data_10 _audit_creation_date 2014-12-02 _audit_creation_method 'by CrystalStructure 4.1' _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2014). CrystalStructure. Version 4.1. Rigaku Corporation, Tokyo, Japan. Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Mallamo, M., Mazzone, A., Polidori, G. and Spagna, R. (2012). J. Appl. Cryst. 45, 357-361. SIR2011 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan. ; _chemical_formula_sum 'C21 H20 As P' _chemical_formula_moiety 'C21 H20 As P' _chemical_formula_weight 378.28 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' #------------------------------------------------------------------------------ _cell_length_a 8.1289(17) _cell_length_b 11.214(2) _cell_length_c 20.239(5) _cell_angle_alpha 84.892(11) _cell_angle_beta 83.6167(10) _cell_angle_gamma 70.879(8) _cell_volume 1729.6(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5220 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.60 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776.00 _exptl_absorpt_coefficient_mu 2.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.940 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.814 _diffrn_reflns_number 24148 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_theta_max 25.404 _diffrn_reflns_theta_min 1.925 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6291 _reflns_number_gt 5185 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0645 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6291 _refine_ls_number_parameters 419 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0217P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.76 _refine_diff_density_min -0.55 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'As' 'As' 0.0499 2.0058 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.1023 0.0942 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.06729(3) 0.28848(2) 0.33200(2) 0.01455(7) Uani 1 1 d . . . . . As31 As 0.10438(3) 0.72643(2) 0.15867(2) 0.01560(7) Uani 1 1 d . . . . . P9 P -0.17570(8) 0.24798(6) 0.39592(3) 0.01568(13) Uani 1 1 d . . . . . P39 P 0.09782(8) 0.59718(6) 0.07209(3) 0.01501(13) Uani 1 1 d . . . . . C1 C 0.1454(3) 0.3262(2) 0.41337(11) 0.0145(5) Uani 1 1 d . . . . . C2 C 0.2868(3) 0.3670(2) 0.41602(12) 0.0173(5) Uani 1 1 d . . . . . H2 H 0.3535 0.3782 0.3758 0.021 Uiso 1 1 calc R U . . . C3 C 0.3363(3) 0.3929(2) 0.47715(12) 0.0181(5) Uani 1 1 d . . . . . H3 H 0.4346 0.4207 0.4775 0.022 Uiso 1 1 calc R U . . . C4 C 0.2401(3) 0.3771(2) 0.53558(11) 0.0148(5) Uani 1 1 d . . . . . C5 C 0.0959(3) 0.3342(2) 0.53275(12) 0.0143(5) Uani 1 1 d . . . . . C6 C 0.0107(3) 0.3185(2) 0.59578(12) 0.0161(5) Uani 1 1 d . . . . . C7 C -0.1316(3) 0.2769(2) 0.59871(12) 0.0180(5) Uani 1 1 d . . . . . H7 H -0.1911 0.2638 0.6404 0.022 Uiso 1 1 calc R U . . . C8 C -0.1890(3) 0.2535(2) 0.53854(12) 0.0178(5) Uani 1 1 d . . . . . H8 H -0.2908 0.2288 0.5410 0.021 Uiso 1 1 calc R U . . . C9 C -0.1023(3) 0.2653(2) 0.47645(11) 0.0148(5) Uani 1 1 d . . . . . C10 C 0.0451(3) 0.3082(2) 0.47345(11) 0.0138(5) Uani 1 1 d . . . . . C11 C 0.2522(3) 0.3977(2) 0.60753(11) 0.0175(5) Uani 1 1 d . . . . . H11A H 0.2317 0.4881 0.6138 0.021 Uiso 1 1 calc R U . . . H11B H 0.3688 0.3478 0.6218 0.021 Uiso 1 1 calc R U . . . C12 C 0.1060(3) 0.3520(2) 0.64817(12) 0.0190(5) Uani 1 1 d . . . . . H12A H 0.1579 0.2772 0.6780 0.023 Uiso 1 1 calc R U . . . H12B H 0.0254 0.4200 0.6753 0.023 Uiso 1 1 calc R U . . . C13 C 0.2334(3) 0.1181(2) 0.32098(11) 0.0150(5) Uani 1 1 d . . . . . C14 C 0.2520(3) 0.0674(2) 0.25913(12) 0.0178(5) Uani 1 1 d . . . . . H14 H 0.1865 0.1161 0.2244 0.021 Uiso 1 1 calc R U . . . C15 C 0.3647(3) -0.0529(2) 0.24771(12) 0.0194(5) Uani 1 1 d . . . . . H15 H 0.3747 -0.0867 0.2055 0.023 Uiso 1 1 calc R U . . . C16 C 0.4630(3) -0.1242(2) 0.29763(12) 0.0181(5) Uani 1 1 d . . . . . H16 H 0.5399 -0.2071 0.2899 0.022 Uiso 1 1 calc R U . . . C17 C 0.4486(3) -0.0741(2) 0.35907(12) 0.0182(5) Uani 1 1 d . . . . . H17 H 0.5172 -0.1225 0.3932 0.022 Uiso 1 1 calc R U . . . C18 C 0.3346(3) 0.0461(2) 0.37102(11) 0.0161(5) Uani 1 1 d . . . . . H18 H 0.3253 0.0797 0.4133 0.019 Uiso 1 1 calc R U . . . C19 C -0.1302(3) 0.0746(2) 0.39026(12) 0.0181(5) Uani 1 1 d . . . . . H19 H -0.0026 0.0299 0.3935 0.022 Uiso 1 1 calc R U . . . C20 C -0.2343(3) 0.0244(2) 0.44687(12) 0.0217(5) Uani 1 1 d . . . . . H20A H -0.1920 0.0309 0.4895 0.026 Uiso 1 1 calc R U . . . H20B H -0.2195 -0.0643 0.4406 0.026 Uiso 1 1 calc R U . . . H20C H -0.3584 0.0743 0.4469 0.026 Uiso 1 1 calc R U . . . C21 C -0.1796(3) 0.0550(3) 0.32169(13) 0.0259(6) Uani 1 1 d . . . . . H21A H -0.3047 0.0982 0.3185 0.031 Uiso 1 1 calc R U . . . H21B H -0.1530 -0.0356 0.3164 0.031 Uiso 1 1 calc R U . . . H21C H -0.1124 0.0898 0.2866 0.031 Uiso 1 1 calc R U . . . C31 C 0.1516(3) 0.8489(2) 0.09041(12) 0.0158(5) Uani 1 1 d . . . . . C32 C 0.1552(3) 0.9680(2) 0.10197(13) 0.0205(5) Uani 1 1 d . . . . . H32 H 0.1239 0.9970 0.1457 0.025 Uiso 1 1 calc R U . . . C33 C 0.2039(3) 1.0478(2) 0.05076(14) 0.0245(6) Uani 1 1 d . . . . . H33 H 0.2069 1.1284 0.0605 0.029 Uiso 1 1 calc R U . . . C34 C 0.2467(3) 1.0079(2) -0.01314(13) 0.0215(6) Uani 1 1 d . . . . . C35 C 0.2342(3) 0.8894(2) -0.02555(12) 0.0172(5) Uani 1 1 d . . . . . C36 C 0.2701(3) 0.8616(2) -0.09330(12) 0.0208(5) Uani 1 1 d . . . . . C37 C 0.2563(3) 0.7503(2) -0.11096(12) 0.0224(6) Uani 1 1 d . . . . . H37 H 0.2784 0.7290 -0.1562 0.027 Uiso 1 1 calc R U . . . C38 C 0.2088(3) 0.6671(2) -0.06140(12) 0.0190(5) Uani 1 1 d . . . . . H38 H 0.1972 0.5913 -0.0747 0.023 Uiso 1 1 calc R U . . . C39 C 0.1786(3) 0.6916(2) 0.00577(11) 0.0151(5) Uani 1 1 d . . . . . C40 C 0.1893(3) 0.8081(2) 0.02447(12) 0.0145(5) Uani 1 1 d . . . . . C41 C 0.3050(3) 1.0653(3) -0.07857(14) 0.0280(6) Uani 1 1 d . . . . . H41A H 0.4210 1.0750 -0.0764 0.034 Uiso 1 1 calc R U . . . H41B H 0.2201 1.1493 -0.0891 0.034 Uiso 1 1 calc R U . . . C42 C 0.3141(3) 0.9712(3) -0.13213(14) 0.0305(7) Uani 1 1 d . . . . . H42A H 0.2285 1.0114 -0.1652 0.037 Uiso 1 1 calc R U . . . H42B H 0.4326 0.9420 -0.1556 0.037 Uiso 1 1 calc R U . . . C43 C 0.3449(3) 0.6464(2) 0.18466(11) 0.0149(5) Uani 1 1 d . . . . . C44 C 0.3692(3) 0.5656(2) 0.24151(12) 0.0186(5) Uani 1 1 d . . . . . H44 H 0.2711 0.5507 0.2665 0.022 Uiso 1 1 calc R U . . . C45 C 0.5362(3) 0.5060(2) 0.26226(12) 0.0211(5) Uani 1 1 d . . . . . H45 H 0.5517 0.4500 0.3008 0.025 Uiso 1 1 calc R U . . . C46 C 0.6794(3) 0.5290(2) 0.22636(12) 0.0188(5) Uani 1 1 d . . . . . H46 H 0.7933 0.4887 0.2403 0.023 Uiso 1 1 calc R U . . . C47 C 0.6558(3) 0.6106(2) 0.17022(12) 0.0170(5) Uani 1 1 d . . . . . H47 H 0.7537 0.6270 0.1459 0.020 Uiso 1 1 calc R U . . . C48 C 0.4892(3) 0.6690(2) 0.14918(11) 0.0156(5) Uani 1 1 d . . . . . H48 H 0.4743 0.7245 0.1104 0.019 Uiso 1 1 calc R U . . . C49 C 0.2848(3) 0.4493(2) 0.08586(11) 0.0165(5) Uani 1 1 d . . . . . H49 H 0.3864 0.4717 0.0981 0.020 Uiso 1 1 calc R U . . . C50 C 0.3380(3) 0.3760(2) 0.02228(12) 0.0215(5) Uani 1 1 d . . . . . H50A H 0.2354 0.3622 0.0074 0.026 Uiso 1 1 calc R U . . . H50B H 0.4267 0.2943 0.0314 0.026 Uiso 1 1 calc R U . . . H50C H 0.3862 0.4248 -0.0126 0.026 Uiso 1 1 calc R U . . . C51 C 0.2250(3) 0.3712(2) 0.14360(13) 0.0238(6) Uani 1 1 d . . . . . H51A H 0.3235 0.2966 0.1549 0.029 Uiso 1 1 calc R U . . . H51B H 0.1307 0.3442 0.1305 0.029 Uiso 1 1 calc R U . . . H51C H 0.1824 0.4226 0.1824 0.029 Uiso 1 1 calc R U . . . 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 0.01572(13) 0.01402(14) 0.01298(12) 0.00011(10) -0.00192(9) -0.00352(10) As31 0.01017(12) 0.02004(15) 0.01390(13) -0.00176(10) -0.00087(9) -0.00104(10) P9 0.0139(3) 0.0164(3) 0.0172(3) -0.0006(3) -0.0028(2) -0.0049(3) P39 0.0117(3) 0.0170(3) 0.0155(3) -0.0001(2) -0.0012(2) -0.0037(2) C1 0.0158(12) 0.0117(12) 0.0151(12) -0.0014(9) -0.0013(9) -0.0028(10) C2 0.0170(12) 0.0166(13) 0.0175(12) 0.0004(10) 0.0025(10) -0.0057(10) C3 0.0139(12) 0.0165(13) 0.0254(13) -0.0021(10) -0.0026(10) -0.0064(10) C4 0.0148(12) 0.0093(12) 0.0181(12) -0.0004(10) -0.0045(9) 0.0001(9) C5 0.0133(11) 0.0090(12) 0.0187(12) -0.0013(9) -0.0011(9) -0.0008(9) C6 0.0184(12) 0.0104(12) 0.0174(12) -0.0020(10) -0.0006(10) -0.0017(10) C7 0.0193(12) 0.0170(13) 0.0156(12) -0.0016(10) 0.0039(10) -0.0045(10) C8 0.0140(12) 0.0158(13) 0.0238(13) -0.0006(10) -0.0002(10) -0.0057(10) C9 0.0139(11) 0.0114(12) 0.0187(12) -0.0025(10) -0.0018(9) -0.0028(9) C10 0.0130(11) 0.0080(12) 0.0185(12) -0.0017(9) -0.0013(9) -0.0003(9) C11 0.0173(12) 0.0151(13) 0.0200(13) -0.0019(10) -0.0058(10) -0.0032(10) C12 0.0208(13) 0.0190(14) 0.0153(12) -0.0015(10) -0.0022(10) -0.0036(11) C13 0.0132(11) 0.0137(13) 0.0184(12) -0.0011(10) 0.0003(9) -0.0051(10) C14 0.0177(12) 0.0206(14) 0.0148(12) 0.0019(10) -0.0041(10) -0.0055(10) C15 0.0197(13) 0.0211(14) 0.0182(12) -0.0046(10) -0.0001(10) -0.0071(11) C16 0.0145(12) 0.0145(13) 0.0241(13) -0.0026(10) -0.0002(10) -0.0032(10) C17 0.0148(12) 0.0190(14) 0.0202(12) 0.0044(10) -0.0045(10) -0.0049(10) C18 0.0164(12) 0.0207(14) 0.0129(11) -0.0022(10) -0.0005(9) -0.0081(10) C19 0.0176(12) 0.0159(13) 0.0217(13) -0.0026(10) -0.0016(10) -0.0061(10) C20 0.0242(13) 0.0181(14) 0.0253(14) 0.0004(11) -0.0032(11) -0.0105(11) C21 0.0298(15) 0.0282(16) 0.0252(14) -0.0066(12) -0.0009(11) -0.0162(12) C31 0.0081(11) 0.0177(13) 0.0194(12) -0.0010(10) -0.0048(9) 0.0000(9) C32 0.0156(12) 0.0190(14) 0.0253(14) -0.0036(11) -0.0091(10) -0.0006(10) C33 0.0171(13) 0.0142(14) 0.0422(16) -0.0007(12) -0.0139(12) -0.0017(10) C34 0.0083(11) 0.0171(14) 0.0375(15) 0.0066(11) -0.0082(10) -0.0018(10) C35 0.0077(11) 0.0160(13) 0.0244(13) 0.0035(10) -0.0037(9) 0.0003(10) C36 0.0101(11) 0.0220(15) 0.0231(13) 0.0069(11) 0.0008(10) 0.0017(10) C37 0.0178(12) 0.0267(15) 0.0148(12) 0.0018(11) 0.0008(10) 0.0022(11) C38 0.0166(12) 0.0181(14) 0.0195(12) -0.0015(10) -0.0041(10) -0.0011(10) C39 0.0094(11) 0.0154(13) 0.0183(12) 0.0013(10) -0.0028(9) -0.0010(9) C40 0.0066(10) 0.0150(13) 0.0193(12) 0.0012(10) -0.0039(9) 0.0002(9) C41 0.0142(13) 0.0228(15) 0.0443(17) 0.0135(13) -0.0072(12) -0.0047(11) C42 0.0216(14) 0.0283(17) 0.0330(16) 0.0131(13) 0.0043(12) -0.0025(12) C43 0.0126(11) 0.0164(13) 0.0144(11) -0.0035(10) -0.0024(9) -0.0019(10) C44 0.0148(12) 0.0239(15) 0.0176(12) -0.0007(10) 0.0006(10) -0.0075(11) C45 0.0210(13) 0.0250(15) 0.0162(12) 0.0043(11) -0.0067(10) -0.0057(11) C46 0.0138(12) 0.0208(14) 0.0202(13) -0.0037(10) -0.0056(10) -0.0016(10) C47 0.0126(11) 0.0190(14) 0.0196(12) -0.0032(10) -0.0007(9) -0.0052(10) C48 0.0167(12) 0.0164(13) 0.0134(11) -0.0006(10) -0.0016(9) -0.0047(10) C49 0.0138(11) 0.0164(13) 0.0183(12) 0.0011(10) -0.0027(10) -0.0034(10) C50 0.0190(13) 0.0183(14) 0.0244(13) -0.0015(11) -0.0045(10) -0.0012(11) C51 0.0255(14) 0.0183(14) 0.0272(14) 0.0041(11) -0.0027(11) -0.0075(11) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)' _computing_cell_refinement 'CrystalClear-SM Expert 2.1 b32' _computing_data_reduction 'CrystalClear-SM Expert 2.1 b32' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _computing_structure_refinement 'SHELXL2013 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.1 (Rigaku, 2014)' _computing_molecular_graphics 'CrystalStructure 4.1' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 1.956(2) . ? As1 C13 1.960(2) . ? As1 P9 2.3867(7) . ? As31 C31 1.957(2) . ? As31 C43 1.974(2) . ? As31 P39 2.3871(8) . ? P9 C9 1.844(2) . ? P9 C19 1.868(2) . ? P39 C39 1.833(2) . ? P39 C49 1.871(2) . ? C1 C2 1.377(3) . ? C1 C10 1.424(3) . ? C2 C3 1.424(3) . ? C2 H2 0.9500 . ? C3 C4 1.374(3) . ? C3 H3 0.9500 . ? C4 C5 1.413(3) . ? C4 C11 1.513(3) . ? C5 C10 1.396(3) . ? C5 C6 1.408(3) . ? C6 C7 1.377(3) . ? C6 C12 1.520(3) . ? C7 C8 1.426(3) . ? C7 H7 0.9500 . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.423(3) . ? C11 C12 1.567(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.393(3) . ? C13 C18 1.400(3) . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.526(3) . ? C19 C21 1.540(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 C32 1.386(3) . ? C31 C40 1.418(3) . ? C32 C33 1.417(4) . ? C32 H32 0.9500 . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 C35 1.411(3) . ? C34 C41 1.517(4) . ? C35 C40 1.400(3) . ? C35 C36 1.411(3) . ? C36 C37 1.371(4) . ? C36 C42 1.519(3) . ? C37 C38 1.417(3) . ? C37 H37 0.9500 . ? C38 C39 1.390(3) . ? C38 H38 0.9500 . ? C39 C40 1.424(3) . ? C41 C42 1.559(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.390(3) . ? C43 C48 1.390(3) . ? C44 C45 1.396(3) . ? C44 H44 0.9500 . ? C45 C46 1.387(3) . ? C45 H45 0.9500 . ? C46 C47 1.384(3) . ? C46 H46 0.9500 . ? C47 C48 1.393(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C51 1.530(3) . ? C49 C50 1.533(3) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 C13 98.78(9) . . ? C1 As1 P9 89.66(7) . . ? C13 As1 P9 102.59(7) . . ? C31 As31 C43 98.11(9) . . ? C31 As31 P39 88.75(7) . . ? C43 As31 P39 101.63(7) . . ? C9 P9 C19 105.59(11) . . ? C9 P9 As1 94.05(8) . . ? C19 P9 As1 103.83(8) . . ? C39 P39 C49 105.99(11) . . ? C39 P39 As31 94.45(8) . . ? C49 P39 As31 103.82(8) . . ? C2 C1 C10 119.4(2) . . ? C2 C1 As1 125.11(18) . . ? C10 C1 As1 115.46(16) . . ? C1 C2 C3 122.1(2) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.5(2) . . ? C3 C4 C11 133.4(2) . . ? C5 C4 C11 108.2(2) . . ? C10 C5 C6 123.5(2) . . ? C10 C5 C4 123.3(2) . . ? C6 C5 C4 113.2(2) . . ? C7 C6 C5 118.0(2) . . ? C7 C6 C12 133.6(2) . . ? C5 C6 C12 108.4(2) . . ? C6 C7 C8 119.4(2) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 122.7(2) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C10 117.8(2) . . ? C8 C9 P9 125.56(17) . . ? C10 C9 P9 116.28(17) . . ? C5 C10 C9 118.5(2) . . ? C5 C10 C1 117.4(2) . . ? C9 C10 C1 124.0(2) . . ? C4 C11 C12 105.27(18) . . ? C4 C11 H11A 110.7 . . ? C12 C11 H11A 110.7 . . ? C4 C11 H11B 110.7 . . ? C12 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? C6 C12 C11 104.75(18) . . ? C6 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? C6 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? C14 C13 C18 118.7(2) . . ? C14 C13 As1 117.39(17) . . ? C18 C13 As1 123.90(18) . . ? C15 C14 C13 120.9(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.2(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.7(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 120.1(2) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C20 C19 C21 111.58(19) . . ? C20 C19 P9 110.25(17) . . ? C21 C19 P9 107.36(17) . . ? C20 C19 H19 109.2 . . ? C21 C19 H19 109.2 . . ? P9 C19 H19 109.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C32 C31 C40 118.8(2) . . ? C32 C31 As31 125.41(18) . . ? C40 C31 As31 115.73(17) . . ? C31 C32 C33 122.3(2) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C34 C33 C32 119.5(2) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 118.2(2) . . ? C33 C34 C41 134.0(2) . . ? C35 C34 C41 107.8(2) . . ? C40 C35 C36 123.4(2) . . ? C40 C35 C34 123.2(2) . . ? C36 C35 C34 113.4(2) . . ? C37 C36 C35 118.0(2) . . ? C37 C36 C42 133.8(2) . . ? C35 C36 C42 108.3(2) . . ? C36 C37 C38 119.7(2) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 122.8(2) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C38 C39 C40 117.9(2) . . ? C38 C39 P39 125.77(19) . . ? C40 C39 P39 115.86(17) . . ? C35 C40 C31 117.9(2) . . ? C35 C40 C39 118.1(2) . . ? C31 C40 C39 123.9(2) . . ? C34 C41 C42 105.6(2) . . ? C34 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? C34 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.7 . . ? C36 C42 C41 104.8(2) . . ? C36 C42 H42A 110.8 . . ? C41 C42 H42A 110.8 . . ? C36 C42 H42B 110.8 . . ? C41 C42 H42B 110.8 . . ? H42A C42 H42B 108.9 . . ? C44 C43 C48 119.0(2) . . ? C44 C43 As31 118.13(17) . . ? C48 C43 As31 122.84(18) . . ? C43 C44 C45 120.7(2) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 119.7(2) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C47 C46 C45 119.8(2) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 120.4(2) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C43 120.3(2) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C51 C49 C50 111.2(2) . . ? C51 C49 P39 107.41(16) . . ? C50 C49 P39 110.05(16) . . ? C51 C49 H49 109.4 . . ? C50 C49 H49 109.4 . . ? P39 C49 H49 109.4 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C1 C2 C3 -0.4(4) . . . . ? As1 C1 C2 C3 179.91(18) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C2 C3 C4 C11 -178.6(2) . . . . ? C3 C4 C5 C10 -0.6(4) . . . . ? C11 C4 C5 C10 178.8(2) . . . . ? C3 C4 C5 C6 178.4(2) . . . . ? C11 C4 C5 C6 -2.2(3) . . . . ? C10 C5 C6 C7 -1.0(4) . . . . ? C4 C5 C6 C7 -179.9(2) . . . . ? C10 C5 C6 C12 178.1(2) . . . . ? C4 C5 C6 C12 -0.8(3) . . . . ? C5 C6 C7 C8 -1.1(3) . . . . ? C12 C6 C7 C8 -179.9(2) . . . . ? C6 C7 C8 C9 3.0(4) . . . . ? C7 C8 C9 C10 -2.9(4) . . . . ? C7 C8 C9 P9 -175.44(18) . . . . ? C19 P9 C9 C8 -74.7(2) . . . . ? As1 P9 C9 C8 179.7(2) . . . . ? C19 P9 C9 C10 112.63(19) . . . . ? As1 P9 C9 C10 7.05(18) . . . . ? C6 C5 C10 C9 1.1(4) . . . . ? C4 C5 C10 C9 180.0(2) . . . . ? C6 C5 C10 C1 -178.8(2) . . . . ? C4 C5 C10 C1 0.0(3) . . . . ? C8 C9 C10 C5 0.8(3) . . . . ? P9 C9 C10 C5 174.07(17) . . . . ? C8 C9 C10 C1 -179.3(2) . . . . ? P9 C9 C10 C1 -6.0(3) . . . . ? C2 C1 C10 C5 0.5(3) . . . . ? As1 C1 C10 C5 -179.83(16) . . . . ? C2 C1 C10 C9 -179.5(2) . . . . ? As1 C1 C10 C9 0.3(3) . . . . ? C3 C4 C11 C12 -176.5(3) . . . . ? C5 C4 C11 C12 4.2(2) . . . . ? C7 C6 C12 C11 -177.7(3) . . . . ? C5 C6 C12 C11 3.4(3) . . . . ? C4 C11 C12 C6 -4.5(2) . . . . ? C18 C13 C14 C15 1.7(4) . . . . ? As1 C13 C14 C15 -179.08(18) . . . . ? C13 C14 C15 C16 -1.0(4) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? C15 C16 C17 C18 0.9(4) . . . . ? C16 C17 C18 C13 -0.2(4) . . . . ? C14 C13 C18 C17 -1.1(3) . . . . ? As1 C13 C18 C17 179.70(17) . . . . ? C9 P9 C19 C20 61.55(18) . . . . ? As1 P9 C19 C20 159.84(14) . . . . ? C9 P9 C19 C21 -176.71(16) . . . . ? As1 P9 C19 C21 -78.41(16) . . . . ? C40 C31 C32 C33 -3.3(3) . . . . ? As31 C31 C32 C33 174.90(17) . . . . ? C31 C32 C33 C34 1.1(4) . . . . ? C32 C33 C34 C35 2.2(3) . . . . ? C32 C33 C34 C41 -179.3(2) . . . . ? C33 C34 C35 C40 -3.4(3) . . . . ? C41 C34 C35 C40 177.7(2) . . . . ? C33 C34 C35 C36 176.1(2) . . . . ? C41 C34 C35 C36 -2.8(3) . . . . ? C40 C35 C36 C37 1.5(3) . . . . ? C34 C35 C36 C37 -178.1(2) . . . . ? C40 C35 C36 C42 -179.8(2) . . . . ? C34 C35 C36 C42 0.7(3) . . . . ? C35 C36 C37 C38 -0.6(3) . . . . ? C42 C36 C37 C38 -179.0(2) . . . . ? C36 C37 C38 C39 -1.5(4) . . . . ? C37 C38 C39 C40 2.6(3) . . . . ? C37 C38 C39 P39 174.11(18) . . . . ? C49 P39 C39 C38 73.6(2) . . . . ? As31 P39 C39 C38 179.40(19) . . . . ? C49 P39 C39 C40 -114.69(18) . . . . ? As31 P39 C39 C40 -8.94(17) . . . . ? C36 C35 C40 C31 -178.2(2) . . . . ? C34 C35 C40 C31 1.2(3) . . . . ? C36 C35 C40 C39 -0.3(3) . . . . ? C34 C35 C40 C39 179.2(2) . . . . ? C32 C31 C40 C35 2.1(3) . . . . ? As31 C31 C40 C35 -176.26(16) . . . . ? C32 C31 C40 C39 -175.7(2) . . . . ? As31 C31 C40 C39 5.9(3) . . . . ? C38 C39 C40 C35 -1.7(3) . . . . ? P39 C39 C40 C35 -174.04(16) . . . . ? C38 C39 C40 C31 176.1(2) . . . . ? P39 C39 C40 C31 3.8(3) . . . . ? C33 C34 C41 C42 -175.1(3) . . . . ? C35 C34 C41 C42 3.6(3) . . . . ? C37 C36 C42 C41 -179.9(3) . . . . ? C35 C36 C42 C41 1.6(3) . . . . ? C34 C41 C42 C36 -3.1(3) . . . . ? C48 C43 C44 C45 -1.1(4) . . . . ? As31 C43 C44 C45 179.83(18) . . . . ? C43 C44 C45 C46 0.9(4) . . . . ? C44 C45 C46 C47 0.0(4) . . . . ? C45 C46 C47 C48 -0.6(4) . . . . ? C46 C47 C48 C43 0.4(4) . . . . ? C44 C43 C48 C47 0.4(3) . . . . ? As31 C43 C48 C47 179.47(17) . . . . ? C39 P39 C49 C51 177.01(16) . . . . ? As31 P39 C49 C51 78.18(16) . . . . ? C39 P39 C49 C50 -61.81(18) . . . . ? As31 P39 C49 C50 -160.65(15) . . . . ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL BCPK151 CELL 0.71075 8.12890 11.21400 20.23900 84.89200 83.61670 70.87900 ZERR 4 0.00170 0.00200 0.00500 0.01100 0.00100 0.00800 LATT 1 SFAC C H AS P UNIT 84 80 4 4 L.S. 20 FMAP 2 PLAN -5 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -180.0 ACTA SIZE 0.100 0.080 0.030 WGHT 0.021700 FVAR 0.40380 AS1 3 0.067293 0.288478 0.332001 11.00000 0.01572 0.01402 = 0.01298 0.00011 -0.00192 -0.00352 AS31 3 0.104384 0.726435 0.158672 11.00000 0.01017 0.02004 = 0.01390 -0.00176 -0.00087 -0.00104 P9 4 -0.175697 0.247979 0.395920 11.00000 0.01386 0.01637 = 0.01716 -0.00059 -0.00281 -0.00494 P39 4 0.097823 0.597180 0.072086 11.00000 0.01167 0.01701 = 0.01549 -0.00010 -0.00116 -0.00365 C1 1 0.145412 0.326164 0.413368 11.00000 0.01579 0.01170 = 0.01507 -0.00136 -0.00128 -0.00284 C2 1 0.286792 0.366987 0.416018 11.00000 0.01697 0.01655 = 0.01750 0.00043 0.00251 -0.00572 AFIX 43 H2 2 0.353507 0.378248 0.375750 11.00000 -1.20000 AFIX 0 C3 1 0.336270 0.392877 0.477154 11.00000 0.01388 0.01646 = 0.02537 -0.00208 -0.00255 -0.00644 AFIX 43 H3 2 0.434643 0.420726 0.477540 11.00000 -1.20000 AFIX 0 C4 1 0.240106 0.377118 0.535578 11.00000 0.01476 0.00934 = 0.01814 -0.00040 -0.00445 0.00011 C5 1 0.095894 0.334246 0.532754 11.00000 0.01333 0.00898 = 0.01867 -0.00134 -0.00114 -0.00075 C6 1 0.010730 0.318501 0.595778 11.00000 0.01839 0.01044 = 0.01743 -0.00199 -0.00064 -0.00172 C7 1 -0.131639 0.276854 0.598708 11.00000 0.01927 0.01698 = 0.01556 -0.00162 0.00392 -0.00448 AFIX 43 H7 2 -0.191130 0.263807 0.640450 11.00000 -1.20000 AFIX 0 C8 1 -0.189001 0.253479 0.538538 11.00000 0.01404 0.01579 = 0.02377 -0.00063 -0.00023 -0.00568 AFIX 43 H8 2 -0.290781 0.228752 0.541022 11.00000 -1.20000 AFIX 0 C9 1 -0.102294 0.265348 0.476446 11.00000 0.01386 0.01139 = 0.01875 -0.00254 -0.00178 -0.00283 C10 1 0.045137 0.308157 0.473447 11.00000 0.01300 0.00797 = 0.01850 -0.00174 -0.00128 -0.00033 C11 1 0.252160 0.397653 0.607531 11.00000 0.01731 0.01507 = 0.01997 -0.00193 -0.00576 -0.00324 AFIX 23 H11A 2 0.231659 0.488116 0.613757 11.00000 -1.20000 H11B 2 0.368765 0.347757 0.621839 11.00000 -1.20000 AFIX 0 C12 1 0.106031 0.351967 0.648171 11.00000 0.02079 0.01901 = 0.01533 -0.00150 -0.00221 -0.00363 AFIX 23 H12A 2 0.157870 0.277219 0.678017 11.00000 -1.20000 H12B 2 0.025399 0.419993 0.675304 11.00000 -1.20000 AFIX 0 C13 1 0.233406 0.118064 0.320976 11.00000 0.01316 0.01367 = 0.01840 -0.00106 0.00030 -0.00513 C14 1 0.252043 0.067374 0.259131 11.00000 0.01766 0.02057 = 0.01483 0.00187 -0.00412 -0.00547 AFIX 43 H14 2 0.186455 0.116115 0.224352 11.00000 -1.20000 AFIX 0 C15 1 0.364719 -0.052916 0.247706 11.00000 0.01971 0.02112 = 0.01817 -0.00463 -0.00009 -0.00712 AFIX 43 H15 2 0.374730 -0.086713 0.205484 11.00000 -1.20000 AFIX 0 C16 1 0.462984 -0.124233 0.297632 11.00000 0.01448 0.01454 = 0.02408 -0.00259 -0.00019 -0.00325 AFIX 43 H16 2 0.539904 -0.207086 0.289864 11.00000 -1.20000 AFIX 0 C17 1 0.448606 -0.074141 0.359070 11.00000 0.01481 0.01901 = 0.02021 0.00439 -0.00449 -0.00491 AFIX 43 H17 2 0.517227 -0.122483 0.393180 11.00000 -1.20000 AFIX 0 C18 1 0.334634 0.046121 0.371019 11.00000 0.01639 0.02069 = 0.01293 -0.00220 -0.00047 -0.00813 AFIX 43 H18 2 0.325296 0.079696 0.413258 11.00000 -1.20000 AFIX 0 C19 1 -0.130162 0.074623 0.390257 11.00000 0.01762 0.01588 = 0.02170 -0.00264 -0.00157 -0.00610 AFIX 13 H19 2 -0.002566 0.029865 0.393451 11.00000 -1.20000 AFIX 0 C20 1 -0.234301 0.024407 0.446875 11.00000 0.02422 0.01811 = 0.02532 0.00038 -0.00325 -0.01048 AFIX 137 H20A 2 -0.191967 0.030922 0.489464 11.00000 -1.20000 H20B 2 -0.219466 -0.064289 0.440610 11.00000 -1.20000 H20C 2 -0.358353 0.074338 0.446911 11.00000 -1.20000 AFIX 0 C21 1 -0.179551 0.054959 0.321690 11.00000 0.02982 0.02825 = 0.02523 -0.00664 -0.00086 -0.01619 AFIX 137 H21A 2 -0.304719 0.098164 0.318473 11.00000 -1.20000 H21B 2 -0.153001 -0.035618 0.316396 11.00000 -1.20000 H21C 2 -0.112360 0.089819 0.286572 11.00000 -1.20000 AFIX 0 C31 1 0.151581 0.848855 0.090407 11.00000 0.00814 0.01769 = 0.01940 -0.00100 -0.00482 0.00005 C32 1 0.155170 0.967961 0.101968 11.00000 0.01563 0.01904 = 0.02528 -0.00356 -0.00913 -0.00065 AFIX 43 H32 2 0.123908 0.997042 0.145730 11.00000 -1.20000 AFIX 0 C33 1 0.203867 1.047846 0.050756 11.00000 0.01707 0.01421 = 0.04220 -0.00073 -0.01391 -0.00170 AFIX 43 H33 2 0.206934 1.128397 0.060453 11.00000 -1.20000 AFIX 0 C34 1 0.246685 1.007858 -0.013137 11.00000 0.00829 0.01712 = 0.03745 0.00657 -0.00824 -0.00184 C35 1 0.234227 0.889418 -0.025549 11.00000 0.00766 0.01602 = 0.02440 0.00352 -0.00366 0.00032 C36 1 0.270052 0.861617 -0.093296 11.00000 0.01009 0.02202 = 0.02307 0.00686 0.00078 0.00166 C37 1 0.256267 0.750273 -0.110955 11.00000 0.01782 0.02667 = 0.01479 0.00177 0.00080 0.00223 AFIX 43 H37 2 0.278410 0.728980 -0.156212 11.00000 -1.20000 AFIX 0 C38 1 0.208843 0.667101 -0.061401 11.00000 0.01665 0.01814 = 0.01954 -0.00149 -0.00406 -0.00114 AFIX 43 H38 2 0.197228 0.591287 -0.074654 11.00000 -1.20000 AFIX 0 C39 1 0.178575 0.691632 0.005774 11.00000 0.00941 0.01540 = 0.01831 0.00130 -0.00278 -0.00102 C40 1 0.189306 0.808141 0.024467 11.00000 0.00665 0.01501 = 0.01933 0.00123 -0.00394 0.00021 C41 1 0.305020 1.065295 -0.078570 11.00000 0.01425 0.02283 = 0.04429 0.01346 -0.00716 -0.00466 AFIX 23 H41A 2 0.421025 1.075000 -0.076432 11.00000 -1.20000 H41B 2 0.220124 1.149313 -0.089070 11.00000 -1.20000 AFIX 0 C42 1 0.314118 0.971158 -0.132127 11.00000 0.02162 0.02832 = 0.03297 0.01309 0.00432 -0.00251 AFIX 23 H42A 2 0.228546 1.011387 -0.165217 11.00000 -1.20000 H42B 2 0.432590 0.941979 -0.155623 11.00000 -1.20000 AFIX 0 C43 1 0.344857 0.646435 0.184661 11.00000 0.01260 0.01644 = 0.01435 -0.00347 -0.00237 -0.00188 C44 1 0.369212 0.565556 0.241512 11.00000 0.01482 0.02390 = 0.01756 -0.00071 0.00065 -0.00752 AFIX 43 H44 2 0.271102 0.550659 0.266513 11.00000 -1.20000 AFIX 0 C45 1 0.536192 0.506011 0.262257 11.00000 0.02101 0.02501 = 0.01618 0.00429 -0.00666 -0.00573 AFIX 43 H45 2 0.551731 0.449973 0.300817 11.00000 -1.20000 AFIX 0 C46 1 0.679370 0.528967 0.226358 11.00000 0.01381 0.02077 = 0.02024 -0.00373 -0.00556 -0.00162 AFIX 43 H46 2 0.793322 0.488731 0.240273 11.00000 -1.20000 AFIX 0 C47 1 0.655759 0.610643 0.170218 11.00000 0.01262 0.01905 = 0.01962 -0.00324 -0.00074 -0.00522 AFIX 43 H47 2 0.753704 0.626990 0.145879 11.00000 -1.20000 AFIX 0 C48 1 0.489245 0.669032 0.149181 11.00000 0.01670 0.01635 = 0.01340 -0.00058 -0.00155 -0.00469 AFIX 43 H48 2 0.474280 0.724543 0.110415 11.00000 -1.20000 AFIX 0 C49 1 0.284790 0.449279 0.085863 11.00000 0.01379 0.01638 = 0.01830 0.00109 -0.00268 -0.00344 AFIX 13 H49 2 0.386379 0.471713 0.098150 11.00000 -1.20000 AFIX 0 C50 1 0.338047 0.376038 0.022281 11.00000 0.01900 0.01832 = 0.02439 -0.00154 -0.00450 -0.00124 AFIX 137 H50A 2 0.235356 0.362235 0.007397 11.00000 -1.20000 H50B 2 0.426666 0.294280 0.031408 11.00000 -1.20000 H50C 2 0.386171 0.424771 -0.012616 11.00000 -1.20000 AFIX 0 C51 1 0.224979 0.371156 0.143600 11.00000 0.02546 0.01827 = 0.02721 0.00410 -0.00270 -0.00745 AFIX 137 H51A 2 0.323504 0.296598 0.154860 11.00000 -1.20000 H51B 2 0.130716 0.344178 0.130492 11.00000 -1.20000 H51C 2 0.182397 0.422642 0.182437 11.00000 -1.20000 AFIX 0 HKLF 4 REM BCPK151 REM R1 = 0.0278 for 5185 Fo > 4sig(Fo) and 0.0335 for all 6291 data REM 419 parameters refined using 0 restraints END WGHT 0.0186 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.755, deepest hole -0.545, 1-sigma level 0.088 Q1 1 0.1360 0.8019 0.1383 11.00000 0.05 0.76 Q2 1 0.0271 0.2112 0.3520 11.00000 0.05 0.60 Q3 1 0.0765 0.6493 0.1655 11.00000 0.05 0.58 Q4 1 0.1021 0.3665 0.3156 11.00000 0.05 0.56 Q5 1 0.1439 0.6619 0.0439 11.00000 0.05 0.49 ; _shelx_res_checksum 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6.78 5 2 -19 7.06 7.12 1 1 24 439.24 22.18 -1 -1 -24 369.48 38.77 -1 -1 -24 475.77 28.14 3 -9 11 50.61 12.39 -3 9 -11 37.42 11.94 -3 9 -11 51.84 12.87 5 13 3 94.52 12.17 5 13 3 90.90 12.79 -5 -13 -3 90.92 16.42 -5 -13 -3 80.78 18.63 5 13 2 15.63 7.45 -5 -13 -2 13.67 14.12 -5 -13 -2 18.27 15.46 5 13 2 18.44 8.37 -1 12 -1 12.38 8.53 1 -12 1 15.63 13.64 -6 1 16 6.02 7.29 2 13 6 -0.67 7.12 -1 -10 14 32.99 14.42 1 10 -14 32.28 10.16 -1 -10 14 47.18 14.31 -7 4 8 375.14 29.66 7 -4 -8 409.74 27.55 4 -7 14 1.90 9.46 -4 7 -14 2.67 10.83 3 13 -3 33.13 10.10 -3 -13 3 36.93 14.22 -3 -13 3 30.80 13.75 8 2 15 133.08 13.83 8 2 15 114.67 14.03 8 2 15 119.57 15.58 -8 -2 -15 98.45 17.26 4 8 20 35.41 7.28 -4 -8 -20 42.56 9.91 -8 3 -6 165.17 22.79 8 -3 6 154.87 14.87 -4 -11 -15 -2.53 10.08 4 11 15 0.12 5.19 8 6 15 102.90 13.71 -8 -6 -15 100.22 17.35 -8 3 3 10.73 7.26 8 -3 -3 13.95 9.02 -4 -9 15 6.44 12.26 4 9 -15 6.10 8.72 -9 -5 -11 26.48 11.93 -2 -5 21 267.24 20.01 -2 -5 21 286.46 29.85 -5 -1 19 2.67 7.81 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