594675 0.214730 11.00000 -1.20000 AFIX 0 C104 1 1.088258 0.696947 0.181321 11.00000 0.06290 0.04312 = 0.03503 -0.01348 0.01534 -0.02579 AFIX 23 H10G 2 1.029853 0.682117 0.209383 11.00000 -1.20000 H10H 2 1.136083 0.776279 0.188851 11.00000 -1.20000 AFIX 0 C105 1 0.931558 0.814597 0.125861 11.00000 0.06935 0.02160 = 0.08571 -0.00323 0.03693 -0.00510 AFIX 23 H10I 2 0.992864 0.885168 0.122277 11.00000 -1.20000 H10J 2 0.886337 0.827969 0.157834 11.00000 -1.20000 AFIX 0 C106 1 0.827586 0.807483 0.078090 11.00000 0.07403 0.03400 = 0.07810 0.02715 0.03461 0.01770 AFIX 23 H10K 2 0.781957 0.888531 0.072962 11.00000 -1.20000 H10L 2 0.873993 0.791254 0.046641 11.00000 -1.20000 AFIX 0 C107 1 1.052242 0.176096 0.103541 11.00000 0.06309 0.02828 = 0.05977 0.00054 0.02985 0.01520 AFIX 23 H10M 2 1.076793 0.089621 0.112926 11.00000 -1.20000 H10N 2 1.133709 0.217128 0.093183 11.00000 -1.20000 AFIX 0 C108 1 0.944956 0.175726 0.057133 11.00000 0.08181 0.03177 = 0.05503 -0.01940 0.02866 -0.00844 AFIX 23 H10O 2 0.973899 0.123659 0.028671 11.00000 -1.20000 H10P 2 0.860510 0.140567 0.067566 11.00000 -1.20000 AFIX 0 C109 1 0.823266 0.301682 -0.007272 11.00000 0.05093 0.08525 = 0.04444 -0.03731 -0.00192 -0.00728 AFIX 23 H10Q 2 0.736009 0.269408 0.001669 11.00000 -1.20000 H10R 2 0.853273 0.248456 -0.035151 11.00000 -1.20000 AFIX 0 C110 1 0.805191 0.430576 -0.027117 11.00000 0.04927 0.10409 = 0.02224 -0.01072 -0.00120 0.00993 AFIX 23 H11A 2 0.893878 0.465978 -0.032679 11.00000 -1.20000 H11B 2 0.746439 0.431096 -0.061354 11.00000 -1.20000 AFIX 0 C111 1 0.718379 0.624203 -0.009145 11.00000 0.07275 0.09526 = 0.03177 0.02374 0.00553 0.02801 AFIX 23 H11C 2 0.662276 0.620927 -0.043945 11.00000 -1.20000 H11D 2 0.804076 0.666804 -0.013614 11.00000 -1.20000 AFIX 0 C112 1 0.644758 0.693809 0.029645 11.00000 0.06272 0.08488 = 0.04556 0.02737 0.00203 0.03782 AFIX 23 H11E 2 0.617855 0.775594 0.014518 11.00000 -1.20000 H11F 2 0.561181 0.648328 0.034684 11.00000 -1.20000 AFIX 0 C113 1 0.919271 0.160448 0.176017 11.00000 0.04903 0.02126 = 0.05094 0.00741 0.01514 0.00319 AFIX 23 H11G 2 0.970271 0.090877 0.194032 11.00000 -1.20000 H11H 2 0.851198 0.125365 0.148516 11.00000 -1.20000 AFIX 0 C114 1 0.847338 0.229484 0.215738 11.00000 0.03965 0.02971 = 0.03673 0.00915 0.00974 -0.00156 AFIX 23 H11I 2 0.792027 0.171622 0.234104 11.00000 -1.20000 H11J 2 0.914059 0.269164 0.242451 11.00000 -1.20000 AFIX 0 C115 1 0.680816 0.379671 0.222586 11.00000 0.04132 0.02915 = 0.03265 -0.00307 0.01871 -0.00690 AFIX 23 H11K 2 0.737505 0.430524 0.248899 11.00000 -1.20000 H11L 2 0.633355 0.316993 0.241724 11.00000 -1.20000 AFIX 0 C116 1 0.580448 0.459442 0.190160 11.00000 0.02728 0.03544 = 0.04398 -0.00819 0.01564 -0.00701 AFIX 23 H11M 2 0.529464 0.409740 0.161831 11.00000 -1.20000 H11N 2 0.515387 0.493785 0.212652 11.00000 -1.20000 AFIX 0 C117 1 0.557606 0.641032 0.139452 11.00000 0.02773 0.04911 = 0.04961 0.00395 0.00751 0.01455 AFIX 23 H11O 2 0.492178 0.671102 0.162741 11.00000 -1.20000 H11P 2 0.506601 0.598731 0.108855 11.00000 -1.20000 AFIX 0 C118 1 0.634559 0.748113 0.120618 11.00000 0.04984 0.03970 = 0.05871 0.01289 0.02004 0.02548 AFIX 23 H11Q 2 0.569550 0.810582 0.104582 11.00000 -1.20000 H11R 2 0.689036 0.786790 0.151343 11.00000 -1.20000 HKLF 4 REM p21n REM R1 = 0.0342 for 5088 Fo > 4sig(Fo) and 0.0390 for all 5677 data REM 289 parameters refined using 0 restraints END WGHT 0.0465 1.0117 REM Highest difference peak 0.630, deepest hole -0.645, 1-sigma level 0.047 Q1 1 0.3403 0.9523 0.1440 11.00000 0.05 0.63 Q2 1 0.3540 1.0033 0.0572 11.00000 0.05 0.30 Q3 1 0.4391 1.0236 0.0748 11.00000 0.05 0.28 Q4 1 0.5911 1.1110 0.1006 11.00000 0.05 0.26 Q5 1 0.4460 1.0203 0.1759 11.00000 0.05 0.25 Q6 1 0.3671 0.9657 0.0830 11.00000 0.05 0.24 Q7 1 0.4032 0.8992 0.2241 11.00000 0.05 0.18 Q8 1 0.8501 0.4844 0.0586 11.00000 0.05 0.18 Q9 1 0.6700 0.7205 0.0910 11.00000 0.05 0.18 Q10 1 0.8832 0.4805 0.1723 11.00000 0.05 0.17 Q11 1 0.8368 0.4351 0.1675 11.00000 0.05 0.17 Q12 1 0.5889 0.3891 0.0748 11.00000 0.05 0.17 Q13 1 1.1320 0.6475 0.1749 11.00000 0.05 0.16 Q14 1 0.7810 0.4725 0.1090 11.00000 0.05 0.16 Q15 1 0.6580 0.6514 0.0084 11.00000 0.05 0.16 Q16 1 0.5157 1.0732 0.2335 11.00000 0.05 0.16 Q17 1 0.5438 0.4794 0.2393 11.00000 0.05 0.16 Q18 1 0.5805 0.3263 0.2271 11.00000 0.05 0.16 Q19 1 0.8623 0.8040 0.1172 11.00000 0.05 0.15 Q20 1 0.7977 0.5663 0.1389 11.00000 0.05 0.15 ; data_1b _database_code_depnum_ccdc_archive 'CCDC 873510' #TrackingRef '10374_web_deposit_cif_file_1_JoseGoicoechea_1332849746.1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(18-crown-6)][P3C2H2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C12 H24 K O6, C2 H2 P3' _chemical_formula_sum 'C14 H26 K O6 P3' _chemical_formula_weight 422.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.08640(10) _cell_length_b 15.5733(2) _cell_length_c 14.6129(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.3280(10) _cell_angle_gamma 90.00 _cell_volume 2040.46(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6998 _cell_measurement_theta_min 3.0621 _cell_measurement_theta_max 76.0842 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 4.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2960 _exptl_absorpt_correction_T_max 0.3963 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.5035 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 10326 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 76.28 _reflns_number_total 4387 _reflns_number_gt 4155 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.4170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4387 _refine_ls_number_parameters 248 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.326 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K101 K 0.81432(7) 0.2500 0.59372(4) 0.02299(17) Uani 1 2 d S . . O11 O 0.5449(2) 0.2500 0.66684(15) 0.0267(5) Uani 1 2 d S . . O12 O 0.70371(17) 0.09444(10) 0.66396(11) 0.0261(3) Uani 1 1 d . . . O13 O 0.96354(17) 0.09158(10) 0.57927(11) 0.0259(3) Uani 1 1 d . . . O14 O 1.1181(2) 0.2500 0.58012(15) 0.0260(5) Uani 1 2 d S . . C101 C 0.5077(2) 0.17425(16) 0.71235(16) 0.0295(5) Uani 1 1 d . . . H10A H 0.3999 0.1740 0.7162 0.035 Uiso 1 1 calc R . . H10B H 0.5644 0.1720 0.7761 0.035 Uiso 1 1 calc R . . C102 C 0.5459(2) 0.09807(15) 0.65777(16) 0.0290(5) Uani 1 1 d . . . H10C H 0.5089 0.0447 0.6831 0.035 Uiso 1 1 calc R . . H10D H 0.4983 0.1037 0.5921 0.035 Uiso 1 1 calc R . . C103 C 0.7503(3) 0.02115(14) 0.61803(16) 0.0287(5) Uani 1 1 d . . . H10E H 0.7081 0.0231 0.5512 0.034 Uiso 1 1 calc R . . H10F H 0.7149 -0.0319 0.6448 0.034 Uiso 1 1 calc R . . C104 C 0.9179(3) 0.02161(14) 0.63058(16) 0.0282(5) Uani 1 1 d . . . H10G H 0.9599 0.0279 0.6971 0.034 Uiso 1 1 calc R . . H10H H 0.9543 -0.0331 0.6081 0.034 Uiso 1 1 calc R . . C105 C 1.1216(2) 0.09827(15) 0.59144(16) 0.0285(5) Uani 1 1 d . . . H10I H 1.1646 0.0453 0.5692 0.034 Uiso 1 1 calc R . . H10J H 1.1625 0.1058 0.6580 0.034 Uiso 1 1 calc R . . C106 C 1.1614(2) 0.17427(15) 0.53710(16) 0.0283(5) Uani 1 1 d . . . H10K H 1.2701 0.1751 0.5363 0.034 Uiso 1 1 calc R . . H10L H 1.1089 0.1708 0.4723 0.034 Uiso 1 1 calc R . . K201 K 0.48181(7) 0.2500 0.14632(5) 0.02689(17) Uani 1 2 d S . . O21 O 0.1841(2) 0.2500 0.17258(15) 0.0282(5) Uani 1 2 d S . . O22 O 0.33741(17) 0.09151(10) 0.17189(11) 0.0267(3) Uani 1 1 d . . . O23 O 0.59639(17) 0.09327(10) 0.08360(11) 0.0269(3) Uani 1 1 d . . . O24 O 0.7566(2) 0.2500 0.08390(15) 0.0249(4) Uani 1 2 d S . . C201 C 0.1393(2) 0.17414(16) 0.21455(16) 0.0294(5) Uani 1 1 d . . . H20A H 0.0305 0.1752 0.2148 0.035 Uiso 1 1 calc R . . H20B H 0.1910 0.1700 0.2795 0.035 Uiso 1 1 calc R . . C202 C 0.1793(2) 0.09863(16) 0.15952(16) 0.0296(5) Uani 1 1 d . . . H20C H 0.1358 0.0455 0.1810 0.036 Uiso 1 1 calc R . . H20D H 0.1388 0.1068 0.0930 0.036 Uiso 1 1 calc R . . C203 C 0.3825(3) 0.02218(15) 0.11943(16) 0.0298(5) Uani 1 1 d . . . H20E H 0.3395 0.0293 0.0532 0.036 Uiso 1 1 calc R . . H20F H 0.3456 -0.0327 0.1413 0.036 Uiso 1 1 calc R . . C204 C 0.5495(3) 0.02054(14) 0.13056(16) 0.0300(5) Uani 1 1 d . . . H20G H 0.5932 0.0227 0.1971 0.036 Uiso 1 1 calc R . . H20H H 0.5831 -0.0330 0.1038 0.036 Uiso 1 1 calc R . . C205 C 0.7546(2) 0.09831(14) 0.09217(16) 0.0279(5) Uani 1 1 d . . . H20I H 0.7943 0.0452 0.0681 0.033 Uiso 1 1 calc R . . H20J H 0.7996 0.1048 0.1582 0.033 Uiso 1 1 calc R . . C206 C 0.7925(2) 0.17433(15) 0.03763(15) 0.0277(5) Uani 1 1 d . . . H20K H 0.9000 0.1738 0.0331 0.033 Uiso 1 1 calc R . . H20L H 0.7348 0.1724 -0.0259 0.033 Uiso 1 1 calc R . . P1 P 0.26252(11) 0.2500 0.91483(7) 0.0549(3) Uani 1 2 d SD . . P2 P 0.11958(10) 0.14795(5) 0.87147(5) 0.0449(2) Uani 1 1 d D . . C1 C -0.0369(3) 0.20732(19) 0.82401(16) 0.0376(5) Uani 1 1 d D . . H1 H -0.1249 0.1778 0.7973 0.045 Uiso 1 1 calc R . . P11 P 0.8069(4) 0.2500 0.3503(3) 0.156(5) Uani 0.471(5) 2 d SPD . 1 P12 P 0.6966(6) 0.1565(2) 0.3625(2) 0.0995(19) Uani 0.471(5) 1 d PD . 1 C11 C 0.5250(7) 0.1991(4) 0.4000(4) 0.0204(7) Uani 0.471(5) 1 d PD . 1 H11 H 0.4476 0.1646 0.4169 0.024 Uiso 0.471(5) 1 calc PR . 1 P11A P 0.4933(3) 0.2500 0.39768(18) 0.120(3) Uani 0.529(5) 2 d SPD . 2 P12A P 0.5832(6) 0.1628(3) 0.39202(19) 0.128(3) Uani 0.529(5) 1 d PD . 2 C11A C 0.7708(5) 0.1949(3) 0.3527(3) 0.0204(7) Uani 0.529(5) 1 d PD . 2 H11A H 0.8457 0.1577 0.3370 0.024 Uiso 0.529(5) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K101 0.0217(3) 0.0188(3) 0.0300(3) 0.000 0.0087(2) 0.000 O11 0.0271(11) 0.0289(11) 0.0260(10) 0.000 0.0099(8) 0.000 O12 0.0244(7) 0.0224(7) 0.0308(8) -0.0022(6) 0.0025(6) -0.0059(6) O13 0.0257(7) 0.0225(7) 0.0289(8) 0.0030(6) 0.0024(6) 0.0040(6) O14 0.0252(10) 0.0283(11) 0.0266(10) 0.000 0.0106(8) 0.000 C101 0.0250(10) 0.0372(13) 0.0276(11) 0.0023(9) 0.0085(8) -0.0075(9) C102 0.0245(10) 0.0313(12) 0.0311(11) 0.0016(9) 0.0042(8) -0.0097(9) C103 0.0345(12) 0.0173(10) 0.0325(11) -0.0021(8) -0.0001(9) -0.0042(8) C104 0.0349(12) 0.0166(10) 0.0316(11) 0.0011(8) 0.0009(9) 0.0017(8) C105 0.0244(10) 0.0309(12) 0.0308(11) 0.0012(9) 0.0059(8) 0.0092(9) C106 0.0253(10) 0.0338(12) 0.0278(10) -0.0005(9) 0.0098(8) 0.0068(9) K201 0.0244(3) 0.0225(3) 0.0359(4) 0.000 0.0114(3) 0.000 O21 0.0278(11) 0.0325(12) 0.0265(11) 0.000 0.0107(9) 0.000 O22 0.0250(7) 0.0278(8) 0.0263(7) -0.0036(6) 0.0018(6) -0.0042(6) O23 0.0254(7) 0.0233(7) 0.0316(8) 0.0026(6) 0.0033(6) 0.0018(6) O24 0.0278(11) 0.0227(10) 0.0258(10) 0.000 0.0092(8) 0.000 C201 0.0238(10) 0.0388(13) 0.0270(10) 0.0018(9) 0.0081(8) -0.0057(9) C202 0.0245(10) 0.0359(12) 0.0280(11) 0.0004(9) 0.0031(8) -0.0091(9) C203 0.0368(12) 0.0222(11) 0.0299(11) -0.0023(8) 0.0046(9) -0.0045(9) C204 0.0361(12) 0.0209(10) 0.0331(11) 0.0026(9) 0.0060(9) 0.0027(9) C205 0.0243(10) 0.0248(11) 0.0332(11) -0.0037(9) 0.0009(8) 0.0047(8) C206 0.0254(10) 0.0313(12) 0.0273(10) -0.0053(9) 0.0069(8) 0.0038(9) P1 0.0290(5) 0.1000(10) 0.0339(5) 0.000 -0.0009(4) 0.000 P2 0.0647(5) 0.0336(4) 0.0370(4) 0.0045(3) 0.0098(3) 0.0174(3) C1 0.0331(12) 0.0532(15) 0.0252(11) -0.0028(10) 0.0013(9) -0.0015(11) P11 0.0288(17) 0.398(15) 0.0414(17) 0.000 0.0116(13) 0.000 P12 0.182(5) 0.0514(17) 0.0467(14) -0.0157(12) -0.037(2) 0.058(2) C11 0.0090(16) 0.035(2) 0.0186(17) -0.0011(14) 0.0056(11) -0.0001(13) P11A 0.0168(12) 0.320(10) 0.0250(11) 0.000 0.0050(8) 0.000 P12A 0.217(5) 0.088(2) 0.0494(16) 0.0359(17) -0.064(2) -0.116(3) C11A 0.0090(16) 0.035(2) 0.0186(17) -0.0011(14) 0.0056(11) -0.0001(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K101 O14 2.799(2) . ? K101 O11 2.825(2) . ? K101 O13 2.8396(15) 4_565 ? K101 O13 2.8396(15) . ? K101 O12 2.8752(15) 4_565 ? K101 O12 2.8752(15) . ? K101 C1 3.481(2) 4_665 ? K101 C1 3.481(2) 1_655 ? K101 P11 3.546(4) . ? K101 P12A 3.596(2) . ? K101 P12A 3.596(2) 4_565 ? K101 P12 3.675(2) . ? O11 C101 1.422(3) 4_565 ? O11 C101 1.422(3) . ? O12 C103 1.423(3) . ? O12 C102 1.424(3) . ? O13 C104 1.422(3) . ? O13 C105 1.422(3) . ? O14 C106 1.422(2) . ? O14 C106 1.422(2) 4_565 ? C101 C102 1.501(3) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.504(3) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.502(3) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? K201 O21 2.793(2) . ? K201 O24 2.794(2) . ? K201 O22 2.8481(16) . ? K201 O22 2.8481(16) 4_565 ? K201 O23 2.8619(16) . ? K201 O23 2.8619(16) 4_565 ? K201 P1 3.6370(12) 1_554 ? K201 P11A 3.658(3) . ? K201 P12 3.730(2) 4_565 ? K201 P12 3.730(2) . ? K201 P12A 3.809(2) 4_565 ? K201 P12A 3.809(2) . ? O21 C201 1.421(3) 4_565 ? O21 C201 1.421(3) . ? O22 C203 1.422(3) . ? O22 C202 1.423(3) . ? O23 C205 1.425(3) . ? O23 C204 1.425(3) . ? O24 C206 1.422(2) . ? O24 C206 1.422(2) 4_565 ? C201 C202 1.502(3) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.500(3) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.498(3) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? P1 P2 2.0851(11) . ? P1 P2 2.0851(11) 4_565 ? P1 K201 3.6370(12) 1_556 ? P2 C1 1.743(3) . ? C1 C1 1.329(6) 4_565 ? C1 K101 3.481(2) 1_455 ? C1 H1 0.9500 . ? P11 P12 1.792(6) . ? P11 P12 1.792(6) 4_565 ? P12 C11 1.856(6) . ? C11 C11 1.584(11) 4_565 ? C11 H11 0.9500 . ? P11A P12A 1.594(6) 4_565 ? P11A P12A 1.594(6) . ? P12A C11A 1.950(6) . ? C11A C11A 1.715(10) 4_565 ? C11A H11A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 K101 O11 162.10(7) . . ? O14 K101 O13 60.43(3) . 4_565 ? O11 K101 O13 118.79(3) . 4_565 ? O14 K101 O13 60.43(3) . . ? O11 K101 O13 118.79(3) . . ? O13 K101 O13 120.65(7) 4_565 . ? O14 K101 O12 115.54(4) . 4_565 ? O11 K101 O12 59.37(3) . 4_565 ? O13 K101 O12 59.55(5) 4_565 4_565 ? O13 K101 O12 163.21(5) . 4_565 ? O14 K101 O12 115.54(4) . . ? O11 K101 O12 59.37(3) . . ? O13 K101 O12 163.21(5) 4_565 . ? O13 K101 O12 59.55(5) . . ? O12 K101 O12 114.83(7) 4_565 . ? O14 K101 C1 80.54(6) . 4_665 ? O11 K101 C1 81.89(6) . 4_665 ? O13 K101 C1 77.91(6) 4_565 4_665 ? O13 K101 C1 97.03(6) . 4_665 ? O12 K101 C1 66.27(6) 4_565 4_665 ? O12 K101 C1 85.37(6) . 4_665 ? O14 K101 C1 80.54(6) . 1_655 ? O11 K101 C1 81.89(6) . 1_655 ? O13 K101 C1 97.03(6) 4_565 1_655 ? O13 K101 C1 77.91(6) . 1_655 ? O12 K101 C1 85.37(6) 4_565 1_655 ? O12 K101 C1 66.27(6) . 1_655 ? C1 K101 C1 22.01(10) 4_665 1_655 ? O14 K101 P11 77.74(8) . . ? O11 K101 P11 120.17(8) . . ? O13 K101 P11 81.79(4) 4_565 . ? O13 K101 P11 81.79(4) . . ? O12 K101 P11 114.02(4) 4_565 . ? O12 K101 P11 114.02(4) . . ? C1 K101 P11 155.61(7) 4_665 . ? C1 K101 P11 155.61(7) 1_655 . ? O14 K101 P12A 113.16(12) . . ? O11 K101 P12A 83.31(11) . . ? O13 K101 P12A 119.31(5) 4_565 . ? O13 K101 P12A 80.41(10) . . ? O12 K101 P12A 114.79(11) 4_565 . ? O12 K101 P12A 77.47(5) . . ? C1 K101 P12A 161.44(7) 4_665 . ? C1 K101 P12A 143.50(6) 1_655 . ? P11 K101 P12A 42.64(7) . . ? O14 K101 P12A 113.16(12) . 4_565 ? O11 K101 P12A 83.31(11) . 4_565 ? O13 K101 P12A 80.41(10) 4_565 4_565 ? O13 K101 P12A 119.31(5) . 4_565 ? O12 K101 P12A 77.47(5) 4_565 4_565 ? O12 K101 P12A 114.79(11) . 4_565 ? C1 K101 P12A 143.50(6) 4_665 4_565 ? C1 K101 P12A 161.44(7) 1_655 4_565 ? P11 K101 P12A 42.64(7) . 4_565 ? P12A K101 P12A 44.37(13) . 4_565 ? O14 K101 P12 94.48(10) . . ? O11 K101 P12 101.94(11) . . ? O13 K101 P12 110.31(10) 4_565 . ? O13 K101 P12 70.05(5) . . ? O12 K101 P12 126.54(5) 4_565 . ? O12 K101 P12 85.87(9) . . ? C1 K101 P12 166.87(6) 4_665 . ? C1 K101 P12 145.34(7) 1_655 . ? P11 K101 P12 28.67(9) . . ? P12A K101 P12 18.69(10) . . ? P12A K101 P12 49.60(5) 4_565 . ? C101 O11 C101 112.1(2) 4_565 . ? C101 O11 K101 117.61(13) 4_565 . ? C101 O11 K101 117.61(13) . . ? C103 O12 C102 112.06(17) . . ? C103 O12 K101 111.07(12) . . ? C102 O12 K101 110.54(13) . . ? C104 O13 C105 111.43(17) . . ? C104 O13 K101 116.28(12) . . ? C105 O13 K101 114.31(13) . . ? C106 O14 C106 112.1(2) . 4_565 ? C106 O14 K101 112.23(13) . . ? C106 O14 K101 112.23(13) 4_565 . ? O11 C101 C102 108.32(18) . . ? O11 C101 H10A 110.0 . . ? C102 C101 H10A 110.0 . . ? O11 C101 H10B 110.0 . . ? C102 C101 H10B 110.0 . . ? H10A C101 H10B 108.4 . . ? O12 C102 C101 108.34(18) . . ? O12 C102 H10C 110.0 . . ? C101 C102 H10C 110.0 . . ? O12 C102 H10D 110.0 . . ? C101 C102 H10D 110.0 . . ? H10C C102 H10D 108.4 . . ? O12 C103 C104 108.15(17) . . ? O12 C103 H10E 110.1 . . ? C104 C103 H10E 110.1 . . ? O12 C103 H10F 110.1 . . ? C104 C103 H10F 110.1 . . ? H10E C103 H10F 108.4 . . ? O13 C104 C103 108.40(17) . . ? O13 C104 H10G 110.0 . . ? C103 C104 H10G 110.0 . . ? O13 C104 H10H 110.0 . . ? C103 C104 H10H 110.0 . . ? H10G C104 H10H 108.4 . . ? O13 C105 C106 108.44(18) . . ? O13 C105 H10I 110.0 . . ? C106 C105 H10I 110.0 . . ? O13 C105 H10J 110.0 . . ? C106 C105 H10J 110.0 . . ? H10I C105 H10J 108.4 . . ? O14 C106 C105 108.20(17) . . ? O14 C106 H10K 110.1 . . ? C105 C106 H10K 110.1 . . ? O14 C106 H10L 110.1 . . ? C105 C106 H10L 110.1 . . ? H10K C106 H10L 108.4 . . ? O21 K201 O24 169.00(7) . . ? O21 K201 O22 60.33(3) . . ? O24 K201 O22 119.86(3) . . ? O21 K201 O22 60.33(3) . 4_565 ? O24 K201 O22 119.86(3) . 4_565 ? O22 K201 O22 120.13(7) . 4_565 ? O21 K201 O23 117.05(4) . . ? O24 K201 O23 60.31(3) . . ? O22 K201 O23 60.14(4) . . ? O22 K201 O23 168.61(5) 4_565 . ? O21 K201 O23 117.05(4) . 4_565 ? O24 K201 O23 60.31(3) . 4_565 ? O22 K201 O23 168.61(5) . 4_565 ? O22 K201 O23 60.14(4) 4_565 4_565 ? O23 K201 O23 117.04(7) . 4_565 ? O21 K201 P1 74.39(5) . 1_554 ? O24 K201 P1 94.60(5) . 1_554 ? O22 K201 P1 85.84(3) . 1_554 ? O22 K201 P1 85.84(3) 4_565 1_554 ? O23 K201 P1 82.82(4) . 1_554 ? O23 K201 P1 82.82(4) 4_565 1_554 ? O21 K201 P11A 74.49(6) . . ? O24 K201 P11A 116.51(6) . . ? O22 K201 P11A 78.87(4) . . ? O22 K201 P11A 78.87(4) 4_565 . ? O23 K201 P11A 111.65(4) . . ? O23 K201 P11A 111.65(4) 4_565 . ? P1 K201 P11A 148.89(5) 1_554 . ? O21 K201 P12 105.61(11) . 4_565 ? O24 K201 P12 84.49(11) . 4_565 ? O22 K201 P12 114.58(5) . 4_565 ? O22 K201 P12 74.91(9) 4_565 4_565 ? O23 K201 P12 115.88(10) . 4_565 ? O23 K201 P12 76.75(5) 4_565 4_565 ? P1 K201 P12 156.99(5) 1_554 4_565 ? P11A K201 P12 39.06(6) . 4_565 ? O21 K201 P12 105.61(11) . . ? O24 K201 P12 84.49(11) . . ? O22 K201 P12 74.91(9) . . ? O22 K201 P12 114.58(5) 4_565 . ? O23 K201 P12 76.75(5) . . ? O23 K201 P12 115.88(10) 4_565 . ? P1 K201 P12 156.99(5) 1_554 . ? P11A K201 P12 39.06(6) . . ? P12 K201 P12 45.94(11) 4_565 . ? O21 K201 P12A 87.84(10) . 4_565 ? O24 K201 P12A 102.43(11) . 4_565 ? O22 K201 P12A 103.38(10) . 4_565 ? O22 K201 P12A 67.27(4) 4_565 4_565 ? O23 K201 P12A 124.11(5) . 4_565 ? O23 K201 P12A 87.30(10) 4_565 4_565 ? P1 K201 P12A 152.75(4) 1_554 4_565 ? P11A K201 P12A 24.54(9) . 4_565 ? P12 K201 P12A 18.02(9) 4_565 4_565 ? P12 K201 P12A 47.72(5) . 4_565 ? O21 K201 P12A 87.84(10) . . ? O24 K201 P12A 102.43(11) . . ? O22 K201 P12A 67.27(4) . . ? O22 K201 P12A 103.38(10) 4_565 . ? O23 K201 P12A 87.30(10) . . ? O23 K201 P12A 124.11(5) 4_565 . ? P1 K201 P12A 152.75(4) 1_554 . ? P11A K201 P12A 24.54(9) . . ? P12 K201 P12A 47.72(5) 4_565 . ? P12 K201 P12A 18.02(9) . . ? P12A K201 P12A 41.76(12) 4_565 . ? C201 O21 C201 112.5(2) 4_565 . ? C201 O21 K201 114.24(13) 4_565 . ? C201 O21 K201 114.24(13) . . ? C203 O22 C202 111.32(17) . . ? C203 O22 K201 114.10(12) . . ? C202 O22 K201 113.14(13) . . ? C205 O23 C204 112.19(17) . . ? C205 O23 K201 109.82(12) . . ? C204 O23 K201 111.77(12) . . ? C206 O24 C206 111.9(2) . 4_565 ? C206 O24 K201 116.16(12) . . ? C206 O24 K201 116.16(12) 4_565 . ? O21 C201 C202 108.01(17) . . ? O21 C201 H20A 110.1 . . ? C202 C201 H20A 110.1 . . ? O21 C201 H20B 110.1 . . ? C202 C201 H20B 110.1 . . ? H20A C201 H20B 108.4 . . ? O22 C202 C201 108.63(18) . . ? O22 C202 H20C 110.0 . . ? C201 C202 H20C 110.0 . . ? O22 C202 H20D 110.0 . . ? C201 C202 H20D 110.0 . . ? H20C C202 H20D 108.3 . . ? O22 C203 C204 109.20(18) . . ? O22 C203 H20E 109.8 . . ? C204 C203 H20E 109.8 . . ? O22 C203 H20F 109.8 . . ? C204 C203 H20F 109.8 . . ? H20E C203 H20F 108.3 . . ? O23 C204 C203 108.10(18) . . ? O23 C204 H20G 110.1 . . ? C203 C204 H20G 110.1 . . ? O23 C204 H20H 110.1 . . ? C203 C204 H20H 110.1 . . ? H20G C204 H20H 108.4 . . ? O23 C205 C206 108.19(17) . . ? O23 C205 H20I 110.1 . . ? C206 C205 H20I 110.1 . . ? O23 C205 H20J 110.1 . . ? C206 C205 H20J 110.1 . . ? H20I C205 H20J 108.4 . . ? O24 C206 C205 108.17(17) . . ? O24 C206 H20K 110.1 . . ? C205 C206 H20K 110.1 . . ? O24 C206 H20L 110.1 . . ? C205 C206 H20L 110.1 . . ? H20K C206 H20L 108.4 . . ? P2 P1 P2 99.32(6) . 4_565 ? P2 P1 K201 120.20(3) . 1_556 ? P2 P1 K201 120.20(3) 4_565 1_556 ? C1 P2 P1 98.29(10) . . ? C1 C1 P2 122.04(10) 4_565 . ? C1 C1 K101 78.99(5) 4_565 1_455 ? P2 C1 K101 130.54(11) . 1_455 ? C1 C1 H1 119.0 4_565 . ? P2 C1 H1 119.0 . . ? K101 C1 H1 61.7 1_455 . ? P12 P11 P12 108.6(3) . 4_565 ? P12 P11 K101 79.65(15) . . ? P12 P11 K101 79.65(15) 4_565 . ? P12 P11 K201 72.86(15) . . ? P12 P11 K201 72.86(15) 4_565 . ? K101 P11 K201 131.73(10) . . ? P11 P12 C11 104.4(2) . . ? P11 P12 K101 71.68(15) . . ? C11 P12 K101 73.8(2) . . ? P11 P12 K201 79.80(16) . . ? C11 P12 K201 76.2(2) . . ? K101 P12 K201 131.19(6) . . ? C11 C11 P12 110.9(2) 4_565 . ? C11 C11 H11 124.5 4_565 . ? P12 C11 H11 124.5 . . ? P12A P11A P12A 116.8(3) 4_565 . ? P12A P11A K201 83.07(14) 4_565 . ? P12A P11A K201 83.07(14) . . ? P12A P11A K101 72.37(12) 4_565 . ? P12A P11A K101 72.37(12) . . ? K201 P11A K101 131.34(8) . . ? P11A P12A C11A 106.1(2) . . ? P11A P12A K101 82.65(15) . . ? C11A P12A K101 73.89(16) . . ? P11A P12A K201 72.39(12) . . ? C11A P12A K201 73.76(16) . . ? K101 P12A K201 131.13(6) . . ? C11A C11A P12A 104.9(2) 4_565 . ? C11A C11A H11A 127.6 4_565 . ? P12A C11A H11A 127.6 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 76.28 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.765 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.063 _iucr_refine_instructions_details ; TITL 1b in P2(1)/m CELL 1.54184 9.0864 15.5733 14.6129 90.000 99.328 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H O P K UNIT 56 104 24 12 4 MERG 2 EQIV $1 X, 0.5000-Y, Z DFIX 2.085 0.020 P11 P12 DFIX 1.755 0.020 P12 C11 DFIX 1.380 0.020 C11 C11_$1 DFIX 2.085 0.020 P11A P12A DFIX 1.755 0.020 P12A C11A DFIX 1.380 0.020 C11A C11A_$1 EADP C11 C11A FMAP 2 PLAN 20 SIZE 0.24 0.30 0.34 ACTA BOND $H L.S. 12 TEMP -123.00 WGHT 0.061000 1.417000 FVAR 0.56284 0.47114 K101 5 0.814316 0.250000 0.593718 10.50000 0.02173 0.01877 = 0.02997 0.00000 0.00869 0.00000 O11 3 0.544944 0.250000 0.666844 10.50000 0.02705 0.02890 = 0.02602 0.00000 0.00993 0.00000 O12 3 0.703714 0.094444 0.663958 11.00000 0.02442 0.02240 = 0.03085 -0.00223 0.00247 -0.00595 O13 3 0.963545 0.091576 0.579268 11.00000 0.02570 0.02250 = 0.02892 0.00300 0.00245 0.00399 O14 3 1.118059 0.250000 0.580124 10.50000 0.02520 0.02829 = 0.02657 0.00000 0.01060 0.00000 C101 1 0.507701 0.174253 0.712350 11.00000 0.02499 0.03721 = 0.02757 0.00229 0.00853 -0.00750 AFIX 23 H10A 2 0.399918 0.173990 0.716185 11.00000 -1.20000 H10B 2 0.564432 0.172013 0.776141 11.00000 -1.20000 AFIX 0 C102 1 0.545852 0.098069 0.657774 11.00000 0.02449 0.03131 = 0.03113 0.00163 0.00422 -0.00966 AFIX 23 H10C 2 0.508882 0.044747 0.683134 11.00000 -1.20000 H10D 2 0.498251 0.103695 0.592142 11.00000 -1.20000 AFIX 0 C103 1 0.750311 0.021149 0.618031 11.00000 0.03449 0.01726 = 0.03253 -0.00206 -0.00011 -0.00416 AFIX 23 H10E 2 0.708070 0.023095 0.551214 11.00000 -1.20000 H10F 2 0.714907 -0.031932 0.644759 11.00000 -1.20000 AFIX 0 C104 1 0.917861 0.021609 0.630584 11.00000 0.03487 0.01661 = 0.03164 0.00111 0.00094 0.00174 AFIX 23 H10G 2 0.959915 0.027932 0.697101 11.00000 -1.20000 H10H 2 0.954342 -0.033124 0.608062 11.00000 -1.20000 AFIX 0 C105 1 1.121631 0.098271 0.591444 11.00000 0.02439 0.03090 = 0.03081 0.00124 0.00587 0.00922 AFIX 23 H10I 2 1.164635 0.045280 0.569241 11.00000 -1.20000 H10J 2 1.162519 0.105784 0.657986 11.00000 -1.20000 AFIX 0 C106 1 1.161383 0.174266 0.537103 11.00000 0.02526 0.03379 = 0.02784 -0.00050 0.00984 0.00677 AFIX 23 H10K 2 1.270100 0.175100 0.536259 11.00000 -1.20000 H10L 2 1.108908 0.170808 0.472320 11.00000 -1.20000 AFIX 0 K201 5 0.481807 0.250000 0.146317 10.50000 0.02443 0.02253 = 0.03587 0.00000 0.01135 0.00000 O21 3 0.184062 0.250000 0.172582 10.50000 0.02777 0.03248 = 0.02653 0.00000 0.01070 0.00000 O22 3 0.337411 0.091514 0.171887 11.00000 0.02504 0.02782 = 0.02630 -0.00362 0.00176 -0.00421 O23 3 0.596390 0.093272 0.083598 11.00000 0.02537 0.02332 = 0.03155 0.00261 0.00332 0.00183 O24 3 0.756604 0.250000 0.083898 10.50000 0.02778 0.02268 = 0.02581 0.00000 0.00916 0.00000 C201 1 0.139327 0.174142 0.214554 11.00000 0.02384 0.03882 = 0.02696 0.00185 0.00807 -0.00575 AFIX 23 H20A 2 0.030461 0.175220 0.214827 11.00000 -1.20000 H20B 2 0.190988 0.169986 0.279472 11.00000 -1.20000 AFIX 0 C202 1 0.179259 0.098628 0.159524 11.00000 0.02449 0.03585 = 0.02804 0.00045 0.00311 -0.00912 AFIX 23 H20C 2 0.135760 0.045476 0.181000 11.00000 -1.20000 H20D 2 0.138780 0.106798 0.093017 11.00000 -1.20000 AFIX 0 C203 1 0.382451 0.022178 0.119433 11.00000 0.03685 0.02225 = 0.02991 -0.00231 0.00462 -0.00447 AFIX 23 H20E 2 0.339507 0.029346 0.053160 11.00000 -1.20000 H20F 2 0.345621 -0.032716 0.141349 11.00000 -1.20000 AFIX 0 C204 1 0.549485 0.020543 0.130562 11.00000 0.03612 0.02087 = 0.03313 0.00263 0.00596 0.00270 AFIX 23 H20G 2 0.593165 0.022656 0.197145 11.00000 -1.20000 H20H 2 0.583144 -0.032983 0.103798 11.00000 -1.20000 AFIX 0 C205 1 0.754597 0.098308 0.092170 11.00000 0.02430 0.02484 = 0.03322 -0.00373 0.00095 0.00468 AFIX 23 H20I 2 0.794260 0.045168 0.068055 11.00000 -1.20000 H20J 2 0.799621 0.104826 0.158177 11.00000 -1.20000 AFIX 0 C206 1 0.792463 0.174328 0.037634 11.00000 0.02536 0.03132 = 0.02734 -0.00529 0.00694 0.00377 AFIX 23 H20K 2 0.900004 0.173799 0.033129 11.00000 -1.20000 H20L 2 0.734761 0.172439 -0.025908 11.00000 -1.20000 AFIX 0 P1 4 0.262515 0.250000 0.914834 10.50000 0.02898 0.09996 = 0.03386 0.00000 -0.00090 0.00000 P2 4 0.119576 0.147947 0.871469 11.00000 0.06468 0.03362 = 0.03698 0.00450 0.00977 0.01741 C1 1 -0.036856 0.207317 0.824006 11.00000 0.03310 0.05318 = 0.02524 -0.00284 0.00129 -0.00148 AFIX 43 H1 2 -0.124870 0.177763 0.797302 11.00000 -1.20000 AFIX 0 PART 1 SAME P1 > C1 P11 4 0.806862 0.250000 0.350328 20.50000 0.02883 0.39833 = 0.04142 0.00000 0.01156 0.00000 P12 4 0.696607 0.156536 0.362531 21.00000 0.18170 0.05142 = 0.04673 -0.01574 -0.03740 0.05764 C11 1 0.525040 0.199138 0.399967 21.00000 0.00900 0.03464 = 0.01864 -0.00109 0.00559 -0.00012 AFIX 43 H11 2 0.447594 0.164560 0.416866 21.00000 -1.20000 AFIX 0 PART 2 SAME P1 > C1 P11A 4 0.493287 0.250000 0.397680 -20.50000 0.01677 0.32017 = 0.02500 0.00000 0.00496 0.00000 P12A 4 0.583235 0.162806 0.392023 -21.00000 0.21741 0.08847 = 0.04941 0.03586 -0.06362 -0.11594 C11A 1 0.770761 0.194938 0.352720 -21.00000 0.00900 0.03464 = 0.01864 -0.00109 0.00559 -0.00012 AFIX 43 H11A 2 0.845705 0.157748 0.337013 -21.00000 -1.20000 HKLF 4 REM p21m in P2(1)/m REM R1 = 0.0433 for 4155 Fo > 4sig(Fo) and 0.0450 for all 4387 data REM 248 parameters refined using 15 restraints END WGHT 0.0610 1.4156 REM Highest difference peak 0.765, deepest hole -0.966, 1-sigma level 0.063 Q1 1 0.5435 0.1635 0.3987 11.00000 0.05 0.76 Q2 1 0.0122 0.2500 0.8256 10.50000 0.05 0.61 Q3 1 0.8189 0.2076 0.3448 11.00000 0.05 0.52 Q4 1 0.7412 0.2500 0.3400 10.50000 0.05 0.43 Q5 1 0.8986 0.2500 0.3406 10.50000 0.05 0.42 Q6 1 0.7405 0.1643 0.3464 11.00000 0.05 0.29 Q7 1 0.0313 0.1763 0.8461 11.00000 0.05 0.29 Q8 1 0.7470 0.1977 0.3953 11.00000 0.05 0.27 Q9 1 0.6248 0.1827 0.3530 11.00000 0.05 0.26 Q10 1 0.6608 0.1704 0.3990 11.00000 0.05 0.22 Q11 1 0.8365 0.0156 0.6233 11.00000 0.05 0.21 Q12 1 0.6272 0.0765 0.3673 11.00000 0.05 0.21 Q13 1 0.9372 0.1932 0.3543 11.00000 0.05 0.20 Q14 1 0.4701 0.0172 0.1268 11.00000 0.05 0.20 Q15 1 0.4105 0.2500 0.4246 10.50000 0.05 0.19 Q16 1 1.1408 0.1369 0.5576 11.00000 0.05 0.18 Q17 1 0.1231 0.0883 0.8794 11.00000 0.05 0.18 Q18 1 0.7819 0.1368 0.0630 11.00000 0.05 0.18 Q19 1 0.1650 0.1397 0.1862 11.00000 0.05 0.18 Q20 1 0.7832 0.1619 0.6329 11.00000 0.05 0.16 ; data_2 _database_code_depnum_ccdc_archive 'CCDC 873511' #TrackingRef '10375_web_deposit_cif_file_2_JoseGoicoechea_1332849746.2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)][As3C2H2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C18 H36 K N2 O6, C2 H2 As3' _chemical_formula_sum 'C20 H38 As3 K N2 O6' _chemical_formula_weight 666.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.00950(10) _cell_length_b 10.83120(10) _cell_length_c 25.7344(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.6210(10) _cell_angle_gamma 90.00 _cell_volume 2776.58(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8702 _cell_measurement_theta_min 3.4486 _cell_measurement_theta_max 76.2479 _exptl_crystal_description block _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 5.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4142 _exptl_absorpt_correction_T_max 0.5357 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.5035 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 14024 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 76.44 _reflns_number_total 5759 _reflns_number_gt 5407 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+2.4945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5759 _refine_ls_number_parameters 305 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.01656(10) 0.11812(15) 0.09251(5) 0.0556(2) Uani 0.8479(14) 1 d PD A 1 As2 As 0.02246(8) 0.08252(7) 0.18088(3) 0.03965(13) Uani 0.8479(14) 1 d PD A 1 As3 As -0.14561(4) -0.06190(3) 0.178070(14) 0.04004(12) Uani 0.8479(14) 1 d PD A 1 C1 C -0.1813(3) -0.0668(4) 0.10568(15) 0.0517(9) Uani 0.8479(14) 1 d PD A 1 H1 H -0.2470 -0.1241 0.0917 0.062 Uiso 0.8479(14) 1 calc PR A 1 C2 C -0.1243(6) 0.0011(5) 0.07268(15) 0.0416(6) Uani 0.8479(14) 1 d PD A 1 H2 H -0.1537 -0.0073 0.0366 0.050 Uiso 0.8479(14) 1 calc PR A 1 As1A As -0.1373(3) 0.0016(3) 0.05507(9) 0.0416(6) Uani 0.1521(14) 1 d PD A 2 As2A As 0.0417(8) 0.1137(9) 0.0969(3) 0.0556(2) Uani 0.1521(14) 1 d PD A 2 As3A As -0.0003(5) 0.0633(5) 0.1813(2) 0.03965(13) Uani 0.1521(14) 1 d PD A 2 C1A C -0.1505(14) -0.0448(14) 0.1597(4) 0.04004(12) Uani 0.1521(14) 1 d PD A 2 H1A H -0.1887 -0.0895 0.1864 0.048 Uiso 0.1521(14) 1 calc PR A 2 C2A C -0.2017(16) -0.0609(16) 0.1135(5) 0.0517(9) Uani 0.1521(14) 1 d PD A 2 H2A H -0.2807 -0.1099 0.1086 0.062 Uiso 0.1521(14) 1 calc PR A 2 K101 K 0.13699(4) -0.02889(4) 0.384379(16) 0.02578(10) Uani 1 1 d . . . N101 N 0.2838(2) 0.2033(2) 0.42010(9) 0.0436(5) Uani 1 1 d . . . N102 N -0.0190(2) -0.25748(19) 0.34930(8) 0.0352(4) Uani 1 1 d . . . O101 O 0.00518(19) 0.20641(16) 0.37247(7) 0.0401(4) Uani 1 1 d . . . O102 O -0.11146(16) -0.00984(18) 0.32717(7) 0.0391(4) Uani 1 1 d . . . O103 O 0.2544(2) -0.0095(2) 0.48901(6) 0.0474(5) Uani 1 1 d . . . O104 O 0.07181(18) -0.20520(17) 0.46034(6) 0.0401(4) Uani 1 1 d . . . O105 O 0.35281(15) 0.05264(15) 0.33179(6) 0.0319(3) Uani 1 1 d . . . O106 O 0.23210(17) -0.18058(15) 0.31017(6) 0.0319(3) Uani 1 1 d . . . C101 C 0.1863(4) 0.3014(3) 0.42594(13) 0.0566(8) Uani 1 1 d . . . H10A H 0.2349 0.3805 0.4319 0.068 Uiso 1 1 calc R . . H10B H 0.1391 0.2842 0.4572 0.068 Uiso 1 1 calc R . . C102 C 0.0840(4) 0.3154(2) 0.37956(14) 0.0550(7) Uani 1 1 d . . . H10C H 0.0251 0.3867 0.3850 0.066 Uiso 1 1 calc R . . H10D H 0.1300 0.3313 0.3479 0.066 Uiso 1 1 calc R . . C103 C -0.0705(3) 0.2047(3) 0.32247(10) 0.0459(6) Uani 1 1 d . . . H10E H -0.0101 0.1882 0.2950 0.055 Uiso 1 1 calc R . . H10F H -0.1135 0.2860 0.3153 0.055 Uiso 1 1 calc R . . C104 C -0.1748(3) 0.1070(3) 0.32156(10) 0.0432(6) Uani 1 1 d . . . H10G H -0.2318 0.1204 0.3504 0.052 Uiso 1 1 calc R . . H10H H -0.2328 0.1103 0.2881 0.052 Uiso 1 1 calc R . . C105 C -0.2051(2) -0.1083(3) 0.32719(12) 0.0473(6) Uani 1 1 d . . . H10I H -0.2833 -0.0915 0.3016 0.057 Uiso 1 1 calc R . . H10J H -0.2375 -0.1163 0.3622 0.057 Uiso 1 1 calc R . . C106 C -0.1374(3) -0.2257(3) 0.31311(11) 0.0456(6) Uani 1 1 d . . . H10K H -0.2030 -0.2942 0.3127 0.055 Uiso 1 1 calc R . . H10L H -0.1094 -0.2175 0.2774 0.055 Uiso 1 1 calc R . . C107 C 0.3631(4) 0.1799(4) 0.47043(12) 0.0620(9) Uani 1 1 d . . . H10M H 0.3934 0.2599 0.4860 0.074 Uiso 1 1 calc R . . H10N H 0.4440 0.1319 0.4640 0.074 Uiso 1 1 calc R . . C108 C 0.2869(4) 0.1106(4) 0.50911(11) 0.0622(9) Uani 1 1 d . . . H10O H 0.3426 0.1037 0.5430 0.075 Uiso 1 1 calc R . . H10P H 0.2037 0.1557 0.5149 0.075 Uiso 1 1 calc R . . C109 C 0.1917(3) -0.0811(4) 0.52583(10) 0.0559(8) Uani 1 1 d . . . H10Q H 0.1049 -0.0431 0.5324 0.067 Uiso 1 1 calc R . . H10R H 0.2496 -0.0842 0.5593 0.067 Uiso 1 1 calc R . . C110 C 0.1688(3) -0.2088(3) 0.50468(11) 0.0549(8) Uani 1 1 d . . . H11A H 0.2542 -0.2432 0.4946 0.066 Uiso 1 1 calc R . . H11B H 0.1366 -0.2628 0.5319 0.066 Uiso 1 1 calc R . . C111 C 0.0435(3) -0.3266(3) 0.44093(11) 0.0513(7) Uani 1 1 d . . . H11C H 0.0119 -0.3787 0.4689 0.062 Uiso 1 1 calc R . . H11D H 0.1262 -0.3642 0.4298 0.062 Uiso 1 1 calc R . . C112 C -0.0627(3) -0.3208(3) 0.39540(11) 0.0482(6) Uani 1 1 d . . . H11E H -0.0903 -0.4060 0.3854 0.058 Uiso 1 1 calc R . . H11F H -0.1422 -0.2776 0.4065 0.058 Uiso 1 1 calc R . . C113 C 0.3751(3) 0.2392(3) 0.38091(12) 0.0502(7) Uani 1 1 d . . . H11G H 0.4421 0.2986 0.3970 0.060 Uiso 1 1 calc R . . H11H H 0.3226 0.2816 0.3516 0.060 Uiso 1 1 calc R . . C114 C 0.4475(3) 0.1315(3) 0.35988(11) 0.0451(6) Uani 1 1 d . . . H11I H 0.5136 0.1613 0.3365 0.054 Uiso 1 1 calc R . . H11J H 0.4965 0.0854 0.3890 0.054 Uiso 1 1 calc R . . C115 C 0.4173(2) -0.0456(2) 0.30722(10) 0.0371(5) Uani 1 1 d . . . H11K H 0.4673 -0.0979 0.3340 0.045 Uiso 1 1 calc R . . H11L H 0.4821 -0.0115 0.2843 0.045 Uiso 1 1 calc R . . C116 C 0.3147(3) -0.1213(2) 0.27577(9) 0.0363(5) Uani 1 1 d . . . H11M H 0.2592 -0.0679 0.2510 0.044 Uiso 1 1 calc R . . H11N H 0.3594 -0.1839 0.2554 0.044 Uiso 1 1 calc R . . C117 C 0.1461(3) -0.2688(2) 0.28324(9) 0.0386(5) Uani 1 1 d . . . H11O H 0.1995 -0.3278 0.2643 0.046 Uiso 1 1 calc R . . H11P H 0.0815 -0.2269 0.2575 0.046 Uiso 1 1 calc R . . C118 C 0.0716(3) -0.3368(2) 0.32291(10) 0.0411(5) Uani 1 1 d . . . H11Q H 0.0190 -0.4046 0.3051 0.049 Uiso 1 1 calc R . . H11R H 0.1378 -0.3743 0.3494 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0661(5) 0.0556(3) 0.0450(3) 0.0185(2) 0.0055(3) 0.0070(4) As2 0.0436(4) 0.0361(3) 0.03762(15) -0.0031(2) -0.0046(2) -0.00943(19) As3 0.03863(18) 0.03212(18) 0.0490(2) -0.00417(14) 0.00246(15) 0.00032(13) C1 0.0344(16) 0.0584(18) 0.0592(19) -0.0386(16) -0.0111(13) 0.0116(14) C2 0.0608(11) 0.0445(8) 0.0181(15) 0.0011(12) -0.0035(12) 0.0111(7) As1A 0.0608(11) 0.0445(8) 0.0181(15) 0.0011(12) -0.0035(12) 0.0111(7) As2A 0.0661(5) 0.0556(3) 0.0450(3) 0.0185(2) 0.0055(3) 0.0070(4) As3A 0.0436(4) 0.0361(3) 0.03762(15) -0.0031(2) -0.0046(2) -0.00943(19) C1A 0.03863(18) 0.03212(18) 0.0490(2) -0.00417(14) 0.00246(15) 0.00032(13) C2A 0.0344(16) 0.0584(18) 0.0592(19) -0.0386(16) -0.0111(13) 0.0116(14) K101 0.0274(2) 0.0251(2) 0.02489(19) -0.00082(15) 0.00279(15) -0.00124(16) N101 0.0487(12) 0.0412(12) 0.0415(11) -0.0121(9) 0.0079(9) -0.0176(10) N102 0.0383(10) 0.0282(9) 0.0393(10) -0.0037(8) 0.0049(8) -0.0077(8) O101 0.0530(10) 0.0286(8) 0.0398(8) 0.0052(7) 0.0094(7) 0.0041(7) O102 0.0276(7) 0.0414(10) 0.0475(9) 0.0021(8) -0.0006(7) 0.0051(7) O103 0.0521(10) 0.0638(13) 0.0259(8) -0.0031(8) 0.0023(7) -0.0080(9) O104 0.0480(10) 0.0387(9) 0.0332(8) 0.0120(7) 0.0013(7) 0.0016(8) O105 0.0257(7) 0.0310(8) 0.0393(8) 0.0013(6) 0.0050(6) -0.0009(6) O106 0.0410(8) 0.0278(8) 0.0282(7) -0.0020(6) 0.0094(6) 0.0005(6) C101 0.074(2) 0.0342(14) 0.0648(18) -0.0216(13) 0.0207(16) -0.0150(14) C102 0.0711(19) 0.0229(12) 0.074(2) 0.0016(12) 0.0245(16) 0.0026(12) C103 0.0621(16) 0.0418(14) 0.0354(12) 0.0128(10) 0.0122(11) 0.0196(12) C104 0.0394(12) 0.0557(16) 0.0341(11) 0.0064(11) 0.0016(10) 0.0211(12) C105 0.0256(11) 0.0618(18) 0.0534(15) -0.0035(13) -0.0018(10) -0.0039(11) C106 0.0352(12) 0.0503(15) 0.0499(14) -0.0112(12) -0.0025(10) -0.0135(11) C107 0.0645(19) 0.072(2) 0.0474(15) -0.0199(15) -0.0065(14) -0.0295(17) C108 0.078(2) 0.077(2) 0.0305(12) -0.0171(14) -0.0034(13) -0.0162(18) C109 0.0540(16) 0.090(2) 0.0227(11) 0.0089(13) -0.0022(10) -0.0052(16) C110 0.0528(16) 0.070(2) 0.0408(13) 0.0274(14) -0.0021(12) 0.0036(14) C111 0.0740(19) 0.0329(13) 0.0493(15) 0.0150(11) 0.0174(14) 0.0009(13) C112 0.0592(16) 0.0339(13) 0.0540(15) -0.0004(11) 0.0179(13) -0.0165(12) C113 0.0540(15) 0.0414(14) 0.0567(15) -0.0088(12) 0.0135(13) -0.0248(13) C114 0.0328(12) 0.0516(16) 0.0508(14) -0.0016(12) 0.0034(10) -0.0141(11) C115 0.0335(11) 0.0366(12) 0.0436(12) 0.0106(10) 0.0151(9) 0.0078(9) C116 0.0478(13) 0.0319(11) 0.0317(10) 0.0041(9) 0.0158(10) 0.0077(10) C117 0.0471(13) 0.0338(12) 0.0347(11) -0.0102(9) 0.0033(10) 0.0024(10) C118 0.0521(14) 0.0245(11) 0.0470(13) -0.0091(10) 0.0068(11) -0.0039(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C2 1.927(6) . ? As1 As2 2.3017(14) . ? As2 As3 2.2931(6) . ? As3 C1 1.863(4) . ? C1 C2 1.297(7) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? As1A C2A 1.823(12) . ? As1A As2A 2.337(9) . ? As2A As3A 2.316(9) . ? As3A C1A 1.943(12) . ? C1A C2A 1.262(12) . ? C1A H1A 0.9500 . ? C2A H2A 0.9500 . ? K101 O106 2.7584(15) . ? K101 O102 2.7708(17) . ? K101 O105 2.8019(16) . ? K101 O103 2.8379(17) . ? K101 O104 2.8536(17) . ? K101 O101 2.8724(18) . ? K101 N101 3.010(2) . ? K101 N102 3.018(2) . ? N101 C101 1.461(4) . ? N101 C107 1.473(4) . ? N101 C113 1.478(3) . ? N102 C118 1.464(3) . ? N102 C112 1.473(3) . ? N102 C106 1.475(3) . ? O101 C102 1.421(3) . ? O101 C103 1.428(3) . ? O102 C104 1.417(3) . ? O102 C105 1.420(3) . ? O103 C109 1.417(4) . ? O103 C108 1.426(4) . ? O104 C110 1.425(3) . ? O104 C111 1.425(4) . ? O105 C114 1.420(3) . ? O105 C115 1.424(3) . ? O106 C117 1.421(3) . ? O106 C116 1.422(3) . ? C101 C102 1.502(5) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.485(4) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.502(4) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.511(5) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.496(5) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.504(4) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.503(4) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.490(4) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.513(4) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 As1 As2 95.67(13) . . ? As3 As2 As1 97.78(5) . . ? C1 As3 As2 96.84(13) . . ? C2 C1 As3 125.8(3) . . ? C2 C1 H1 117.1 . . ? As3 C1 H1 117.1 . . ? C1 C2 As1 123.8(3) . . ? C1 C2 H2 118.1 . . ? As1 C2 H2 118.1 . . ? C2A As1A As2A 97.5(4) . . ? As3A As2A As1A 96.2(3) . . ? C1A As3A As2A 94.7(4) . . ? C2A C1A As3A 125.7(10) . . ? C2A C1A H1A 117.1 . . ? As3A C1A H1A 117.1 . . ? C1A C2A As1A 125.6(10) . . ? C1A C2A H2A 117.2 . . ? As1A C2A H2A 117.2 . . ? O106 K101 O102 91.67(5) . . ? O106 K101 O105 61.23(5) . . ? O102 K101 O105 114.47(5) . . ? O106 K101 O103 124.19(6) . . ? O102 K101 O103 139.92(6) . . ? O105 K101 O103 99.67(5) . . ? O106 K101 O104 101.14(5) . . ? O102 K101 O104 99.22(5) . . ? O105 K101 O104 141.32(5) . . ? O103 K101 O104 60.05(6) . . ? O106 K101 O101 129.84(5) . . ? O102 K101 O101 59.88(6) . . ? O105 K101 O101 92.10(5) . . ? O103 K101 O101 100.30(6) . . ? O104 K101 O101 122.24(5) . . ? O106 K101 N101 121.18(6) . . ? O102 K101 N101 119.07(7) . . ? O105 K101 N101 60.52(5) . . ? O103 K101 N101 60.28(6) . . ? O104 K101 N101 119.16(6) . . ? O101 K101 N101 59.79(6) . . ? O106 K101 N102 60.51(5) . . ? O102 K101 N102 59.40(6) . . ? O105 K101 N102 120.99(5) . . ? O103 K101 N102 119.89(6) . . ? O104 K101 N102 60.63(5) . . ? O101 K101 N102 118.50(6) . . ? N101 K101 N102 178.05(6) . . ? C101 N101 C107 110.0(2) . . ? C101 N101 C113 110.0(2) . . ? C107 N101 C113 109.2(2) . . ? C101 N101 K101 109.18(16) . . ? C107 N101 K101 109.25(18) . . ? C113 N101 K101 109.14(15) . . ? C118 N102 C112 110.3(2) . . ? C118 N102 C106 109.9(2) . . ? C112 N102 C106 109.5(2) . . ? C118 N102 K101 107.12(14) . . ? C112 N102 K101 109.08(15) . . ? C106 N102 K101 110.97(15) . . ? C102 O101 C103 111.4(2) . . ? C102 O101 K101 118.67(17) . . ? C103 O101 K101 106.37(14) . . ? C104 O102 C105 112.5(2) . . ? C104 O102 K101 119.35(15) . . ? C105 O102 K101 120.13(15) . . ? C109 O103 C108 110.9(2) . . ? C109 O103 K101 115.14(16) . . ? C108 O103 K101 118.05(17) . . ? C110 O104 C111 110.6(2) . . ? C110 O104 K101 112.53(16) . . ? C111 O104 K101 115.36(14) . . ? C114 O105 C115 111.50(19) . . ? C114 O105 K101 116.84(14) . . ? C115 O105 K101 112.53(13) . . ? C117 O106 C116 111.18(18) . . ? C117 O106 K101 120.32(13) . . ? C116 O106 K101 115.04(13) . . ? N101 C101 C102 113.7(2) . . ? N101 C101 H10A 108.8 . . ? C102 C101 H10A 108.8 . . ? N101 C101 H10B 108.8 . . ? C102 C101 H10B 108.8 . . ? H10A C101 H10B 107.7 . . ? O101 C102 C101 110.2(2) . . ? O101 C102 H10C 109.6 . . ? C101 C102 H10C 109.6 . . ? O101 C102 H10D 109.6 . . ? C101 C102 H10D 109.6 . . ? H10C C102 H10D 108.1 . . ? O101 C103 C104 109.5(2) . . ? O101 C103 H10E 109.8 . . ? C104 C103 H10E 109.8 . . ? O101 C103 H10F 109.8 . . ? C104 C103 H10F 109.8 . . ? H10E C103 H10F 108.2 . . ? O102 C104 C103 109.1(2) . . ? O102 C104 H10G 109.9 . . ? C103 C104 H10G 109.9 . . ? O102 C104 H10H 109.9 . . ? C103 C104 H10H 109.9 . . ? H10G C104 H10H 108.3 . . ? O102 C105 C106 108.8(2) . . ? O102 C105 H10I 109.9 . . ? C106 C105 H10I 109.9 . . ? O102 C105 H10J 109.9 . . ? C106 C105 H10J 109.9 . . ? H10I C105 H10J 108.3 . . ? N102 C106 C105 113.5(2) . . ? N102 C106 H10K 108.9 . . ? C105 C106 H10K 108.9 . . ? N102 C106 H10L 108.9 . . ? C105 C106 H10L 108.9 . . ? H10K C106 H10L 107.7 . . ? N101 C107 C108 113.7(3) . . ? N101 C107 H10M 108.8 . . ? C108 C107 H10M 108.8 . . ? N101 C107 H10N 108.8 . . ? C108 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? O103 C108 C107 109.0(2) . . ? O103 C108 H10O 109.9 . . ? C107 C108 H10O 109.9 . . ? O103 C108 H10P 109.9 . . ? C107 C108 H10P 109.9 . . ? H10O C108 H10P 108.3 . . ? O103 C109 C110 108.9(2) . . ? O103 C109 H10Q 109.9 . . ? C110 C109 H10Q 109.9 . . ? O103 C109 H10R 109.9 . . ? C110 C109 H10R 109.9 . . ? H10Q C109 H10R 108.3 . . ? O104 C110 C109 109.5(2) . . ? O104 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O104 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.2 . . ? O104 C111 C112 109.6(2) . . ? O104 C111 H11C 109.7 . . ? C112 C111 H11C 109.7 . . ? O104 C111 H11D 109.7 . . ? C112 C111 H11D 109.7 . . ? H11C C111 H11D 108.2 . . ? N102 C112 C111 113.8(2) . . ? N102 C112 H11E 108.8 . . ? C111 C112 H11E 108.8 . . ? N102 C112 H11F 108.8 . . ? C111 C112 H11F 108.8 . . ? H11E C112 H11F 107.7 . . ? N101 C113 C114 113.2(2) . . ? N101 C113 H11G 108.9 . . ? C114 C113 H11G 108.9 . . ? N101 C113 H11H 108.9 . . ? C114 C113 H11H 108.9 . . ? H11G C113 H11H 107.8 . . ? O105 C114 C113 109.2(2) . . ? O105 C114 H11I 109.8 . . ? C113 C114 H11I 109.8 . . ? O105 C114 H11J 109.8 . . ? C113 C114 H11J 109.8 . . ? H11I C114 H11J 108.3 . . ? O105 C115 C116 109.55(19) . . ? O105 C115 H11K 109.8 . . ? C116 C115 H11K 109.8 . . ? O105 C115 H11L 109.8 . . ? C116 C115 H11L 109.8 . . ? H11K C115 H11L 108.2 . . ? O106 C116 C115 108.78(19) . . ? O106 C116 H11M 109.9 . . ? C115 C116 H11M 109.9 . . ? O106 C116 H11N 109.9 . . ? C115 C116 H11N 109.9 . . ? H11M C116 H11N 108.3 . . ? O106 C117 C118 108.25(19) . . ? O106 C117 H11O 110.0 . . ? C118 C117 H11O 110.0 . . ? O106 C117 H11P 110.0 . . ? C118 C117 H11P 110.0 . . ? H11O C117 H11P 108.4 . . ? N102 C118 C117 113.3(2) . . ? N102 C118 H11Q 108.9 . . ? C117 C118 H11Q 108.9 . . ? N102 C118 H11R 108.9 . . ? C117 C118 H11R 108.9 . . ? H11Q C118 H11R 107.7 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 76.44 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.932 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.069 _iucr_refine_instructions_details ; TITL 2 in P2(1)/n CELL 1.54178 10.0095 10.8312 25.7344 90.000 95.621 90.000 ZERR 4.00 0.0001 0.0001 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O K AS UNIT 80 152 8 24 4 12 MERG 2 DFIX 1.380 0.020 C1A C2A DFIX 1.380 0.020 C1 C2 DFIX 1.880 0.020 C2A AS1A DFIX 1.880 0.020 C1A AS3A DFIX 1.890 0.020 C1 AS3 DFIX 1.880 0.020 C2 AS1 DFIX 2.300 0.020 AS1 AS2 DFIX 2.300 0.020 AS2 AS3 DFIX 2.300 0.020 AS1A AS2A DFIX 2.300 0.020 AS2A AS3A EADP AS1 AS2A EADP AS2 AS3A EADP AS3 C1A EADP C1 C2A EADP C2 AS1A FLAT 0.100 AS1A AS2A AS3A C1A C2A FLAT 0.100 AS1 AS2 AS3 C1 C2 DFIX 2.800 0.020 C1A AS1A DFIX 2.800 0.020 C2A AS3A DFIX 3.100 0.020 AS2A C2A DFIX 2.800 0.020 C1A AS1A TEMP -123 SIZE 0.18 0.14 0.12 ACTA FMAP 2 PLAN 20 BOND $H L.S. 12 WGHT 0.037800 2.494500 FVAR 0.09099 0.84790 PART 1 AS1 6 0.016558 0.118120 0.092505 21.00000 0.06607 0.05561 = 0.04502 0.01853 0.00545 0.00698 AS2 6 0.022456 0.082517 0.180876 21.00000 0.04357 0.03607 = 0.03762 -0.00311 -0.00460 -0.00943 AS3 6 -0.145606 -0.061902 0.178070 21.00000 0.03863 0.03212 = 0.04902 -0.00417 0.00246 0.00032 C1 1 -0.181267 -0.066796 0.105680 21.00000 0.03437 0.05841 = 0.05917 -0.03859 -0.01111 0.01155 AFIX 43 H1 2 -0.247050 -0.124135 0.091685 21.00000 -1.20000 AFIX 0 C2 1 -0.124264 0.001129 0.072675 21.00000 0.06080 0.04449 = 0.01810 0.00107 -0.00350 0.01107 AFIX 43 H2 2 -0.153681 -0.007312 0.036619 21.00000 -1.20000 AFIX 0 PART 2 SAME AS1 > C2 AS1A 6 -0.137257 0.001616 0.055073 -21.00000 0.06080 0.04449 = 0.01810 0.00107 -0.00350 0.01107 AS2A 6 0.041655 0.113694 0.096928 -21.00000 0.06607 0.05561 = 0.04502 0.01853 0.00545 0.00698 AS3A 6 -0.000293 0.063327 0.181257 -21.00000 0.04357 0.03607 = 0.03762 -0.00311 -0.00460 -0.00943 C1A 1 -0.150470 -0.044821 0.159743 -21.00000 0.03863 0.03212 = 0.04902 -0.00417 0.00246 0.00032 AFIX 43 H1A 2 -0.188676 -0.089491 0.186405 -21.00000 -1.20000 AFIX 0 C2A 1 -0.201699 -0.060922 0.113465 -21.00000 0.03437 0.05841 = 0.05917 -0.03859 -0.01111 0.01155 AFIX 43 H2A 2 -0.280692 -0.109875 0.108635 -21.00000 -1.20000 AFIX 0 PART 0 K101 5 0.136992 -0.028890 0.384379 11.00000 0.02741 0.02508 = 0.02489 -0.00082 0.00279 -0.00124 N101 3 0.283776 0.203260 0.420096 11.00000 0.04866 0.04124 = 0.04152 -0.01213 0.00791 -0.01760 N102 3 -0.019005 -0.257476 0.349301 11.00000 0.03830 0.02824 = 0.03925 -0.00372 0.00485 -0.00767 O101 4 0.005183 0.206415 0.372466 11.00000 0.05296 0.02855 = 0.03978 0.00521 0.00941 0.00413 O102 4 -0.111456 -0.009835 0.327171 11.00000 0.02755 0.04137 = 0.04750 0.00211 -0.00063 0.00507 O103 4 0.254358 -0.009533 0.489006 11.00000 0.05214 0.06382 = 0.02587 -0.00310 0.00229 -0.00803 O104 4 0.071810 -0.205196 0.460338 11.00000 0.04797 0.03874 = 0.03319 0.01196 0.00129 0.00163 O105 4 0.352805 0.052644 0.331787 11.00000 0.02574 0.03104 = 0.03933 0.00130 0.00502 -0.00089 O106 4 0.232097 -0.180580 0.310171 11.00000 0.04103 0.02780 = 0.02817 -0.00204 0.00936 0.00048 C101 1 0.186298 0.301424 0.425939 11.00000 0.07367 0.03416 = 0.06475 -0.02164 0.02069 -0.01501 AFIX 23 H10A 2 0.234928 0.380538 0.431896 11.00000 -1.20000 H10B 2 0.139145 0.284166 0.457219 11.00000 -1.20000 AFIX 0 C102 1 0.083960 0.315360 0.379557 11.00000 0.07113 0.02293 = 0.07444 0.00156 0.02446 0.00256 AFIX 23 H10C 2 0.025074 0.386712 0.384964 11.00000 -1.20000 H10D 2 0.129975 0.331261 0.347875 11.00000 -1.20000 AFIX 0 C103 1 -0.070473 0.204650 0.322466 11.00000 0.06210 0.04175 = 0.03541 0.01282 0.01224 0.01965 AFIX 23 H10E 2 -0.010059 0.188184 0.295018 11.00000 -1.20000 H10F 2 -0.113515 0.285990 0.315318 11.00000 -1.20000 AFIX 0 C104 1 -0.174801 0.107018 0.321558 11.00000 0.03936 0.05568 = 0.03410 0.00643 0.00163 0.02113 AFIX 23 H10G 2 -0.231785 0.120432 0.350396 11.00000 -1.20000 H10H 2 -0.232824 0.110339 0.288146 11.00000 -1.20000 AFIX 0 C105 1 -0.205112 -0.108316 0.327190 11.00000 0.02556 0.06180 = 0.05336 -0.00353 -0.00184 -0.00391 AFIX 23 H10I 2 -0.283334 -0.091522 0.301557 11.00000 -1.20000 H10J 2 -0.237455 -0.116320 0.362178 11.00000 -1.20000 AFIX 0 C106 1 -0.137428 -0.225715 0.313106 11.00000 0.03518 0.05029 = 0.04991 -0.01124 -0.00250 -0.01351 AFIX 23 H10K 2 -0.202989 -0.294237 0.312656 11.00000 -1.20000 H10L 2 -0.109390 -0.217511 0.277429 11.00000 -1.20000 AFIX 0 C107 1 0.363060 0.179873 0.470429 11.00000 0.06453 0.07152 = 0.04743 -0.01993 -0.00649 -0.02951 AFIX 23 H10M 2 0.393382 0.259895 0.486001 11.00000 -1.20000 H10N 2 0.443995 0.131871 0.464011 11.00000 -1.20000 AFIX 0 C108 1 0.286904 0.110557 0.509105 11.00000 0.07761 0.07678 = 0.03052 -0.01706 -0.00339 -0.01619 AFIX 23 H10O 2 0.342591 0.103714 0.542960 11.00000 -1.20000 H10P 2 0.203677 0.155736 0.514907 11.00000 -1.20000 AFIX 0 C109 1 0.191700 -0.081066 0.525830 11.00000 0.05395 0.08973 = 0.02274 0.00889 -0.00219 -0.00523 AFIX 23 H10Q 2 0.104948 -0.043142 0.532401 11.00000 -1.20000 H10R 2 0.249589 -0.084188 0.559278 11.00000 -1.20000 AFIX 0 C110 1 0.168846 -0.208790 0.504676 11.00000 0.05281 0.06992 = 0.04076 0.02744 -0.00210 0.00357 AFIX 23 H11A 2 0.254222 -0.243168 0.494571 11.00000 -1.20000 H11B 2 0.136606 -0.262812 0.531860 11.00000 -1.20000 AFIX 0 C111 1 0.043523 -0.326603 0.440934 11.00000 0.07399 0.03291 = 0.04929 0.01499 0.01741 0.00090 AFIX 23 H11C 2 0.011918 -0.378686 0.468880 11.00000 -1.20000 H11D 2 0.126225 -0.364165 0.429760 11.00000 -1.20000 AFIX 0 C112 1 -0.062661 -0.320841 0.395398 11.00000 0.05921 0.03385 = 0.05398 -0.00035 0.01789 -0.01646 AFIX 23 H11E 2 -0.090318 -0.406019 0.385394 11.00000 -1.20000 H11F 2 -0.142249 -0.277587 0.406488 11.00000 -1.20000 AFIX 0 C113 1 0.375122 0.239249 0.380906 11.00000 0.05401 0.04143 = 0.05665 -0.00882 0.01353 -0.02484 AFIX 23 H11G 2 0.442082 0.298646 0.396991 11.00000 -1.20000 H11H 2 0.322563 0.281641 0.351560 11.00000 -1.20000 AFIX 0 C114 1 0.447535 0.131473 0.359885 11.00000 0.03283 0.05161 = 0.05075 -0.00159 0.00343 -0.01407 AFIX 23 H11I 2 0.513579 0.161292 0.336538 11.00000 -1.20000 H11J 2 0.496538 0.085412 0.389034 11.00000 -1.20000 AFIX 0 C115 1 0.417251 -0.045596 0.307217 11.00000 0.03349 0.03659 = 0.04356 0.01065 0.01509 0.00778 AFIX 23 H11K 2 0.467256 -0.097900 0.334035 11.00000 -1.20000 H11L 2 0.482051 -0.011550 0.284280 11.00000 -1.20000 AFIX 0 C116 1 0.314671 -0.121333 0.275766 11.00000 0.04778 0.03190 = 0.03169 0.00412 0.01577 0.00768 AFIX 23 H11M 2 0.259189 -0.067882 0.251012 11.00000 -1.20000 H11N 2 0.359415 -0.183917 0.255422 11.00000 -1.20000 AFIX 0 C117 1 0.146091 -0.268837 0.283235 11.00000 0.04707 0.03383 = 0.03471 -0.01017 0.00330 0.00242 AFIX 23 H11O 2 0.199488 -0.327762 0.264350 11.00000 -1.20000 H11P 2 0.081496 -0.226895 0.257469 11.00000 -1.20000 AFIX 0 C118 1 0.071643 -0.336823 0.322910 11.00000 0.05210 0.02449 = 0.04704 -0.00911 0.00681 -0.00394 AFIX 23 H11Q 2 0.018976 -0.404648 0.305111 11.00000 -1.20000 H11R 2 0.137805 -0.374288 0.349419 11.00000 -1.20000 HKLF 4 REM p21n in P2(1)/n REM R1 = 0.0327 for 5407 Fo > 4sig(Fo) and 0.0351 for all 5759 data REM 305 parameters refined using 28 restraints END WGHT 0.0378 2.5002 REM Highest difference peak 0.932, deepest hole -0.975, 1-sigma level 0.069 Q1 1 -0.1614 -0.0659 0.1476 11.00000 0.05 0.93 Q2 1 -0.0732 0.1541 0.1367 11.00000 0.05 0.91 Q3 1 -0.1909 -0.0044 0.0860 11.00000 0.05 0.58 Q4 1 -0.0582 -0.0324 0.1775 11.00000 0.05 0.57 Q5 1 -0.0658 0.0358 0.0686 11.00000 0.05 0.46 Q6 1 0.1130 -0.3031 0.3035 11.00000 0.05 0.23 Q7 1 0.0968 0.1193 0.0968 11.00000 0.05 0.22 Q8 1 0.2931 0.1895 0.4456 11.00000 0.05 0.21 Q9 1 0.3272 0.2080 0.4081 11.00000 0.05 0.20 Q10 1 -0.0437 -0.0260 0.3266 11.00000 0.05 0.20 Q11 1 -0.0643 -0.0200 0.0266 11.00000 0.05 0.20 Q12 1 -0.0306 -0.2781 0.3689 11.00000 0.05 0.19 Q13 1 -0.0219 -0.3130 0.4219 11.00000 0.05 0.19 Q14 1 0.1794 -0.0289 0.3854 11.00000 0.05 0.19 Q15 1 0.1739 -0.3485 0.4412 11.00000 0.05 0.19 Q16 1 0.0297 -0.2859 0.3350 11.00000 0.05 0.19 Q17 1 0.2951 0.0604 0.3356 11.00000 0.05 0.19 Q18 1 0.1324 -0.0084 0.3944 11.00000 0.05 0.19 Q19 1 0.3190 -0.0293 0.4802 11.00000 0.05 0.18 Q20 1 0.2676 -0.1542 0.2960 11.00000 0.05 0.18 ; data_2b _database_code_depnum_ccdc_archive 'CCDC 873512' #TrackingRef '10376_web_deposit_cif_file_3_JoseGoicoechea_1332849746.2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(18-crown-6)][As3C2H2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C12 H24 K O6, C2 H2 As3' _chemical_formula_sum 'C14 H26 As3 K O6' _chemical_formula_weight 554.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.1068(2) _cell_length_b 15.6018(4) _cell_length_c 14.9447(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.208(2) _cell_angle_gamma 90.00 _cell_volume 2101.63(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4124 _cell_measurement_theta_min 2.9850 _cell_measurement_theta_max 76.2093 _exptl_crystal_description needle _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 7.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6557 _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.5035 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 11024 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 76.39 _reflns_number_total 4517 _reflns_number_gt 3684 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1448P)^2^+17.8392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4517 _refine_ls_number_parameters 242 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.1012 _refine_ls_wR_factor_ref 0.2929 _refine_ls_wR_factor_gt 0.2778 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.289 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K101 K 0.8132(3) 0.2500 0.59420(19) 0.0346(6) Uani 1 2 d S . . O11 O 0.5428(9) 0.2500 0.6649(6) 0.0359(18) Uani 1 2 d S . . O12 O 0.7020(6) 0.0951(4) 0.6629(4) 0.0348(13) Uani 1 1 d . . . O13 O 0.9638(7) 0.0918(4) 0.5795(4) 0.0364(13) Uani 1 1 d . . . O14 O 1.1168(9) 0.2500 0.5798(6) 0.0363(18) Uani 1 2 d S . . C101 C 0.5052(10) 0.1741(6) 0.7099(6) 0.040(2) Uani 1 1 d . . . H10A H 0.3976 0.1735 0.7139 0.048 Uiso 1 1 calc R . . H10B H 0.5600 0.1724 0.7721 0.048 Uiso 1 1 calc R . . C102 C 0.5456(10) 0.0975(6) 0.6571(6) 0.041(2) Uani 1 1 d . . . H10C H 0.5092 0.0443 0.6826 0.049 Uiso 1 1 calc R . . H10D H 0.4996 0.1023 0.5932 0.049 Uiso 1 1 calc R . . C103 C 0.7500(10) 0.0203(5) 0.6187(6) 0.0373(18) Uani 1 1 d . . . H10E H 0.7082 0.0208 0.5538 0.045 Uiso 1 1 calc R . . H10F H 0.7155 -0.0322 0.6465 0.045 Uiso 1 1 calc R . . C104 C 0.9162(11) 0.0217(5) 0.6293(6) 0.0385(19) Uani 1 1 d . . . H10G H 0.9572 0.0276 0.6940 0.046 Uiso 1 1 calc R . . H10H H 0.9531 -0.0328 0.6068 0.046 Uiso 1 1 calc R . . C105 C 1.1217(10) 0.0981(6) 0.5906(7) 0.041(2) Uani 1 1 d . . . H10I H 1.1646 0.0454 0.5680 0.049 Uiso 1 1 calc R . . H10J H 1.1615 0.1050 0.6554 0.049 Uiso 1 1 calc R . . C106 C 1.1621(10) 0.1743(6) 0.5382(6) 0.041(2) Uani 1 1 d . . . H10K H 1.2706 0.1755 0.5375 0.049 Uiso 1 1 calc R . . H10L H 1.1121 0.1707 0.4750 0.049 Uiso 1 1 calc R . . K201 K 0.4749(3) 0.2500 0.1479(2) 0.0398(6) Uani 1 2 d S . . O21 O 0.1773(10) 0.2500 0.1727(6) 0.041(2) Uani 1 2 d S . . O22 O 0.3288(7) 0.0916(4) 0.1703(4) 0.0402(14) Uani 1 1 d . . . O23 O 0.5878(7) 0.0938(4) 0.0833(4) 0.0379(13) Uani 1 1 d . . . O24 O 0.7468(10) 0.2500 0.0829(6) 0.0364(18) Uani 1 2 d S . . C201 C 0.1291(10) 0.1746(7) 0.2128(6) 0.046(2) Uani 1 1 d . . . H20A H 0.0203 0.1763 0.2119 0.056 Uiso 1 1 calc R . . H20B H 0.1767 0.1704 0.2765 0.056 Uiso 1 1 calc R . . C202 C 0.1711(10) 0.0983(7) 0.1601(7) 0.045(2) Uani 1 1 d . . . H20C H 0.1285 0.0455 0.1825 0.054 Uiso 1 1 calc R . . H20D H 0.1309 0.1052 0.0953 0.054 Uiso 1 1 calc R . . C203 C 0.3751(11) 0.0213(6) 0.1203(6) 0.043(2) Uani 1 1 d . . . H20E H 0.3314 0.0265 0.0559 0.051 Uiso 1 1 calc R . . H20F H 0.3400 -0.0331 0.1439 0.051 Uiso 1 1 calc R . . C204 C 0.5405(11) 0.0205(6) 0.1282(7) 0.043(2) Uani 1 1 d . . . H20G H 0.5845 0.0214 0.1927 0.052 Uiso 1 1 calc R . . H20H H 0.5739 -0.0324 0.1004 0.052 Uiso 1 1 calc R . . C205 C 0.7452(10) 0.0985(6) 0.0906(7) 0.044(2) Uani 1 1 d . . . H20I H 0.7847 0.0455 0.0666 0.053 Uiso 1 1 calc R . . H20J H 0.7892 0.1048 0.1547 0.053 Uiso 1 1 calc R . . C206 C 0.7841(10) 0.1742(6) 0.0375(6) 0.041(2) Uani 1 1 d . . . H20K H 0.8915 0.1738 0.0329 0.049 Uiso 1 1 calc R . . H20L H 0.7282 0.1723 -0.0244 0.049 Uiso 1 1 calc R . . As1 As 0.26783(19) 0.2500 0.91674(13) 0.0638(6) Uani 1 2 d SD . . As2 As 0.10951(15) 0.13987(8) 0.86973(8) 0.0536(4) Uani 1 1 d D . . C1 C -0.0481(10) 0.2096(6) 0.8217(6) 0.055(3) Uani 1 1 d D . . H1 H -0.1364 0.1819 0.7949 0.065 Uiso 1 1 calc R . . As11 As 0.8115(8) 0.2500 0.3499(5) 0.268(12) Uani 0.369(6) 2 d SPDU . 1 As12 As 0.6915(10) 0.1497(3) 0.3635(4) 0.152(4) Uani 0.369(6) 1 d PDU . 1 C11 C 0.520(3) 0.2040(7) 0.3912(18) 0.152(4) Uani 0.369(6) 1 d PDU . 1 H11 H 0.4373 0.1721 0.4046 0.182 Uiso 0.369(6) 1 calc PR . 1 As21 As 0.4847(3) 0.2500 0.3934(2) 0.158(4) Uani 0.631(6) 2 d SPD . 2 As22 As 0.6028(9) 0.1505(3) 0.3864(3) 0.213(4) Uani 0.631(6) 1 d PD . 2 C21 C 0.7825(19) 0.2028(8) 0.3630(16) 0.158(4) Uani 0.631(6) 1 d PD . 2 H11A H 0.8663 0.1703 0.3521 0.190 Uiso 0.631(6) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K101 0.0293(11) 0.0259(11) 0.0510(15) 0.000 0.0144(10) 0.000 O11 0.033(4) 0.039(5) 0.039(4) 0.000 0.015(3) 0.000 O12 0.033(3) 0.028(3) 0.043(3) -0.002(2) 0.004(2) -0.008(2) O13 0.036(3) 0.029(3) 0.043(3) 0.003(2) 0.003(2) 0.006(2) O14 0.035(4) 0.037(4) 0.040(4) 0.000 0.018(4) 0.000 C101 0.034(4) 0.044(5) 0.043(5) 0.006(4) 0.010(4) -0.008(4) C102 0.032(4) 0.046(5) 0.045(5) 0.000(4) 0.009(3) -0.012(4) C103 0.045(5) 0.022(4) 0.044(4) -0.002(3) 0.003(4) -0.004(3) C104 0.050(5) 0.022(4) 0.043(5) 0.001(3) 0.004(4) 0.001(3) C105 0.036(4) 0.042(5) 0.046(5) 0.006(4) 0.010(4) 0.010(4) C106 0.035(4) 0.050(5) 0.040(4) -0.001(4) 0.013(4) 0.009(4) K201 0.0368(13) 0.0319(13) 0.0539(16) 0.000 0.0178(11) 0.000 O21 0.041(5) 0.049(5) 0.037(4) 0.000 0.012(4) 0.000 O22 0.041(3) 0.037(3) 0.041(3) -0.001(3) 0.002(3) -0.008(3) O23 0.038(3) 0.031(3) 0.044(3) 0.003(3) 0.003(3) 0.001(2) O24 0.039(4) 0.033(4) 0.040(4) 0.000 0.014(4) 0.000 C201 0.036(4) 0.067(7) 0.039(5) 0.002(4) 0.012(4) -0.009(4) C202 0.038(5) 0.053(6) 0.042(5) -0.002(4) 0.001(4) -0.016(4) C203 0.056(6) 0.030(4) 0.042(5) 0.001(4) 0.004(4) -0.007(4) C204 0.052(5) 0.030(4) 0.047(5) 0.003(4) 0.008(4) 0.006(4) C205 0.040(5) 0.036(5) 0.054(5) -0.002(4) 0.001(4) 0.012(4) C206 0.036(4) 0.046(5) 0.042(5) -0.006(4) 0.009(4) 0.004(4) As1 0.0364(8) 0.1025(16) 0.0509(10) 0.000 0.0003(7) 0.000 As2 0.0721(9) 0.0391(7) 0.0500(7) 0.0034(5) 0.0098(6) 0.0139(5) C1 0.039(4) 0.096(8) 0.028(4) -0.002(4) -0.001(3) 0.017(5) As11 0.043(4) 0.73(4) 0.040(4) 0.000 0.021(3) 0.000 As12 0.276(9) 0.073(3) 0.073(3) -0.046(3) -0.089(5) 0.127(5) C11 0.276(9) 0.073(3) 0.073(3) -0.046(3) -0.089(5) 0.127(5) As21 0.0286(15) 0.406(12) 0.0421(18) 0.000 0.0135(13) 0.000 As22 0.371(9) 0.126(3) 0.096(3) 0.068(3) -0.127(4) -0.189(5) C21 0.0286(15) 0.406(12) 0.0421(18) 0.000 0.0135(13) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K101 O14 2.804(9) . ? K101 O11 2.815(8) . ? K101 O13 2.847(6) 4_565 ? K101 O13 2.847(6) . ? K101 O12 2.866(6) 4_565 ? K101 O12 2.866(6) . ? K101 C21 3.50(2) . ? K101 C21 3.50(2) 4_565 ? K101 C1 3.511(9) 4_665 ? K101 C1 3.511(9) 1_655 ? K101 As11 3.649(8) . ? K101 As22 3.745(4) . ? O11 C101 1.428(10) 4_565 ? O11 C101 1.428(10) . ? O12 C102 1.416(10) . ? O12 C103 1.439(10) . ? O13 C104 1.426(10) . ? O13 C105 1.427(11) . ? O14 C106 1.423(10) . ? O14 C106 1.423(10) 4_565 ? C101 C102 1.506(13) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.499(13) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.497(13) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? K201 O24 2.786(9) . ? K201 O21 2.787(9) . ? K201 O22 2.849(6) . ? K201 O22 2.849(6) 4_565 ? K201 O23 2.866(6) 4_565 ? K201 O23 2.866(6) . ? K201 As21 3.657(5) . ? K201 As1 3.692(4) 1_554 ? K201 As12 3.860(5) 4_565 ? K201 As12 3.860(5) . ? K201 As22 3.909(5) 4_565 ? K201 As22 3.909(5) . ? O21 C201 1.417(11) 4_565 ? O21 C201 1.417(11) . ? O22 C203 1.424(11) . ? O22 C202 1.427(11) . ? O23 C204 1.423(11) . ? O23 C205 1.424(11) . ? O24 C206 1.429(10) . ? O24 C206 1.429(10) 4_565 ? C201 C202 1.507(15) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.494(14) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.493(14) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? As1 As2 2.2881(18) . ? As1 As2 2.2881(18) 4_565 ? As1 K201 3.692(4) 1_556 ? As2 C1 1.861(8) . ? C1 C1 1.260(17) 4_565 ? C1 K101 3.511(9) 1_455 ? C1 H1 0.9500 . ? As11 As12 1.935(9) . ? As11 As12 1.935(9) 4_565 ? As12 C11 1.871(19) . ? C11 C11 1.44(2) 4_565 ? C11 H11 0.9500 . ? As21 As22 1.900(8) 4_565 ? As21 As22 1.900(8) . ? As22 C21 1.906(14) . ? C21 C21 1.47(2) 4_565 ? C21 H11A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 K101 O11 162.6(3) . . ? O14 K101 O13 60.18(13) . 4_565 ? O11 K101 O13 119.09(13) . 4_565 ? O14 K101 O13 60.18(13) . . ? O11 K101 O13 119.09(13) . . ? O13 K101 O13 120.2(3) 4_565 . ? O14 K101 O12 115.47(15) . 4_565 ? O11 K101 O12 59.54(13) . 4_565 ? O13 K101 O12 59.71(18) 4_565 4_565 ? O13 K101 O12 163.2(2) . 4_565 ? O14 K101 O12 115.47(15) . . ? O11 K101 O12 59.54(13) . . ? O13 K101 O12 163.2(2) 4_565 . ? O13 K101 O12 59.71(18) . . ? O12 K101 O12 115.0(3) 4_565 . ? O14 K101 C21 82.2(3) . . ? O11 K101 C21 114.8(3) . . ? O13 K101 C21 94.4(2) 4_565 . ? O13 K101 C21 73.3(3) . . ? O12 K101 C21 123.2(3) 4_565 . ? O12 K101 C21 101.2(2) . . ? O14 K101 C21 82.2(3) . 4_565 ? O11 K101 C21 114.8(3) . 4_565 ? O13 K101 C21 73.3(3) 4_565 4_565 ? O13 K101 C21 94.4(2) . 4_565 ? O12 K101 C21 101.2(2) 4_565 4_565 ? O12 K101 C21 123.2(3) . 4_565 ? C21 K101 C21 24.2(4) . 4_565 ? O14 K101 C1 81.5(2) . 4_665 ? O11 K101 C1 81.4(2) . 4_665 ? O13 K101 C1 78.98(19) 4_565 4_665 ? O13 K101 C1 96.9(2) . 4_665 ? O12 K101 C1 66.3(2) 4_565 4_665 ? O12 K101 C1 84.33(19) . 4_665 ? C21 K101 C1 163.6(3) . 4_665 ? C21 K101 C1 152.1(3) 4_565 4_665 ? O14 K101 C1 81.5(2) . 1_655 ? O11 K101 C1 81.4(2) . 1_655 ? O13 K101 C1 96.9(2) 4_565 1_655 ? O13 K101 C1 78.98(19) . 1_655 ? O12 K101 C1 84.33(19) 4_565 1_655 ? O12 K101 C1 66.3(2) . 1_655 ? C21 K101 C1 152.1(3) . 1_655 ? C21 K101 C1 163.6(3) 4_565 1_655 ? C1 K101 C1 20.7(3) 4_665 1_655 ? O14 K101 As11 77.7(2) . . ? O11 K101 As11 119.8(2) . . ? O13 K101 As11 81.71(15) 4_565 . ? O13 K101 As11 81.71(15) . . ? O12 K101 As11 114.02(14) 4_565 . ? O12 K101 As11 114.02(14) . . ? C21 K101 As11 12.88(19) . . ? C21 K101 As11 12.88(19) 4_565 . ? C1 K101 As11 156.72(19) 4_665 . ? C1 K101 As11 156.72(19) 1_655 . ? O14 K101 As22 109.2(2) . . ? O11 K101 As22 86.5(2) . . ? O13 K101 As22 119.36(15) 4_565 . ? O13 K101 As22 76.80(17) . . ? O12 K101 As22 118.78(19) 4_565 . ? O12 K101 As22 77.43(14) . . ? C21 K101 As22 30.2(2) . . ? C21 K101 As22 46.4(3) 4_565 . ? C1 K101 As22 161.46(16) 4_665 . ? C1 K101 As22 143.07(16) 1_655 . ? As11 K101 As22 40.69(12) . . ? C101 O11 C101 112.1(9) 4_565 . ? C101 O11 K101 117.3(5) 4_565 . ? C101 O11 K101 117.3(5) . . ? C102 O12 C103 111.3(7) . . ? C102 O12 K101 111.1(5) . . ? C103 O12 K101 112.0(5) . . ? C104 O13 C105 111.6(7) . . ? C104 O13 K101 116.0(5) . . ? C105 O13 K101 114.8(5) . . ? C106 O14 C106 112.2(9) . 4_565 ? C106 O14 K101 112.6(5) . . ? C106 O14 K101 112.6(5) 4_565 . ? O11 C101 C102 108.5(7) . . ? O11 C101 H10A 110.0 . . ? C102 C101 H10A 110.0 . . ? O11 C101 H10B 110.0 . . ? C102 C101 H10B 110.0 . . ? H10A C101 H10B 108.4 . . ? O12 C102 C101 108.0(7) . . ? O12 C102 H10C 110.1 . . ? C101 C102 H10C 110.1 . . ? O12 C102 H10D 110.1 . . ? C101 C102 H10D 110.1 . . ? H10C C102 H10D 108.4 . . ? O12 C103 C104 108.0(7) . . ? O12 C103 H10E 110.1 . . ? C104 C103 H10E 110.1 . . ? O12 C103 H10F 110.1 . . ? C104 C103 H10F 110.1 . . ? H10E C103 H10F 108.4 . . ? O13 C104 C103 109.5(7) . . ? O13 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O13 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O13 C105 C106 108.2(7) . . ? O13 C105 H10I 110.1 . . ? C106 C105 H10I 110.1 . . ? O13 C105 H10J 110.1 . . ? C106 C105 H10J 110.1 . . ? H10I C105 H10J 108.4 . . ? O14 C106 C105 108.8(7) . . ? O14 C106 H10K 109.9 . . ? C105 C106 H10K 109.9 . . ? O14 C106 H10L 109.9 . . ? C105 C106 H10L 109.9 . . ? H10K C106 H10L 108.3 . . ? O24 K201 O21 167.4(3) . . ? O24 K201 O22 119.59(14) . . ? O21 K201 O22 60.36(14) . . ? O24 K201 O22 119.59(14) . 4_565 ? O21 K201 O22 60.36(14) . 4_565 ? O22 K201 O22 120.4(3) . 4_565 ? O24 K201 O23 60.20(14) . 4_565 ? O21 K201 O23 116.56(15) . 4_565 ? O22 K201 O23 166.7(2) . 4_565 ? O22 K201 O23 59.83(19) 4_565 4_565 ? O24 K201 O23 60.20(14) . . ? O21 K201 O23 116.56(15) . . ? O22 K201 O23 59.83(19) . . ? O22 K201 O23 166.7(2) 4_565 . ? O23 K201 O23 116.5(3) 4_565 . ? O24 K201 As21 117.0(2) . . ? O21 K201 As21 75.6(2) . . ? O22 K201 As21 80.05(14) . . ? O22 K201 As21 80.05(14) 4_565 . ? O23 K201 As21 112.29(14) 4_565 . ? O23 K201 As21 112.29(14) . . ? O24 K201 As1 92.0(2) . 1_554 ? O21 K201 As1 75.4(2) . 1_554 ? O22 K201 As1 85.71(14) . 1_554 ? O22 K201 As1 85.71(14) 4_565 1_554 ? O23 K201 As1 81.06(14) 4_565 1_554 ? O23 K201 As1 81.06(14) . 1_554 ? As21 K201 As1 151.02(10) . 1_554 ? O24 K201 As12 85.3(2) . 4_565 ? O21 K201 As12 106.2(2) . 4_565 ? O22 K201 As12 116.44(16) . 4_565 ? O22 K201 As12 75.05(18) 4_565 4_565 ? O23 K201 As12 76.77(15) 4_565 4_565 ? O23 K201 As12 117.4(2) . 4_565 ? As21 K201 As12 39.33(11) . 4_565 ? As1 K201 As12 155.88(7) 1_554 4_565 ? O24 K201 As12 85.3(2) . . ? O21 K201 As12 106.2(2) . . ? O22 K201 As12 75.05(18) . . ? O22 K201 As12 116.44(16) 4_565 . ? O23 K201 As12 117.4(2) 4_565 . ? O23 K201 As12 76.77(15) . . ? As21 K201 As12 39.33(11) . . ? As1 K201 As12 155.88(7) 1_554 . ? As12 K201 As12 47.82(16) 4_565 . ? O24 K201 As22 98.9(2) . 4_565 ? O21 K201 As22 92.7(2) . 4_565 ? O22 K201 As22 108.72(19) . 4_565 ? O22 K201 As22 68.39(14) 4_565 4_565 ? O23 K201 As22 83.95(17) 4_565 4_565 ? O23 K201 As22 124.77(16) . 4_565 ? As21 K201 As22 28.85(13) . 4_565 ? As1 K201 As22 154.02(6) 1_554 4_565 ? As12 K201 As22 13.60(17) 4_565 4_565 ? As12 K201 As22 49.46(7) . 4_565 ? O24 K201 As22 98.9(2) . . ? O21 K201 As22 92.7(2) . . ? O22 K201 As22 68.39(14) . . ? O22 K201 As22 108.72(19) 4_565 . ? O23 K201 As22 124.77(16) 4_565 . ? O23 K201 As22 83.95(17) . . ? As21 K201 As22 28.85(13) . . ? As1 K201 As22 154.02(6) 1_554 . ? As12 K201 As22 49.46(7) 4_565 . ? As12 K201 As22 13.60(17) . . ? As22 K201 As22 46.81(15) 4_565 . ? C201 O21 C201 112.1(10) 4_565 . ? C201 O21 K201 114.9(5) 4_565 . ? C201 O21 K201 114.9(5) . . ? C203 O22 C202 111.7(7) . . ? C203 O22 K201 115.4(5) . . ? C202 O22 K201 113.8(6) . . ? C204 O23 C205 112.1(7) . . ? C204 O23 K201 112.2(5) . . ? C205 O23 K201 109.6(5) . . ? C206 O24 C206 111.7(9) . 4_565 ? C206 O24 K201 116.7(5) . . ? C206 O24 K201 116.7(5) 4_565 . ? O21 C201 C202 108.5(7) . . ? O21 C201 H20A 110.0 . . ? C202 C201 H20A 110.0 . . ? O21 C201 H20B 110.0 . . ? C202 C201 H20B 110.0 . . ? H20A C201 H20B 108.4 . . ? O22 C202 C201 109.2(7) . . ? O22 C202 H20C 109.8 . . ? C201 C202 H20C 109.8 . . ? O22 C202 H20D 109.8 . . ? C201 C202 H20D 109.8 . . ? H20C C202 H20D 108.3 . . ? O22 C203 C204 109.6(8) . . ? O22 C203 H20E 109.8 . . ? C204 C203 H20E 109.8 . . ? O22 C203 H20F 109.8 . . ? C204 C203 H20F 109.8 . . ? H20E C203 H20F 108.2 . . ? O23 C204 C203 109.0(8) . . ? O23 C204 H20G 109.9 . . ? C203 C204 H20G 109.9 . . ? O23 C204 H20H 109.9 . . ? C203 C204 H20H 109.9 . . ? H20G C204 H20H 108.3 . . ? O23 C205 C206 108.3(7) . . ? O23 C205 H20I 110.0 . . ? C206 C205 H20I 110.0 . . ? O23 C205 H20J 110.0 . . ? C206 C205 H20J 110.0 . . ? H20I C205 H20J 108.4 . . ? O24 C206 C205 108.1(7) . . ? O24 C206 H20K 110.1 . . ? C205 C206 H20K 110.1 . . ? O24 C206 H20L 110.1 . . ? C205 C206 H20L 110.1 . . ? H20K C206 H20L 108.4 . . ? As2 As1 As2 97.34(9) . 4_565 ? As2 As1 K201 120.17(6) . 1_556 ? As2 As1 K201 120.17(6) 4_565 1_556 ? C1 As2 As1 95.6(3) . . ? C1 C1 As2 125.8(3) 4_565 . ? C1 C1 K101 79.66(14) 4_565 1_455 ? As2 C1 K101 129.0(4) . 1_455 ? C1 C1 H1 117.1 4_565 . ? As2 C1 H1 117.1 . . ? K101 C1 H1 60.5 1_455 . ? As12 As11 As12 107.9(4) . 4_565 ? As12 As11 K101 79.5(2) . . ? As12 As11 K101 79.5(2) 4_565 . ? C11 As12 As11 99.1(5) . . ? C11 As12 K101 76.0(8) . . ? As11 As12 K101 70.5(3) . . ? C11 As12 K201 70.0(8) . . ? As11 As12 K201 79.3(3) . . ? K101 As12 K201 129.62(10) . . ? C11 C11 As12 116.9(5) 4_565 . ? C11 C11 H11 121.6 4_565 . ? As12 C11 H11 121.6 . . ? As22 As21 As22 109.6(3) 4_565 . ? As22 As21 K201 82.97(17) 4_565 . ? As22 As21 K201 82.97(17) . . ? As22 As21 K101 70.51(14) 4_565 . ? As22 As21 K101 70.51(14) . . ? K201 As21 K101 132.38(10) . . ? As21 As22 C21 99.7(4) . . ? As21 As22 K101 80.92(19) . . ? C21 As22 K101 67.9(7) . . ? As21 As22 K201 68.18(15) . . ? C21 As22 K201 79.3(7) . . ? K101 As22 K201 129.92(9) . . ? C21 C21 As22 115.4(4) 4_565 . ? C21 C21 K101 77.9(2) 4_565 . ? As22 C21 K101 81.9(7) . . ? C21 C21 H11A 122.3 4_565 . ? As22 C21 H11A 122.3 . . ? K101 C21 H11A 109.2 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 76.39 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 4.377 _refine_diff_density_min -2.552 _refine_diff_density_rms 0.186 _iucr_refine_instructions_details ; TITL 2b in P2(1)/m CELL 1.54178 9.1068 15.6018 14.9447 90.000 98.208 90.000 ZERR 4.00 0.0002 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H O AS K UNIT 56 104 24 12 4 MERG 2 EQIV $1 X, 0.5000-Y, Z DFIX 2.300 0.020 AS11 AS12 DFIX 1.900 0.020 AS12 AS11 DFIX 1.400 0.020 C11 C11_$1 DFIX 2.300 0.020 AS21 AS22 DFIX 1.900 0.020 AS22 C21 DFIX 1.400 0.020 C21 C21_$1 DFIX 1.400 0.020 C1 C1_$1 FLAT 0.100 AS11 AS12 C11 AS12_$1 C11_$1 FLAT 0.100 AS21 AS22 C21 AS22_$1 C21_$1 ISOR 0.05 AS11 ISOR 0.02 AS12 C11 EADP C11 AS12 EADP C21 AS21 FMAP 2 PLAN 20 TEMP -123 SIZE 0.06 0.02 0.01 ACTA BOND $H L.S. 12 TEMP -123.00 WGHT 0.144800 17.839212 FVAR 0.06343 0.36901 K101 5 0.813181 0.250000 0.594199 10.50000 0.02934 0.02589 = 0.05097 0.00000 0.01443 0.00000 O11 3 0.542765 0.250000 0.664874 10.50000 0.03258 0.03937 = 0.03872 0.00000 0.01504 0.00000 O12 3 0.702044 0.095115 0.662863 11.00000 0.03294 0.02750 = 0.04340 -0.00217 0.00357 -0.00792 O13 3 0.963822 0.091849 0.579450 11.00000 0.03556 0.02940 = 0.04332 0.00293 0.00276 0.00565 O14 3 1.116832 0.250000 0.579790 10.50000 0.03517 0.03714 = 0.04000 0.00000 0.01750 0.00000 C101 1 0.505168 0.174097 0.709918 11.00000 0.03382 0.04407 = 0.04326 0.00600 0.01032 -0.00758 AFIX 23 H10A 2 0.397574 0.173508 0.713858 11.00000 -1.20000 H10B 2 0.560004 0.172393 0.772058 11.00000 -1.20000 AFIX 0 C102 1 0.545586 0.097502 0.657132 11.00000 0.03157 0.04628 = 0.04488 0.00044 0.00877 -0.01161 AFIX 23 H10C 2 0.509205 0.044281 0.682600 11.00000 -1.20000 H10D 2 0.499593 0.102330 0.593186 11.00000 -1.20000 AFIX 0 C103 1 0.750021 0.020335 0.618733 11.00000 0.04488 0.02242 = 0.04367 -0.00188 0.00280 -0.00407 AFIX 23 H10E 2 0.708236 0.020795 0.553836 11.00000 -1.20000 H10F 2 0.715517 -0.032198 0.646513 11.00000 -1.20000 AFIX 0 C104 1 0.916213 0.021703 0.629267 11.00000 0.04982 0.02240 = 0.04263 0.00061 0.00442 0.00106 AFIX 23 H10G 2 0.957225 0.027606 0.693978 11.00000 -1.20000 H10H 2 0.953075 -0.032759 0.606757 11.00000 -1.20000 AFIX 0 C105 1 1.121747 0.098137 0.590585 11.00000 0.03558 0.04248 = 0.04633 0.00568 0.01012 0.01011 AFIX 23 H10I 2 1.164625 0.045417 0.568042 11.00000 -1.20000 H10J 2 1.161491 0.104991 0.655382 11.00000 -1.20000 AFIX 0 C106 1 1.162121 0.174291 0.538187 11.00000 0.03469 0.05032 = 0.04010 -0.00105 0.01302 0.00910 AFIX 23 H10K 2 1.270636 0.175505 0.537466 11.00000 -1.20000 H10L 2 1.112131 0.170742 0.474969 11.00000 -1.20000 AFIX 0 K201 5 0.474871 0.250000 0.147937 10.50000 0.03682 0.03190 = 0.05385 0.00000 0.01785 0.00000 O21 3 0.177274 0.250000 0.172745 10.50000 0.04053 0.04866 = 0.03677 0.00000 0.01220 0.00000 O22 3 0.328847 0.091562 0.170299 11.00000 0.04112 0.03744 = 0.04091 -0.00066 0.00178 -0.00801 O23 3 0.587786 0.093753 0.083346 11.00000 0.03818 0.03094 = 0.04367 0.00255 0.00263 0.00141 O24 3 0.746787 0.250000 0.082916 10.50000 0.03893 0.03287 = 0.03986 0.00000 0.01416 0.00000 C201 1 0.129136 0.174637 0.212815 11.00000 0.03568 0.06714 = 0.03855 0.00233 0.01221 -0.00859 AFIX 23 H20A 2 0.020258 0.176311 0.211894 11.00000 -1.20000 H20B 2 0.176702 0.170439 0.276502 11.00000 -1.20000 AFIX 0 C202 1 0.171108 0.098317 0.160054 11.00000 0.03771 0.05339 = 0.04204 -0.00183 0.00124 -0.01573 AFIX 23 H20C 2 0.128513 0.045480 0.182534 11.00000 -1.20000 H20D 2 0.130876 0.105194 0.095333 11.00000 -1.20000 AFIX 0 C203 1 0.375059 0.021260 0.120276 11.00000 0.05555 0.02968 = 0.04219 0.00068 0.00439 -0.00748 AFIX 23 H20E 2 0.331406 0.026524 0.055940 11.00000 -1.20000 H20F 2 0.339957 -0.033147 0.143943 11.00000 -1.20000 AFIX 0 C204 1 0.540485 0.020485 0.128193 11.00000 0.05203 0.02980 = 0.04747 0.00340 0.00752 0.00579 AFIX 23 H20G 2 0.584457 0.021373 0.192715 11.00000 -1.20000 H20H 2 0.573874 -0.032357 0.100446 11.00000 -1.20000 AFIX 0 C205 1 0.745165 0.098541 0.090566 11.00000 0.04034 0.03605 = 0.05387 -0.00249 0.00100 0.01158 AFIX 23 H20I 2 0.784673 0.045480 0.066581 11.00000 -1.20000 H20J 2 0.789185 0.104809 0.154733 11.00000 -1.20000 AFIX 0 C206 1 0.784090 0.174205 0.037476 11.00000 0.03560 0.04643 = 0.04182 -0.00593 0.00860 0.00411 AFIX 23 H20K 2 0.891457 0.173756 0.032862 11.00000 -1.20000 H20L 2 0.728212 0.172308 -0.024382 11.00000 -1.20000 AFIX 0 AS1 4 0.267832 0.250000 0.916738 10.50000 0.03637 0.10247 = 0.05091 0.00000 0.00032 0.00000 AS2 4 0.109512 0.139867 0.869726 11.00000 0.07209 0.03905 = 0.05000 0.00344 0.00981 0.01387 C1 1 -0.048117 0.209613 0.821746 11.00000 0.03866 0.09577 = 0.02771 -0.00202 -0.00079 0.01713 AFIX 43 H1 2 -0.136374 0.181861 0.794882 11.00000 -1.20000 AFIX 0 PART 1 SAME AS1 > C1 AS11 4 0.811483 0.250000 0.349917 20.50000 0.04302 0.72670 = 0.03951 0.00000 0.02089 0.00000 AS12 4 0.691478 0.149730 0.363453 21.00000 0.27603 0.07266 = 0.07325 -0.04607 -0.08902 0.12739 C11 1 0.520294 0.203958 0.391161 21.00000 0.27603 0.07266 = 0.07325 -0.04607 -0.08902 0.12739 AFIX 43 H11 2 0.437275 0.172088 0.404598 21.00000 -1.20000 AFIX 0 PART 2 SAME AS1 > C1 AS21 4 0.484662 0.250000 0.393395 -20.50000 0.02858 0.40567 = 0.04212 0.00000 0.01350 0.00000 AS22 4 0.602779 0.150475 0.386392 -21.00000 0.37119 0.12575 = 0.09593 0.06836 -0.12745 -0.18865 C21 1 0.782537 0.202828 0.363008 -21.00000 0.02858 0.40567 = 0.04212 0.00000 0.01350 0.00000 AFIX 43 H11A 2 0.866350 0.170280 0.352105 -21.00000 -1.20000 HKLF 4 REM p21m in P2(1)/m REM R1 = 0.1012 for 3684 Fo > 4sig(Fo) and 0.1155 for all 4517 data REM 242 parameters refined using 38 restraints END WGHT 0.1391 18.9446 REM Highest difference peak 4.377, deepest hole -2.552, 1-sigma level 0.186 Q1 1 0.7787 0.1883 0.3468 11.00000 0.05 4.32 Q2 1 0.4753 0.2500 0.3508 10.50000 0.05 2.04 Q3 1 0.9225 0.2500 0.6585 10.50000 0.05 1.61 Q4 1 -0.0078 0.2500 0.8193 10.50000 0.05 1.60 Q5 1 0.6438 0.1469 0.3745 11.00000 0.05 1.40 Q6 1 0.2578 0.2500 0.1093 10.50000 0.05 1.39 Q7 1 0.4357 0.2500 0.3954 10.50000 0.05 1.37 Q8 1 0.8204 0.2500 0.3986 10.50000 0.05 1.15 Q9 1 0.1271 0.1747 0.9234 11.00000 0.05 0.81 Q10 1 0.1570 0.1479 0.8621 11.00000 0.05 0.75 Q11 1 0.2470 0.1999 0.8516 11.00000 0.05 0.63 Q12 1 0.6114 0.2500 0.6843 10.50000 0.05 0.60 Q13 1 -0.0187 0.1912 0.8604 11.00000 0.05 0.58 Q14 1 1.0855 0.0907 0.5988 11.00000 0.05 0.58 Q15 1 0.7318 0.2500 0.2994 10.50000 0.05 0.57 Q16 1 0.1451 0.0878 0.1392 11.00000 0.05 0.56 Q17 1 0.4331 0.0899 0.0859 11.00000 0.05 0.49 Q18 1 1.0530 0.2500 0.6395 10.50000 0.05 0.48 Q19 1 0.1906 0.2377 0.9796 11.00000 0.05 0.46 Q20 1 -0.0798 0.2194 0.8954 11.00000 0.05 0.45 ; data_3 _database_code_depnum_ccdc_archive 'CCDC 873513' #TrackingRef '10377_web_deposit_cif_file_4_JoseGoicoechea_1332849746.4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K-(2,2,2-crypt)][(As3C2H2)Ru(Me-allyl)2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C18 H36 K N2 O6, C10 H16 As3 Ru' _chemical_formula_sum 'C28 H52 As3 K N2 O6 Ru' _chemical_formula_weight 877.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.73910(10) _cell_length_b 17.42280(10) _cell_length_c 18.64660(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.6810(10) _cell_angle_gamma 90.00 _cell_volume 3633.60(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.00(10) _cell_measurement_reflns_used 53310 _cell_measurement_theta_min 3.5502 _cell_measurement_theta_max 76.2207 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 7.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2341 _exptl_absorpt_correction_T_max 0.5717 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ; _diffrn_ambient_temperature 150.00(10) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5035 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 78137 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0086 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 76.41 _reflns_number_total 7613 _reflns_number_gt 7422 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+1.1971P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7613 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.702955(15) 0.297795(11) -0.031725(10) 0.04009(5) Uani 1 1 d . . . As2 As 0.587541(17) 0.388823(10) 0.008707(10) 0.03940(5) Uani 1 1 d . . . As3 As 0.396552(16) 0.346110(11) -0.062709(10) 0.03979(5) Uani 1 1 d . . . C1 C 0.45497(15) 0.26263(10) -0.10699(9) 0.0372(3) Uani 1 1 d . . . H1 H 0.3961 0.2302 -0.1390 0.045 Uiso 1 1 calc R . . C2 C 0.57261(15) 0.24335(9) -0.09824(9) 0.0361(3) Uani 1 1 d . . . H2 H 0.5890 0.2016 -0.1263 0.043 Uiso 1 1 calc R . . Ru1 Ru 0.539225(10) 0.244307(6) 0.016293(6) 0.02958(4) Uani 1 1 d . . . C3 C 0.52901(18) 0.24904(10) 0.13083(9) 0.0406(4) Uani 1 1 d . . . C4 C 0.64613(16) 0.22779(10) 0.13070(9) 0.0392(3) Uani 1 1 d . . . C5 C 0.65819(16) 0.16092(10) 0.08971(9) 0.0398(3) Uani 1 1 d . . . C6 C 0.75252(18) 0.27793(12) 0.16753(10) 0.0508(4) Uani 1 1 d . . . H6A H 0.7891 0.2613 0.2197 0.076 Uiso 1 1 calc R . . H6B H 0.7265 0.3314 0.1669 0.076 Uiso 1 1 calc R . . H6C H 0.8112 0.2736 0.1399 0.076 Uiso 1 1 calc R . . C7 C 0.40948(15) 0.14992(9) 0.00215(10) 0.0377(3) Uani 1 1 d . . . H7A H 0.4315 0.1096 -0.0286 0.045 Uiso 1 1 calc R . . H7B H 0.4189 0.1275 0.0524 0.045 Uiso 1 1 calc R . . C8 C 0.28125(16) 0.16813(10) -0.03280(11) 0.0441(4) Uani 1 1 d . . . C9 C 0.2189(2) 0.20583(13) 0.01761(15) 0.0630(6) Uani 1 1 d . . . H9A H 0.1369 0.2191 -0.0119 0.095 Uiso 1 1 calc R . . H9B H 0.2620 0.2526 0.0394 0.095 Uiso 1 1 calc R . . H9C H 0.2171 0.1704 0.0581 0.095 Uiso 1 1 calc R . . C10 C 0.22102(17) 0.15188(12) -0.10404(13) 0.0543(5) Uani 1 1 d . . . H10A H 0.2603 0.1273 -0.1354 0.065 Uiso 1 1 calc R . . H10B H 0.1388 0.1649 -0.1235 0.065 Uiso 1 1 calc R . . K101 K 0.20862(3) 0.529637(18) 0.244222(17) 0.03275(7) Uani 1 1 d . . . N101 N -0.05742(12) 0.51738(8) 0.20798(8) 0.0377(3) Uani 1 1 d . . . N102 N 0.47533(12) 0.53967(8) 0.28185(8) 0.0380(3) Uani 1 1 d . . . O101 O 0.11217(10) 0.45116(7) 0.34495(6) 0.0378(2) Uani 1 1 d . . . O102 O 0.36034(10) 0.48528(7) 0.39335(6) 0.0381(2) Uani 1 1 d . . . O103 O 0.07086(10) 0.66388(7) 0.22804(7) 0.0388(2) Uani 1 1 d . . . O104 O 0.31423(10) 0.67326(7) 0.24233(7) 0.0400(2) Uani 1 1 d . . . O105 O 0.07014(11) 0.45929(7) 0.10703(7) 0.0450(3) Uani 1 1 d . . . O106 O 0.32398(11) 0.44386(7) 0.15742(7) 0.0438(3) Uani 1 1 d . . . C101 C -0.08362(15) 0.45792(11) 0.25636(11) 0.0466(4) Uani 1 1 d . . . H10C H -0.0696 0.4070 0.2371 0.056 Uiso 1 1 calc R . . H10D H -0.1693 0.4610 0.2529 0.056 Uiso 1 1 calc R . . C102 C -0.01048(15) 0.46374(11) 0.33772(10) 0.0454(4) Uani 1 1 d . . . H10E H -0.0207 0.5153 0.3573 0.054 Uiso 1 1 calc R . . H10F H -0.0382 0.4251 0.3676 0.054 Uiso 1 1 calc R . . C103 C 0.18319(15) 0.45206(10) 0.42256(9) 0.0387(3) Uani 1 1 d . . . H10G H 0.1491 0.4165 0.4520 0.046 Uiso 1 1 calc R . . H10H H 0.1844 0.5043 0.4436 0.046 Uiso 1 1 calc R . . C104 C 0.30706(15) 0.42771(10) 0.42685(9) 0.0393(3) Uani 1 1 d . . . H10I H 0.3551 0.4203 0.4801 0.047 Uiso 1 1 calc R . . H10J H 0.3045 0.3784 0.4000 0.047 Uiso 1 1 calc R . . C105 C 0.47870(14) 0.46452(11) 0.39618(10) 0.0416(4) Uani 1 1 d . . . H10K H 0.4774 0.4168 0.3672 0.050 Uiso 1 1 calc R . . H10L H 0.5274 0.4552 0.4490 0.050 Uiso 1 1 calc R . . C106 C 0.53251(14) 0.52892(11) 0.36315(10) 0.0435(4) Uani 1 1 d . . . H10M H 0.5258 0.5772 0.3895 0.052 Uiso 1 1 calc R . . H10N H 0.6186 0.5183 0.3723 0.052 Uiso 1 1 calc R . . C107 C -0.10393(14) 0.59177(10) 0.22352(10) 0.0402(3) Uani 1 1 d . . . H10O H -0.0850 0.5979 0.2787 0.048 Uiso 1 1 calc R . . H10P H -0.1921 0.5915 0.2018 0.048 Uiso 1 1 calc R . . C108 C -0.05500(15) 0.65960(10) 0.19274(10) 0.0423(4) Uani 1 1 d . . . H10Q H -0.0721 0.6541 0.1376 0.051 Uiso 1 1 calc R . . H10R H -0.0936 0.7073 0.2026 0.051 Uiso 1 1 calc R . . C109 C 0.12119(17) 0.73028(10) 0.20565(12) 0.0470(4) Uani 1 1 d . . . H10S H 0.0752 0.7763 0.2113 0.056 Uiso 1 1 calc R . . H10T H 0.1176 0.7259 0.1521 0.056 Uiso 1 1 calc R . . C110 C 0.24845(18) 0.73808(10) 0.25370(12) 0.0468(4) Uani 1 1 d . . . H11A H 0.2835 0.7856 0.2402 0.056 Uiso 1 1 calc R . . H11B H 0.2521 0.7415 0.3074 0.056 Uiso 1 1 calc R . . C111 C 0.43845(15) 0.68111(11) 0.28036(10) 0.0440(4) Uani 1 1 d . . . H11C H 0.4525 0.6806 0.3355 0.053 Uiso 1 1 calc R . . H11D H 0.4677 0.7307 0.2667 0.053 Uiso 1 1 calc R . . C112 C 0.50513(15) 0.61591(11) 0.25841(11) 0.0440(4) Uani 1 1 d . . . H11E H 0.4877 0.6162 0.2030 0.053 Uiso 1 1 calc R . . H11F H 0.5920 0.6247 0.2810 0.053 Uiso 1 1 calc R . . C113 C -0.11235(16) 0.49698(12) 0.12826(10) 0.0505(4) Uani 1 1 d . . . H11G H -0.1148 0.5433 0.0970 0.061 Uiso 1 1 calc R . . H11H H -0.1958 0.4804 0.1208 0.061 Uiso 1 1 calc R . . C114 C -0.04738(17) 0.43429(12) 0.10138(12) 0.0535(5) Uani 1 1 d . . . H11I H -0.0436 0.3877 0.1324 0.064 Uiso 1 1 calc R . . H11J H -0.0908 0.4213 0.0484 0.064 Uiso 1 1 calc R . . C115 C 0.13320(19) 0.40331(11) 0.07862(11) 0.0502(4) Uani 1 1 d . . . H11K H 0.0873 0.3902 0.0261 0.060 Uiso 1 1 calc R . . H11L H 0.1429 0.3560 0.1093 0.060 Uiso 1 1 calc R . . C116 C 0.25245(19) 0.43380(12) 0.08106(10) 0.0524(4) Uani 1 1 d . . . H11M H 0.2924 0.3976 0.0555 0.063 Uiso 1 1 calc R . . H11N H 0.2430 0.4836 0.0543 0.063 Uiso 1 1 calc R . . C117 C 0.43902(17) 0.47165(11) 0.15933(10) 0.0470(4) Uani 1 1 d . . . H11O H 0.4310 0.5221 0.1338 0.056 Uiso 1 1 calc R . . H11P H 0.4768 0.4355 0.1324 0.056 Uiso 1 1 calc R . . C118 C 0.51613(16) 0.47964(11) 0.23979(11) 0.0468(4) Uani 1 1 d . . . H11Q H 0.5177 0.4299 0.2657 0.056 Uiso 1 1 calc R . . H11R H 0.5989 0.4915 0.2404 0.056 Uiso 1 1 calc R . . H3A H 0.5188(16) 0.2951(12) 0.1523(11) 0.036(5) Uiso 1 1 d . . . H5A H 0.7333(19) 0.1534(11) 0.0851(11) 0.041(5) Uiso 1 1 d . . . H5B H 0.6119(19) 0.1173(13) 0.0892(12) 0.049(6) Uiso 1 1 d . . . H3B H 0.4709(19) 0.2115(13) 0.1355(12) 0.050(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.03323(9) 0.04703(11) 0.04077(10) 0.00249(7) 0.01238(7) -0.00262(7) As2 0.04678(10) 0.03279(9) 0.03752(9) 0.00033(7) 0.01114(8) -0.00366(7) As3 0.03663(9) 0.04398(10) 0.03758(9) 0.00619(7) 0.00951(7) 0.00735(7) C1 0.0413(8) 0.0414(8) 0.0261(7) 0.0021(6) 0.0060(6) -0.0043(6) C2 0.0427(8) 0.0374(8) 0.0312(7) 0.0007(6) 0.0156(7) 0.0004(6) Ru1 0.03107(6) 0.03054(6) 0.02643(6) 0.00107(4) 0.00768(4) -0.00109(4) C3 0.0540(10) 0.0395(9) 0.0295(8) 0.0019(6) 0.0146(7) 0.0000(7) C4 0.0466(9) 0.0401(8) 0.0259(7) 0.0049(6) 0.0036(6) -0.0004(7) C5 0.0427(9) 0.0384(8) 0.0343(8) 0.0060(6) 0.0055(7) 0.0053(7) C6 0.0524(10) 0.0506(10) 0.0376(9) -0.0007(8) -0.0038(8) -0.0038(8) C7 0.0406(8) 0.0329(8) 0.0408(8) -0.0004(6) 0.0140(7) -0.0054(6) C8 0.0396(8) 0.0373(8) 0.0579(10) -0.0005(8) 0.0183(8) -0.0077(7) C9 0.0516(11) 0.0573(12) 0.0917(17) -0.0085(11) 0.0390(12) -0.0053(9) C10 0.0375(9) 0.0535(11) 0.0665(12) -0.0005(9) 0.0075(8) -0.0109(8) K101 0.03259(15) 0.03372(15) 0.03072(14) 0.00020(11) 0.00780(12) 0.00117(11) N101 0.0319(6) 0.0400(7) 0.0359(7) -0.0020(6) 0.0026(5) 0.0000(5) N102 0.0328(6) 0.0445(7) 0.0361(7) 0.0081(6) 0.0094(5) 0.0020(5) O101 0.0338(5) 0.0446(6) 0.0349(5) 0.0045(5) 0.0105(4) 0.0009(5) O102 0.0346(5) 0.0409(6) 0.0377(6) 0.0088(5) 0.0092(4) 0.0016(4) O103 0.0374(6) 0.0351(6) 0.0425(6) 0.0048(5) 0.0100(5) 0.0039(4) O104 0.0379(6) 0.0368(6) 0.0442(6) 0.0003(5) 0.0107(5) -0.0019(5) O105 0.0495(7) 0.0429(6) 0.0393(6) -0.0102(5) 0.0087(5) -0.0030(5) O106 0.0497(7) 0.0469(7) 0.0391(6) -0.0004(5) 0.0199(5) 0.0033(5) C101 0.0318(8) 0.0463(9) 0.0583(11) 0.0042(8) 0.0084(7) -0.0049(7) C102 0.0375(8) 0.0519(10) 0.0502(10) 0.0121(8) 0.0184(7) 0.0050(7) C103 0.0445(8) 0.0408(8) 0.0317(7) 0.0032(6) 0.0129(6) -0.0023(7) C104 0.0424(8) 0.0394(8) 0.0329(7) 0.0076(6) 0.0068(6) -0.0013(7) C105 0.0349(8) 0.0483(9) 0.0382(8) 0.0101(7) 0.0059(6) 0.0045(7) C106 0.0314(7) 0.0551(10) 0.0395(8) 0.0101(7) 0.0038(6) -0.0017(7) C107 0.0323(7) 0.0451(9) 0.0407(8) 0.0011(7) 0.0073(6) 0.0056(6) C108 0.0384(8) 0.0430(9) 0.0414(8) 0.0029(7) 0.0060(7) 0.0081(7) C109 0.0493(10) 0.0354(8) 0.0570(11) 0.0100(8) 0.0171(8) 0.0059(7) C110 0.0514(10) 0.0335(8) 0.0564(11) -0.0001(7) 0.0179(8) -0.0021(7) C111 0.0400(8) 0.0442(9) 0.0426(9) 0.0048(7) 0.0050(7) -0.0080(7) C112 0.0357(8) 0.0499(10) 0.0461(9) 0.0099(7) 0.0122(7) -0.0039(7) C113 0.0384(9) 0.0587(11) 0.0434(9) -0.0107(8) -0.0040(7) -0.0002(8) C114 0.0482(10) 0.0544(11) 0.0509(10) -0.0170(9) 0.0044(8) -0.0077(8) C115 0.0667(12) 0.0449(10) 0.0405(9) -0.0116(8) 0.0185(8) -0.0037(9) C116 0.0689(12) 0.0554(11) 0.0376(9) -0.0103(8) 0.0231(9) -0.0035(9) C117 0.0507(10) 0.0512(10) 0.0464(9) 0.0044(8) 0.0255(8) 0.0075(8) C118 0.0392(8) 0.0543(10) 0.0507(10) 0.0100(8) 0.0194(8) 0.0112(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C2 1.9044(17) . ? As1 As2 2.3537(3) . ? As1 Ru1 2.5318(2) . ? As2 As3 2.3538(3) . ? As2 Ru1 2.5943(2) . ? As3 C1 1.9003(17) . ? As3 Ru1 2.5734(2) . ? C1 C2 1.382(2) . ? C1 Ru1 2.2324(15) . ? C1 H1 0.9500 . ? C2 Ru1 2.2855(16) . ? C2 H2 0.9500 . ? Ru1 C4 2.1407(15) . ? Ru1 C3 2.1767(17) . ? Ru1 C5 2.1849(16) . ? Ru1 C7 2.2022(15) . ? C3 C4 1.424(3) . ? C3 H3A 0.92(2) . ? C3 H3B 0.97(2) . ? C4 C5 1.424(2) . ? C4 C6 1.508(2) . ? C5 H5A 0.92(2) . ? C5 H5B 0.93(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.482(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.332(3) . ? C8 C9 1.507(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9500 . ? C10 H10B 0.9500 . ? K101 O104 2.7976(12) . ? K101 O103 2.8071(12) . ? K101 O101 2.8234(11) . ? K101 O106 2.8318(12) . ? K101 O105 2.8571(12) . ? K101 O102 2.9144(11) . ? K101 N101 2.9956(14) . ? K101 N102 2.9986(13) . ? N101 C101 1.466(2) . ? N101 C107 1.469(2) . ? N101 C113 1.473(2) . ? N102 C106 1.472(2) . ? N102 C118 1.472(2) . ? N102 C112 1.473(2) . ? O101 C102 1.4216(19) . ? O101 C103 1.4340(19) . ? O102 C105 1.421(2) . ? O102 C104 1.4229(19) . ? O103 C109 1.418(2) . ? O103 C108 1.425(2) . ? O104 C110 1.420(2) . ? O104 C111 1.421(2) . ? O105 C115 1.421(2) . ? O105 C114 1.420(2) . ? O106 C117 1.425(2) . ? O106 C116 1.427(2) . ? C101 C102 1.503(3) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? C103 C104 1.493(2) . ? C103 H10G 0.9900 . ? C103 H10H 0.9900 . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? C105 C106 1.508(2) . ? C105 H10K 0.9900 . ? C105 H10L 0.9900 . ? C106 H10M 0.9900 . ? C106 H10N 0.9900 . ? C107 C108 1.502(2) . ? C107 H10O 0.9900 . ? C107 H10P 0.9900 . ? C108 H10Q 0.9900 . ? C108 H10R 0.9900 . ? C109 C110 1.497(3) . ? C109 H10S 0.9900 . ? C109 H10T 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.505(3) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.503(3) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.485(3) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.505(3) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 As1 As2 96.75(5) . . ? C2 As1 Ru1 60.06(5) . . ? As2 As1 Ru1 64.027(7) . . ? As1 As2 As3 98.499(9) . . ? As1 As2 Ru1 61.323(7) . . ? As3 As2 Ru1 62.454(7) . . ? C1 As3 As2 94.61(5) . . ? C1 As3 Ru1 57.53(5) . . ? As2 As3 Ru1 63.356(7) . . ? C2 C1 As3 127.91(13) . . ? C2 C1 Ru1 74.30(9) . . ? As3 C1 Ru1 76.56(6) . . ? C2 C1 H1 116.0 . . ? As3 C1 H1 116.0 . . ? Ru1 C1 H1 125.0 . . ? C1 C2 As1 122.15(12) . . ? C1 C2 Ru1 70.10(9) . . ? As1 C2 Ru1 73.72(5) . . ? C1 C2 H2 118.9 . . ? As1 C2 H2 118.9 . . ? Ru1 C2 H2 129.9 . . ? C4 Ru1 C3 38.52(7) . . ? C4 Ru1 C5 38.42(7) . . ? C3 Ru1 C5 68.01(7) . . ? C4 Ru1 C7 101.17(6) . . ? C3 Ru1 C7 84.47(7) . . ? C5 Ru1 C7 82.28(7) . . ? C4 Ru1 C1 171.01(6) . . ? C3 Ru1 C1 149.97(7) . . ? C5 Ru1 C1 137.67(6) . . ? C7 Ru1 C1 84.81(6) . . ? C4 Ru1 C2 135.66(6) . . ? C3 Ru1 C2 173.37(7) . . ? C5 Ru1 C2 108.80(6) . . ? C7 Ru1 C2 101.03(6) . . ? C1 Ru1 C2 35.60(6) . . ? C4 Ru1 As1 97.11(5) . . ? C3 Ru1 As1 127.37(5) . . ? C5 Ru1 As1 93.26(5) . . ? C7 Ru1 As1 143.54(4) . . ? C1 Ru1 As1 74.32(4) . . ? C2 Ru1 As1 46.22(4) . . ? C4 Ru1 As3 138.22(5) . . ? C3 Ru1 As3 108.38(5) . . ? C5 Ru1 As3 176.36(5) . . ? C7 Ru1 As3 98.04(4) . . ? C1 Ru1 As3 45.91(4) . . ? C2 Ru1 As3 74.73(4) . . ? As1 Ru1 As3 88.617(7) . . ? C4 Ru1 As2 96.49(5) . . ? C3 Ru1 As2 95.44(5) . . ? C5 Ru1 As2 124.81(5) . . ? C7 Ru1 As2 150.80(4) . . ? C1 Ru1 As2 80.84(4) . . ? C2 Ru1 As2 81.59(4) . . ? As1 Ru1 As2 54.650(6) . . ? As3 Ru1 As2 54.190(6) . . ? C4 C3 Ru1 69.38(9) . . ? C4 C3 H3A 118.7(12) . . ? Ru1 C3 H3A 120.8(12) . . ? C4 C3 H3B 122.1(13) . . ? Ru1 C3 H3B 108.2(13) . . ? H3A C3 H3B 111.3(17) . . ? C5 C4 C3 117.83(16) . . ? C5 C4 C6 120.99(17) . . ? C3 C4 C6 121.00(17) . . ? C5 C4 Ru1 72.47(9) . . ? C3 C4 Ru1 72.11(9) . . ? C6 C4 Ru1 121.99(12) . . ? C4 C5 Ru1 69.11(9) . . ? C4 C5 H5A 114.8(13) . . ? Ru1 C5 H5A 119.0(13) . . ? C4 C5 H5B 121.3(13) . . ? Ru1 C5 H5B 106.1(13) . . ? H5A C5 H5B 117.0(18) . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 Ru1 117.78(11) . . ? C8 C7 H7A 107.9 . . ? Ru1 C7 H7A 107.9 . . ? C8 C7 H7B 107.9 . . ? Ru1 C7 H7B 107.9 . . ? H7A C7 H7B 107.2 . . ? C10 C8 C7 123.62(18) . . ? C10 C8 C9 120.24(19) . . ? C7 C8 C9 116.13(17) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 120.0 . . ? C8 C10 H10B 120.0 . . ? H10A C10 H10B 120.0 . . ? O104 K101 O103 59.76(3) . . ? O104 K101 O101 135.26(4) . . ? O103 K101 O101 98.09(3) . . ? O104 K101 O106 100.03(4) . . ? O103 K101 O106 137.58(4) . . ? O101 K101 O106 118.86(4) . . ? O104 K101 O105 120.41(4) . . ? O103 K101 O105 96.24(4) . . ? O101 K101 O105 98.85(4) . . ? O106 K101 O105 60.17(4) . . ? O104 K101 O102 96.00(3) . . ? O103 K101 O102 119.25(3) . . ? O101 K101 O102 59.28(3) . . ? O106 K101 O102 98.38(4) . . ? O105 K101 O102 139.22(4) . . ? O104 K101 N101 119.77(4) . . ? O103 K101 N101 60.53(4) . . ? O101 K101 N101 60.94(4) . . ? O106 K101 N101 118.70(4) . . ? O105 K101 N101 59.79(4) . . ? O102 K101 N101 119.30(4) . . ? O104 K101 N102 61.02(4) . . ? O103 K101 N102 120.20(4) . . ? O101 K101 N102 118.28(3) . . ? O106 K101 N102 61.18(4) . . ? O105 K101 N102 120.28(4) . . ? O102 K101 N102 60.01(3) . . ? N101 K101 N102 179.12(4) . . ? C101 N101 C107 110.01(14) . . ? C101 N101 C113 109.94(15) . . ? C107 N101 C113 109.69(13) . . ? C101 N101 K101 108.10(9) . . ? C107 N101 K101 108.48(9) . . ? C113 N101 K101 110.59(10) . . ? C106 N102 C118 109.75(14) . . ? C106 N102 C112 110.20(14) . . ? C118 N102 C112 109.73(13) . . ? C106 N102 K101 110.53(9) . . ? C118 N102 K101 108.64(10) . . ? C112 N102 K101 107.95(9) . . ? C102 O101 C103 110.84(12) . . ? C102 O101 K101 117.47(9) . . ? C103 O101 K101 115.99(9) . . ? C105 O102 C104 111.07(12) . . ? C105 O102 K101 114.21(9) . . ? C104 O102 K101 112.52(9) . . ? C109 O103 C108 111.89(13) . . ? C109 O103 K101 115.68(10) . . ? C108 O103 K101 119.25(10) . . ? C110 O104 C111 111.79(14) . . ? C110 O104 K101 116.51(10) . . ? C111 O104 K101 118.12(10) . . ? C115 O105 C114 111.50(14) . . ? C115 O105 K101 114.16(10) . . ? C114 O105 K101 118.28(10) . . ? C117 O106 C116 109.44(13) . . ? C117 O106 K101 114.87(10) . . ? C116 O106 K101 113.36(10) . . ? N101 C101 C102 114.28(14) . . ? N101 C101 H10C 108.7 . . ? C102 C101 H10C 108.7 . . ? N101 C101 H10D 108.7 . . ? C102 C101 H10D 108.7 . . ? H10C C101 H10D 107.6 . . ? O101 C102 C101 109.70(14) . . ? O101 C102 H10E 109.7 . . ? C101 C102 H10E 109.7 . . ? O101 C102 H10F 109.7 . . ? C101 C102 H10F 109.7 . . ? H10E C102 H10F 108.2 . . ? O101 C103 C104 108.01(13) . . ? O101 C103 H10G 110.1 . . ? C104 C103 H10G 110.1 . . ? O101 C103 H10H 110.1 . . ? C104 C103 H10H 110.1 . . ? H10G C103 H10H 108.4 . . ? O102 C104 C103 109.08(13) . . ? O102 C104 H10I 109.9 . . ? C103 C104 H10I 109.9 . . ? O102 C104 H10J 109.9 . . ? C103 C104 H10J 109.9 . . ? H10I C104 H10J 108.3 . . ? O102 C105 C106 108.77(14) . . ? O102 C105 H10K 109.9 . . ? C106 C105 H10K 109.9 . . ? O102 C105 H10L 109.9 . . ? C106 C105 H10L 109.9 . . ? H10K C105 H10L 108.3 . . ? N102 C106 C105 113.51(14) . . ? N102 C106 H10M 108.9 . . ? C105 C106 H10M 108.9 . . ? N102 C106 H10N 108.9 . . ? C105 C106 H10N 108.9 . . ? H10M C106 H10N 107.7 . . ? N101 C107 C108 114.25(14) . . ? N101 C107 H10O 108.7 . . ? C108 C107 H10O 108.7 . . ? N101 C107 H10P 108.7 . . ? C108 C107 H10P 108.7 . . ? H10O C107 H10P 107.6 . . ? O103 C108 C107 109.14(13) . . ? O103 C108 H10Q 109.9 . . ? C107 C108 H10Q 109.9 . . ? O103 C108 H10R 109.9 . . ? C107 C108 H10R 109.9 . . ? H10Q C108 H10R 108.3 . . ? O103 C109 C110 109.09(14) . . ? O103 C109 H10S 109.9 . . ? C110 C109 H10S 109.9 . . ? O103 C109 H10T 109.9 . . ? C110 C109 H10T 109.9 . . ? H10S C109 H10T 108.3 . . ? O104 C110 C109 109.13(15) . . ? O104 C110 H11A 109.9 . . ? C109 C110 H11A 109.9 . . ? O104 C110 H11B 109.9 . . ? C109 C110 H11B 109.9 . . ? H11A C110 H11B 108.3 . . ? O104 C111 C112 109.34(14) . . ? O104 C111 H11C 109.8 . . ? C112 C111 H11C 109.8 . . ? O104 C111 H11D 109.8 . . ? C112 C111 H11D 109.8 . . ? H11C C111 H11D 108.3 . . ? N102 C112 C111 114.20(14) . . ? N102 C112 H11E 108.7 . . ? C111 C112 H11E 108.7 . . ? N102 C112 H11F 108.7 . . ? C111 C112 H11F 108.7 . . ? H11E C112 H11F 107.6 . . ? N101 C113 C114 113.64(15) . . ? N101 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? N101 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? O105 C114 C113 109.43(16) . . ? O105 C114 H11I 109.8 . . ? C113 C114 H11I 109.8 . . ? O105 C114 H11J 109.8 . . ? C113 C114 H11J 109.8 . . ? H11I C114 H11J 108.2 . . ? O105 C115 C116 109.64(15) . . ? O105 C115 H11K 109.7 . . ? C116 C115 H11K 109.7 . . ? O105 C115 H11L 109.7 . . ? C116 C115 H11L 109.7 . . ? H11K C115 H11L 108.2 . . ? O106 C116 C115 109.76(15) . . ? O106 C116 H11M 109.7 . . ? C115 C116 H11M 109.7 . . ? O106 C116 H11N 109.7 . . ? C115 C116 H11N 109.7 . . ? H11M C116 H11N 108.2 . . ? O106 C117 C118 109.57(14) . . ? O106 C117 H11O 109.8 . . ? C118 C117 H11O 109.8 . . ? O106 C117 H11P 109.8 . . ? C118 C117 H11P 109.8 . . ? H11O C117 H11P 108.2 . . ? N102 C118 C117 113.72(14) . . ? N102 C118 H11Q 108.8 . . ? C117 C118 H11Q 108.8 . . ? N102 C118 H11R 108.8 . . ? C117 C118 H11R 108.8 . . ? H11Q C118 H11R 107.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 76.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.629 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.047 _iucr_refine_instructions_details ; TITL 3 in P2(1)/n CELL 1.54178 11.7391 17.4228 18.6466 90.000 107.681 90.000 ZERR 4.00 0.0001 0.0001 0.0001 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O K AS RU UNIT 112 208 8 24 4 12 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.080 0.160 0.260 ACTA BOND $H L.S. 4 TEMP -123.00 WGHT 0.028100 1.197100 FVAR 0.06755 AS1 6 0.702955 0.297795 -0.031725 11.00000 0.03323 0.04703 = 0.04077 0.00249 0.01238 -0.00262 AS2 6 0.587541 0.388823 0.008707 11.00000 0.04678 0.03279 = 0.03752 0.00033 0.01114 -0.00366 AS3 6 0.396552 0.346110 -0.062709 11.00000 0.03663 0.04398 = 0.03758 0.00619 0.00951 0.00735 C1 1 0.454970 0.262635 -0.106988 11.00000 0.04135 0.04141 = 0.02608 0.00212 0.00605 -0.00431 AFIX 43 H1 2 0.396140 0.230215 -0.139042 11.00000 -1.20000 AFIX 0 C2 1 0.572612 0.243345 -0.098241 11.00000 0.04266 0.03739 = 0.03123 0.00075 0.01560 0.00039 AFIX 43 H2 2 0.588995 0.201557 -0.126326 11.00000 -1.20000 AFIX 0 RU1 7 0.539225 0.244307 0.016293 11.00000 0.03107 0.03054 = 0.02643 0.00107 0.00768 -0.00109 C3 1 0.529014 0.249039 0.130828 11.00000 0.05402 0.03953 = 0.02951 0.00186 0.01460 0.00001 C4 1 0.646127 0.227790 0.130704 11.00000 0.04662 0.04012 = 0.02594 0.00489 0.00359 -0.00045 C5 1 0.658187 0.160922 0.089709 11.00000 0.04266 0.03837 = 0.03425 0.00599 0.00550 0.00534 C6 1 0.752524 0.277932 0.167529 11.00000 0.05238 0.05062 = 0.03756 -0.00070 -0.00384 -0.00381 AFIX 137 H6A 2 0.789097 0.261310 0.219685 11.00000 -1.50000 H6B 2 0.726463 0.331428 0.166941 11.00000 -1.50000 H6C 2 0.811160 0.273646 0.139893 11.00000 -1.50000 AFIX 0 C7 1 0.409479 0.149919 0.002150 11.00000 0.04061 0.03287 = 0.04076 -0.00043 0.01402 -0.00542 AFIX 23 H7A 2 0.431525 0.109567 -0.028598 11.00000 -1.20000 H7B 2 0.418854 0.127544 0.052420 11.00000 -1.20000 AFIX 0 C8 1 0.281248 0.168133 -0.032801 11.00000 0.03957 0.03726 = 0.05791 -0.00053 0.01828 -0.00766 C9 1 0.218856 0.205829 0.017615 11.00000 0.05159 0.05733 = 0.09171 -0.00848 0.03896 -0.00526 AFIX 137 H9A 2 0.136858 0.219052 -0.011864 11.00000 -1.50000 H9B 2 0.262014 0.252578 0.039432 11.00000 -1.50000 H9C 2 0.217112 0.170376 0.058071 11.00000 -1.50000 AFIX 0 C10 1 0.221023 0.151875 -0.104039 11.00000 0.03746 0.05351 = 0.06646 -0.00046 0.00747 -0.01094 AFIX 93 H10A 2 0.260314 0.127255 -0.135398 11.00000 -1.20000 H10B 2 0.138777 0.164900 -0.123489 11.00000 -1.20000 AFIX 0 K101 5 0.208618 0.529637 0.244222 11.00000 0.03259 0.03372 = 0.03072 0.00020 0.00780 0.00117 N101 3 -0.057421 0.517378 0.207984 11.00000 0.03194 0.04002 = 0.03592 -0.00201 0.00263 -0.00002 N102 3 0.475330 0.539672 0.281846 11.00000 0.03285 0.04449 = 0.03608 0.00805 0.00938 0.00204 O101 4 0.112166 0.451156 0.344954 11.00000 0.03380 0.04460 = 0.03493 0.00446 0.01047 0.00095 O102 4 0.360336 0.485276 0.393353 11.00000 0.03461 0.04091 = 0.03775 0.00878 0.00923 0.00158 O103 4 0.070862 0.663879 0.228043 11.00000 0.03735 0.03506 = 0.04253 0.00482 0.00996 0.00393 O104 4 0.314231 0.673264 0.242332 11.00000 0.03785 0.03684 = 0.04418 0.00029 0.01072 -0.00190 O105 4 0.070143 0.459288 0.107026 11.00000 0.04952 0.04293 = 0.03925 -0.01024 0.00867 -0.00301 O106 4 0.323980 0.443860 0.157416 11.00000 0.04966 0.04689 = 0.03909 -0.00043 0.01991 0.00332 C101 1 -0.083618 0.457921 0.256359 11.00000 0.03184 0.04629 = 0.05827 0.00417 0.00845 -0.00490 AFIX 23 H10C 2 -0.069583 0.406991 0.237056 11.00000 -1.20000 H10D 2 -0.169345 0.460988 0.252872 11.00000 -1.20000 AFIX 0 C102 1 -0.010476 0.463743 0.337720 11.00000 0.03747 0.05192 = 0.05022 0.01209 0.01839 0.00496 AFIX 23 H10E 2 -0.020697 0.515261 0.357308 11.00000 -1.20000 H10F 2 -0.038155 0.425056 0.367593 11.00000 -1.20000 AFIX 0 C103 1 0.183189 0.452063 0.422555 11.00000 0.04453 0.04083 = 0.03167 0.00320 0.01285 -0.00231 AFIX 23 H10G 2 0.149072 0.416473 0.452007 11.00000 -1.20000 H10H 2 0.184390 0.504341 0.443577 11.00000 -1.20000 AFIX 0 C104 1 0.307057 0.427707 0.426847 11.00000 0.04240 0.03945 = 0.03292 0.00757 0.00677 -0.00125 AFIX 23 H10I 2 0.355101 0.420272 0.480080 11.00000 -1.20000 H10J 2 0.304492 0.378399 0.400015 11.00000 -1.20000 AFIX 0 C105 1 0.478696 0.464525 0.396180 11.00000 0.03486 0.04834 = 0.03823 0.01009 0.00586 0.00446 AFIX 23 H10K 2 0.477398 0.416770 0.367170 11.00000 -1.20000 H10L 2 0.527367 0.455239 0.448975 11.00000 -1.20000 AFIX 0 C106 1 0.532510 0.528916 0.363147 11.00000 0.03137 0.05508 = 0.03948 0.01009 0.00376 -0.00166 AFIX 23 H10M 2 0.525817 0.577229 0.389526 11.00000 -1.20000 H10N 2 0.618605 0.518308 0.372278 11.00000 -1.20000 AFIX 0 C107 1 -0.103927 0.591773 0.223520 11.00000 0.03229 0.04509 = 0.04074 0.00113 0.00733 0.00564 AFIX 23 H10O 2 -0.084957 0.597918 0.278688 11.00000 -1.20000 H10P 2 -0.192070 0.591536 0.201810 11.00000 -1.20000 AFIX 0 C108 1 -0.054998 0.659598 0.192741 11.00000 0.03838 0.04300 = 0.04141 0.00289 0.00596 0.00812 AFIX 23 H10Q 2 -0.072114 0.654081 0.137633 11.00000 -1.20000 H10R 2 -0.093641 0.707283 0.202568 11.00000 -1.20000 AFIX 0 C109 1 0.121188 0.730284 0.205655 11.00000 0.04930 0.03542 = 0.05703 0.01002 0.01707 0.00594 AFIX 23 H10S 2 0.075225 0.776304 0.211350 11.00000 -1.20000 H10T 2 0.117613 0.725866 0.152082 11.00000 -1.20000 AFIX 0 C110 1 0.248449 0.738080 0.253699 11.00000 0.05137 0.03350 = 0.05644 -0.00011 0.01794 -0.00211 AFIX 23 H11A 2 0.283480 0.785557 0.240164 11.00000 -1.20000 H11B 2 0.252132 0.741478 0.307355 11.00000 -1.20000 AFIX 0 C111 1 0.438447 0.681113 0.280361 11.00000 0.04005 0.04421 = 0.04261 0.00483 0.00503 -0.00796 AFIX 23 H11C 2 0.452465 0.680574 0.335462 11.00000 -1.20000 H11D 2 0.467671 0.730652 0.266740 11.00000 -1.20000 AFIX 0 C112 1 0.505127 0.615915 0.258409 11.00000 0.03571 0.04991 = 0.04612 0.00995 0.01215 -0.00389 AFIX 23 H11E 2 0.487691 0.616153 0.203023 11.00000 -1.20000 H11F 2 0.591999 0.624747 0.280982 11.00000 -1.20000 AFIX 0 C113 1 -0.112354 0.496976 0.128260 11.00000 0.03844 0.05865 = 0.04338 -0.01070 -0.00397 -0.00020 AFIX 23 H11G 2 -0.114822 0.543257 0.097021 11.00000 -1.20000 H11H 2 -0.195831 0.480432 0.120828 11.00000 -1.20000 AFIX 0 C114 1 -0.047379 0.434292 0.101384 11.00000 0.04817 0.05437 = 0.05090 -0.01700 0.00435 -0.00771 AFIX 23 H11I 2 -0.043640 0.387677 0.132376 11.00000 -1.20000 H11J 2 -0.090825 0.421324 0.048434 11.00000 -1.20000 AFIX 0 C115 1 0.133202 0.403308 0.078616 11.00000 0.06667 0.04492 = 0.04053 -0.01158 0.01853 -0.00372 AFIX 23 H11K 2 0.087285 0.390232 0.026121 11.00000 -1.20000 H11L 2 0.142942 0.356003 0.109306 11.00000 -1.20000 AFIX 0 C116 1 0.252449 0.433800 0.081061 11.00000 0.06892 0.05541 = 0.03757 -0.01032 0.02314 -0.00345 AFIX 23 H11M 2 0.292390 0.397623 0.055498 11.00000 -1.20000 H11N 2 0.242964 0.483585 0.054296 11.00000 -1.20000 AFIX 0 C117 1 0.439021 0.471649 0.159333 11.00000 0.05073 0.05122 = 0.04637 0.00437 0.02548 0.00752 AFIX 23 H11O 2 0.430959 0.522074 0.133800 11.00000 -1.20000 H11P 2 0.476776 0.435508 0.132411 11.00000 -1.20000 AFIX 0 C118 1 0.516133 0.479643 0.239794 11.00000 0.03916 0.05427 = 0.05074 0.01000 0.01936 0.01123 AFIX 23 H11Q 2 0.517715 0.429900 0.265742 11.00000 -1.20000 H11R 2 0.598924 0.491481 0.240446 11.00000 -1.20000 AFIX 0 H3A 2 0.518778 0.295148 0.152278 11.00000 0.03571 H5A 2 0.733257 0.153419 0.085132 11.00000 0.04130 H5B 2 0.611946 0.117271 0.089195 11.00000 0.04880 H3B 2 0.470928 0.211457 0.135487 11.00000 0.05043 HKLF 4 REM p21n in P2(1)/n REM R1 = 0.0180 for 7422 Fo > 4sig(Fo) and 0.0185 for all 7613 data REM 388 parameters refined using 0 restraints END WGHT 0.0277 1.2167 REM Highest difference peak 0.629, deepest hole -0.462, 1-sigma level 0.047 Q1 1 0.4927 0.2779 0.0248 11.00000 0.05 0.63 Q2 1 0.6325 0.2593 -0.0001 11.00000 0.05 0.32 Q3 1 0.6438 0.3515 -0.0125 11.00000 0.05 0.32 Q4 1 0.5211 0.2560 -0.1039 11.00000 0.05 0.28 Q5 1 0.4300 0.2991 -0.0976 11.00000 0.05 0.27 Q6 1 0.6208 0.2633 -0.0760 11.00000 0.05 0.27 Q7 1 0.6147 0.2259 0.0039 11.00000 0.05 0.26 Q8 1 0.7849 0.2865 -0.0483 11.00000 0.05 0.25 Q9 1 0.5027 0.4990 0.3804 11.00000 0.05 0.24 Q10 1 0.7163 0.2013 0.0808 11.00000 0.05 0.23 Q11 1 0.4831 0.3815 -0.0518 11.00000 0.05 0.23 Q12 1 -0.0826 0.4650 0.1202 11.00000 0.05 0.23 Q13 1 -0.0810 0.6213 0.2060 11.00000 0.05 0.22 Q14 1 0.6640 0.3044 0.1351 11.00000 0.05 0.21 Q15 1 0.4549 0.1997 0.0091 11.00000 0.05 0.21 Q16 1 0.4173 0.4759 0.3940 11.00000 0.05 0.20 Q17 1 0.5959 0.2430 0.1254 11.00000 0.05 0.20 Q18 1 0.3192 0.3548 -0.0490 11.00000 0.05 0.20 Q19 1 0.0792 0.5042 0.0986 11.00000 0.05 0.19 Q20 1 0.2428 0.4415 0.4222 11.00000 0.05 0.19 ;