# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_global loop_ _publ_author_name 'Nitta, Makoto' 'Mitsumoto, Yuhki' _publ_contact_author_name 'Dr Makoto Nitta' _publ_contact_author_address ; Department of Chemistry School of Science and Engineering Materials Research Laboratory for b Waseda University Shinjuku-ku Tokyo 169-8555 JAPAN ; _publ_contact_author_email 'NITTA@MN.WASEDA.AC.JP' _publ_requested_journal 'Perkin Transactions 1' _publ_section_title ; Synthesis, structure, and reactivity of (triphenyaroranylidene)methyltropone derivatives: reactions with heterocumulenes and an activated acetylene. ; data_ _database_code_CSD 187524 _audit_creation_method 'maXus' _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All diagrams and calculations were performed using maXus (Bruker Nonius, Delft & MacScience, Japan). ; _publ_section_synopsis ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'yellow' _cell_measurement_temperature 250 _refine_ls_hydrogen_treatment 'refxyz' # Submission details _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 loop_ _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 0.06177 _diffrn_orient_matrix_UB_12 0.01078 _diffrn_orient_matrix_UB_13 -0.01438 _diffrn_orient_matrix_UB_21 -0.01189 _diffrn_orient_matrix_UB_22 0.05770 _diffrn_orient_matrix_UB_23 -0.00218 _diffrn_orient_matrix_UB_31 0.00773 _diffrn_orient_matrix_UB_32 0.00251 _diffrn_orient_matrix_UB_33 0.11188 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 496.438 _diffrn_radiation_type ' CuK\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X,-Y,+Z+ 1/2' '-X+ 1/2,+Y+ 1/2,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,+Z' _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_cell_setting 'Orthorhombic' _chemical_formula_moiety 'C29 H25 As O3 ' _chemical_formula_sum 'C29 H25 As O3 ' _chemical_name_systematic ; ? ; _cell_length_a 17.021(6) _cell_length_b 8.864(5) _cell_length_c 15.780(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2381.(2) _diffrn_reflns_number 9091 _diffrn_reflns_theta_max 70.02 _diffrn_reflns_av_R_equivalents 0.068 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' _exptl_absorpt_coefficient_mu 2.155 _reflns_number_total 4449 _reflns_number_gt 4441 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 4449 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.581 _refine_ls_restrained_S_all 1.581 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 -0.520255(14) -0.14904(3) -0.2740 0.03308(17) Uani 1 1 d . . . O2 O -0.55558(13) 0.0771(2) -0.21183(16) 0.0424(5) Uani 1 1 d . . . O3 O -0.61209(14) -0.4492(2) -0.11874(19) 0.0470(5) Uani 1 1 d . . . O4 O -0.48669(14) -0.4063(3) -0.1562(2) 0.0461(6) Uani 1 1 d . . . C5 C -0.61560(15) -0.1046(3) -0.12578(17) 0.0338(5) Uani 1 1 d . . . C6 C -0.57260(15) -0.2083(3) -0.17442(18) 0.0338(5) Uani 1 1 d . . . C7 C -0.5619(2) -0.3638(3) -0.1471(2) 0.0360(7) Uani 1 1 d . . . C8 C -0.5058(3) -0.3427(3) -0.3326(3) 0.0366(7) Uani 1 1 d . . . C9 C -0.60275(17) 0.0555(3) -0.15068(19) 0.0340(5) Uani 1 1 d . . . C10 C -0.41612(18) -0.0649(3) -0.2675(2) 0.0410(6) Uani 1 1 d . . . C11 C -0.3560(3) -0.1522(4) -0.2332(3) 0.0504(9) Uani 1 1 d . . . C12 C -0.5701(2) -0.4379(4) -0.3392(3) 0.0508(8) Uani 1 1 d . . . C13 C -0.4367(2) -0.3813(5) -0.3755(3) 0.0504(8) Uani 1 1 d . . . C14 C -0.7066(3) -0.0644(5) 0.0013(3) 0.0546(9) Uani 1 1 d . . . C15 C -0.6634(2) -0.1497(3) -0.0566(3) 0.0424(7) Uani 1 1 d . . . C16 C -0.58026(18) -0.0588(3) -0.3642(2) 0.0371(6) Uani 1 1 d . . . C17 C -0.5453(2) -0.0433(4) -0.4434(2) 0.0501(7) Uani 1 1 d . . . C18 C -0.4032(2) 0.0828(4) -0.2930(2) 0.0496(7) Uani 1 1 d . . . C19 C -0.6876(2) 0.1969(4) -0.0424(3) 0.0534(8) Uani 1 1 d . . . C20 C -0.6584(2) -0.0203(4) -0.3533(2) 0.0516(7) Uani 1 1 d . . . C21 C -0.6662(3) 0.0508(6) -0.4997(3) 0.0687(12) Uani 1 1 d . . . C22 C -0.4328(2) -0.5150(5) -0.4205(3) 0.0572(9) Uani 1 1 d . . . C23 C -0.5644(3) -0.5745(5) -0.3838(3) 0.0593(9) Uani 1 1 d . . . C24 C -0.6373(2) 0.1825(4) -0.1112(2) 0.0443(6) Uani 1 1 d . . . C25 C -0.2816(2) -0.0908(7) -0.2255(2) 0.0616(10) Uani 1 1 d . . . C26 C -0.4971(4) -0.6110(5) -0.4242(3) 0.0615(9) Uani 1 1 d . . . C27 C -0.2674(2) 0.0553(5) -0.2497(3) 0.0616(10) Uani 1 1 d . . . C28 C -0.3267(3) 0.1425(4) -0.2840(4) 0.0626(12) Uani 1 1 d . . . C29 C -0.7183(2) 0.0886(5) 0.0096(3) 0.0577(9) Uani 1 1 d . . . C30 C -0.7004(2) 0.0341(6) -0.4221(3) 0.0674(11) Uani 1 1 d . . . C31 C -0.5877(3) 0.0154(6) -0.5103(3) 0.0638(10) Uani 1 1 d . . . C32 C -0.4681(3) -0.5645(5) -0.1400(4) 0.0595(11) Uani 1 1 d . . . C33 C -0.3825(3) -0.5770(6) -0.1302(6) 0.093(2) Uani 1 1 d . . . H11 H -0.3668 -0.2538 -0.2157 0.060 Uiso 1 1 d R . . H12 H -0.6191 -0.4105 -0.3133 0.061 Uiso 1 1 d R . . H13 H -0.3921 -0.3149 -0.3733 0.061 Uiso 1 1 d R . . H14 H -0.7355 -0.1149 0.0452 0.066 Uiso 1 1 d R . . H15 H -0.6687 -0.2550 -0.0438 0.051 Uiso 1 1 d R . . H17 H -0.4908 -0.0679 -0.4502 0.060 Uiso 1 1 d R . . H18 H -0.4456 0.1415 -0.3159 0.059 Uiso 1 1 d R . . H19 H -0.7046 0.2948 -0.0240 0.064 Uiso 1 1 d R . . H20 H -0.6826 -0.0324 -0.2987 0.062 Uiso 1 1 d R . . H21 H -0.6970 0.0859 -0.5467 0.082 Uiso 1 1 d R . . H22 H -0.3859 -0.5431 -0.4503 0.069 Uiso 1 1 d R . . H23 H -0.6086 -0.6418 -0.3846 0.071 Uiso 1 1 d R . . H24 H -0.6273 0.2823 -0.1323 0.053 Uiso 1 1 d R . . H25 H -0.2395 -0.1501 -0.2024 0.074 Uiso 1 1 d R . . H26 H -0.4945 -0.7035 -0.4557 0.074 Uiso 1 1 d R . . H27 H -0.2154 0.0954 -0.2433 0.074 Uiso 1 1 d R . . H28 H -0.3162 0.2442 -0.3015 0.075 Uiso 1 1 d R . . H29 H -0.7513 0.1264 0.0541 0.069 Uiso 1 1 d R . . H30 H -0.7541 0.0649 -0.4157 0.081 Uiso 1 1 d R . . H31 H -0.5641 0.0280 -0.5651 0.077 Uiso 1 1 d R . . H32A H -0.4864 -0.6254 -0.1862 0.071 Uiso 1 1 d R . . H32B H -0.4938 -0.5955 -0.0887 0.071 Uiso 1 1 d R . . H33A H -0.3651 -0.6781 -0.1189 0.112 Uiso 1 1 d R . . H33B H -0.3594 -0.5421 -0.1821 0.112 Uiso 1 1 d R . . H33C H -0.3668 -0.5122 -0.0845 0.112 Uiso 1 1 d 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 0.0278(2) 0.0393(2) 0.0321(2) 0.00160(14) 0.00035(12) -0.00183(8) O2 0.0446(13) 0.0377(9) 0.0448(11) 0.0004(8) 0.0060(9) -0.0019(7) O3 0.0455(12) 0.0374(10) 0.0582(14) 0.0105(9) 0.0031(11) 0.0018(8) O4 0.0355(14) 0.0463(15) 0.0564(16) 0.0054(11) -0.0030(9) 0.0071(9) C5 0.0289(12) 0.0418(12) 0.0307(13) -0.0029(12) -0.0026(11) -0.0009(10) C6 0.0292(13) 0.0381(14) 0.0340(13) 0.0029(10) 0.0033(10) -0.0011(9) C7 0.0307(16) 0.0377(15) 0.0394(16) 0.0020(10) -0.0022(12) -0.0031(10) C8 0.0347(17) 0.0429(18) 0.0321(18) -0.0029(10) 0.0023(17) 0.0046(11) C9 0.0346(14) 0.0347(12) 0.0328(13) 0.0005(10) -0.0021(10) 0.0010(10) C10 0.0309(12) 0.0533(14) 0.0386(14) -0.0040(12) 0.0044(13) -0.0077(11) C11 0.0419(19) 0.072(2) 0.0377(17) 0.0012(12) -0.0027(14) -0.0087(13) C12 0.0451(18) 0.0577(18) 0.0495(19) -0.0050(14) 0.0024(15) -0.0088(14) C13 0.0385(19) 0.0654(18) 0.047(2) -0.0109(17) 0.0074(15) -0.0007(15) C14 0.054(2) 0.0597(18) 0.0499(19) -0.0005(15) 0.0186(18) 0.0008(15) C15 0.0435(17) 0.0418(15) 0.0420(17) 0.0053(10) 0.0056(16) 0.0016(10) C16 0.0310(13) 0.0419(13) 0.0384(15) 0.0045(11) -0.0056(11) 0.0013(10) C17 0.0494(19) 0.0604(19) 0.0405(18) 0.0056(14) 0.0017(15) -0.0030(16) C18 0.0403(16) 0.0577(18) 0.0507(19) -0.0021(13) 0.0085(13) -0.0115(13) C19 0.0493(16) 0.0512(18) 0.060(2) -0.0156(15) 0.0112(16) 0.0054(14) C20 0.0387(16) 0.0684(18) 0.0478(18) 0.0010(15) -0.0019(14) 0.0068(14) C21 0.066(3) 0.090(3) 0.051(2) 0.012(2) -0.023(2) 0.005(2) C22 0.0425(17) 0.074(2) 0.055(2) -0.0155(18) 0.0005(15) 0.0110(16) C23 0.063(2) 0.057(2) 0.058(2) -0.0065(15) 0.0021(18) -0.0138(17) C24 0.0402(15) 0.0380(13) 0.0545(17) -0.0103(14) 0.0042(14) -0.0017(12) C25 0.0365(18) 0.107(3) 0.042(2) -0.015(2) -0.0029(13) -0.0024(19) C26 0.088(2) 0.0501(18) 0.047(2) -0.014(2) 0.001(3) 0.011(3) C27 0.0388(18) 0.083(2) 0.063(2) -0.0196(18) 0.0088(15) -0.0148(16) C28 0.058(2) 0.059(2) 0.070(3) -0.0125(17) 0.019(2) -0.0231(15) C29 0.051(2) 0.073(2) 0.0491(18) -0.0153(17) 0.0123(15) 0.0028(18) C30 0.0369(19) 0.094(3) 0.071(3) 0.001(2) -0.0191(19) 0.0156(17) C31 0.068(2) 0.076(2) 0.046(2) 0.0106(18) -0.0043(17) 0.009(2) C32 0.055(2) 0.0421(17) 0.082(3) 0.0013(18) -0.002(2) 0.0156(15) C33 0.067(3) 0.069(3) 0.143(6) -0.007(3) -0.029(4) 0.027(2) _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 C6 1.881(3) . ? As1 C16 1.926(3) . ? As1 C10 1.926(3) . ? As1 C8 1.966(3) . ? As1 O2 2.311(2) . ? O2 C9 1.270(4) . ? O3 C7 1.227(4) . ? O4 C7 1.342(5) . ? O4 C32 1.460(5) . ? C5 C6 1.404(4) . ? C5 C15 1.419(4) . ? C5 C9 1.488(4) . ? C6 C7 1.455(4) . ? C8 C12 1.386(6) . ? C8 C13 1.400(6) . ? C9 C24 1.414(4) . ? C10 C18 1.387(5) . ? C10 C11 1.393(5) . ? C11 C25 1.383(6) . ? C12 C23 1.404(6) . ? C13 C22 1.384(6) . ? C14 C29 1.377(6) . ? C14 C15 1.396(6) . ? C16 C20 1.385(5) . ? C16 C17 1.391(5) . ? C17 C31 1.381(6) . ? C18 C28 1.412(5) . ? C19 C29 1.367(6) . ? C19 C24 1.388(5) . ? C20 C30 1.386(5) . ? C21 C30 1.364(8) . ? C21 C31 1.382(8) . ? C22 C26 1.387(8) . ? C23 C26 1.351(8) . ? C25 C27 1.372(8) . ? C27 C28 1.381(7) . ? C32 C33 1.470(8) . ? 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 C6 As1 C16 118.83(13) . . ? C6 As1 C10 119.98(14) . . ? C16 As1 C10 111.50(14) . . ? C6 As1 C8 102.03(15) . . ? C16 As1 C8 94.66(16) . . ? C10 As1 C8 104.36(18) . . ? C6 As1 O2 76.39(10) . . ? C16 As1 O2 79.38(11) . . ? C10 As1 O2 83.15(11) . . ? C8 As1 O2 171.82(16) . . ? C9 O2 As1 110.85(16) . . ? C7 O4 C32 117.2(3) . . ? C6 C5 C15 122.3(3) . . ? C6 C5 C9 113.8(2) . . ? C15 C5 C9 123.8(3) . . ? C5 C6 C7 121.6(3) . . ? C5 C6 As1 121.4(2) . . ? C7 C6 As1 116.9(2) . . ? O3 C7 O4 122.0(3) . . ? O3 C7 C6 127.2(3) . . ? O4 C7 C6 110.8(3) . . ? C12 C8 C13 118.6(3) . . ? C12 C8 As1 117.9(3) . . ? C13 C8 As1 123.1(3) . . ? O2 C9 C24 118.5(3) . . ? O2 C9 C5 115.9(2) . . ? C24 C9 C5 125.5(3) . . ? C18 C10 C11 121.4(3) . . ? C18 C10 As1 119.8(3) . . ? C11 C10 As1 118.8(2) . . ? C25 C11 C10 119.2(4) . . ? C8 C12 C23 120.6(4) . . ? C22 C13 C8 119.8(4) . . ? C29 C14 C15 132.2(4) . . ? C14 C15 C5 130.8(3) . . ? C20 C16 C17 119.9(3) . . ? C20 C16 As1 121.3(3) . . ? C17 C16 As1 118.6(3) . . ? C31 C17 C16 120.1(4) . . ? C10 C18 C28 118.1(4) . . ? C29 C19 C24 129.9(3) . . ? C16 C20 C30 118.9(4) . . ? C30 C21 C31 119.8(4) . . ? C13 C22 C26 120.7(4) . . ? C26 C23 C12 120.1(4) . . ? C19 C24 C9 132.4(3) . . ? C27 C25 C11 120.6(4) . . ? C23 C26 C22 120.2(4) . . ? C25 C27 C28 120.6(3) . . ? C27 C28 C18 120.2(4) . . ? C19 C29 C14 125.4(4) . . ? C21 C30 C20 121.5(4) . . ? C17 C31 C21 119.8(4) . . ? O4 C32 C33 107.8(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 70.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.490 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.067 data_YMAsCN _database_code_CSD 187525 _audit_creation_date '2002-08-02' _audit_creation_method 'by CrystalStructure v3.00' _audit_update_record ? #=========================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #=========================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.00. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. Larson, A. C. (1970), Crystallographic Computing, 291-294. ed F. R. Ahmed, Munksgaard, Copenhagen. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #=========================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H20 As N O ' _chemical_formula_moiety 'C27 H20 As N O ' _chemical_formula_weight 449.38 _chemical_melting_point ? #=========================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' #--------------------------------------------------------------------------- _cell_length_a 8.0799(5) _cell_length_b 13.4532(7) _cell_length_c 9.6920(4) _cell_angle_alpha 90 _cell_angle_beta 97.948(3) _cell_angle_gamma 90 _cell_volume 1043.4(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10766 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.1 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460.00 _exptl_absorpt_coefficient_mu 1.648 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 0.848 #=========================================================================== #== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 9624 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9992 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 #=========================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). 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 2490 _reflns_number_gt 9409 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1030 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 9409 _refine_ls_number_parameters 293 _refine_ls_goodness_of_fit_ref 1.527 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.5000\s^2^(Fo) + 0.0010]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 3.73 _refine_diff_density_min -1.44 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 35.1(10) _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 6892 Friedel Pairs' _refine_ls_abs_structure_Flack 0.001(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'As' 'As' -0.093 2.226 ; International Tables for Crystallography (1992, 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.39200(2) 0.29468(3) 0.84465(1) 0.01728(5) Uani 1.00 1 d . . . O1 O 0.1520(2) 0.3863(1) 0.7430(1) 0.0227(4) Uani 1.00 1 d . . . N1 N 0.3518(3) 0.0236(1) 0.7352(2) 0.0377(5) Uani 1.00 1 d . . . C1 C 0.0618(3) 0.3349(2) 0.6534(2) 0.0183(5) Uani 1.00 1 d . . . C2 C 0.1175(2) 0.2328(2) 0.6341(2) 0.0187(5) Uani 1.00 1 d . . . C3 C 0.0339(3) 0.1627(1) 0.5421(2) 0.0225(5) Uani 1.00 1 d . . . C4 C -0.1114(3) 0.1676(2) 0.4490(2) 0.0281(5) Uani 1.00 1 d . . . C5 C -0.2198(3) 0.2471(2) 0.4186(3) 0.0287(6) Uani 1.00 1 d . . . C6 C -0.2057(3) 0.3400(2) 0.4776(3) 0.0268(5) Uani 1.00 1 d . . . C7 C -0.0857(3) 0.3786(2) 0.5800(2) 0.0231(5) Uani 1.00 1 d . . . C8 C 0.2664(3) 0.2072(1) 0.7198(2) 0.0197(4) Uani 1.00 1 d . . . C9 C 0.3176(3) 0.1065(2) 0.7291(2) 0.0251(5) Uani 1.00 1 d . . . C10 C 0.5840(2) 0.2107(1) 0.9060(2) 0.0197(4) Uani 1.00 1 d . . . C11 C 0.6019(3) 0.1627(1) 1.0350(2) 0.0227(5) Uani 1.00 1 d . . . C12 C 0.7285(3) 0.0933(2) 1.0669(2) 0.0267(5) Uani 1.00 1 d . . . C13 C 0.8362(3) 0.0709(2) 0.9718(3) 0.0284(5) Uani 1.00 1 d . . . C14 C 0.8197(3) 0.1204(2) 0.8437(2) 0.0274(5) Uani 1.00 1 d . . . C15 C 0.6952(3) 0.1905(1) 0.8112(2) 0.0238(5) Uani 1.00 1 d . . . C16 C 0.5020(3) 0.4090(1) 0.7764(2) 0.0216(5) Uani 1.00 1 d . . . C17 C 0.6365(3) 0.4493(2) 0.8636(3) 0.0283(5) Uani 1.00 1 d . . . C18 C 0.7128(3) 0.5345(2) 0.8229(3) 0.0336(6) Uani 1.00 1 d . . . C19 C 0.6592(3) 0.5778(2) 0.6948(3) 0.0350(6) Uani 1.00 1 d . . . C20 C 0.5288(3) 0.5348(2) 0.6067(3) 0.0338(6) Uani 1.00 1 d . . . C21 C 0.4492(3) 0.4507(2) 0.6466(2) 0.0273(5) Uani 1.00 1 d . . . C22 C 0.2954(3) 0.3185(1) 1.0129(2) 0.0194(4) Uani 1.00 1 d . . . C23 C 0.1309(2) 0.2881(2) 1.0171(2) 0.0264(4) Uani 1.00 1 d . . . C24 C 0.0607(3) 0.3004(3) 1.1389(2) 0.0306(5) Uani 1.00 1 d . . . C25 C 0.1525(3) 0.3458(2) 1.2540(2) 0.0299(6) Uani 1.00 1 d . . . C26 C 0.3160(3) 0.3756(2) 1.2483(2) 0.0265(5) Uani 1.00 1 d . . . C27 C 0.3880(3) 0.3623(1) 1.1279(2) 0.0222(4) Uani 1.00 1 d . . . H1 H 0.0987(3) 0.0958(1) 0.5474(2) 0.026(1) Uiso 1.00 1 c . . . H2 H -0.1588(3) 0.1141(2) 0.3808(2) 0.033(1) Uiso 1.00 1 c . . . H3 H -0.3146(3) 0.2369(2) 0.3495(3) 0.034(1) Uiso 1.00 1 c . . . H4 H -0.2944(3) 0.3818(2) 0.4471(3) 0.032(1) Uiso 1.00 1 c . . . H5 H -0.0985(3) 0.4555(2) 0.6109(2) 0.028(1) Uiso 1.00 1 c . . . H6 H 0.3688(3) 0.4156(2) 0.5904(2) 0.033(1) Uiso 1.00 1 c . . . H7 H 0.5112(3) 0.5658(2) 0.5291(3) 0.042(1) Uiso 1.00 1 c . . . H8 H 0.6600(3) 0.6654(2) 0.6635(3) 0.045(1) Uiso 1.00 1 c . . . H9 H 0.7983(3) 0.5684(2) 0.8815(3) 0.041(1) Uiso 1.00 1 c . . . H10 H 0.6694(3) 0.4181(2) 0.9509(3) 0.034(1) Uiso 1.00 1 c . . . H11 H 0.6990(3) 0.2180(1) 0.7316(2) 0.028(1) Uiso 1.00 1 c . . . H12 H 0.8996(3) 0.1077(2) 0.7753(2) 0.032(1) Uiso 1.00 1 c . . . H13 H 0.9156(3) 0.0175(2) 0.9813(3) 0.033(1) Uiso 1.00 1 c . . . H14 H 0.7441(3) 0.0607(2) 1.1464(2) 0.031(1) Uiso 1.00 1 c . . . H15 H 0.5250(3) 0.1828(1) 1.1164(2) 0.027(1) Uiso 1.00 1 c . . . H16 H 0.5039(3) 0.3898(1) 1.1295(2) 0.027(1) Uiso 1.00 1 c . . . H17 H 0.3719(3) 0.4154(2) 1.3315(2) 0.032(1) Uiso 1.00 1 c . . . H18 H 0.1079(3) 0.3549(2) 1.3534(2) 0.037(1) Uiso 1.00 1 c . . . H19 H -0.0495(3) 0.2864(3) 1.1318(2) 0.037(1) Uiso 1.00 1 c . . . H21 H 0.0613(2) 0.2460(2) 0.9388(2) 0.032(1) Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As1 0.0190(1) 0.0177(1) 0.0147(1) -0.00152(9) 0.00099(6) -0.00153(9) O1 0.0246(7) 0.0194(7) 0.0232(7) 0.0015(5) 0.0008(6) -0.0021(6) N1 0.042(1) 0.0230(9) 0.042(1) 0.0096(8) -0.0160(9) -0.0085(9) C1 0.0199(9) 0.0200(9) 0.0153(9) -0.0006(8) 0.0032(7) 0.0018(7) C2 0.020(1) 0.018(1) 0.0183(9) -0.0003(7) 0.0036(7) 0.0004(8) C3 0.024(1) 0.0237(9) 0.0185(9) 0.0008(8) -0.0022(7) -0.0022(8) C4 0.026(1) 0.033(1) 0.023(1) -0.0015(9) -0.0026(8) -0.0029(9) C5 0.022(1) 0.038(1) 0.024(1) 0.0020(9) -0.0040(9) 0.003(1) C6 0.020(1) 0.038(1) 0.022(1) 0.0041(9) 0.0017(9) 0.010(1) C7 0.023(1) 0.024(1) 0.023(1) 0.0052(7) 0.0047(8) 0.0025(8) C8 0.023(1) 0.0188(9) 0.0159(8) -0.0006(7) -0.0011(7) 0.0009(7) C9 0.024(1) 0.026(1) 0.023(1) 0.0032(8) -0.0063(8) -0.0064(8) C10 0.0198(9) 0.0183(8) 0.0202(9) -0.0017(7) -0.0001(7) 0.0019(8) C11 0.027(1) 0.024(1) 0.0173(8) -0.0060(8) 0.0010(7) 0.0030(8) C12 0.032(1) 0.024(1) 0.0217(9) -0.0041(8) -0.0049(8) 0.0048(8) C13 0.021(1) 0.0206(9) 0.041(1) -0.0014(7) -0.0027(9) 0.0021(9) C14 0.021(1) 0.027(1) 0.034(1) -0.0026(8) 0.0039(8) -0.003(1) C15 0.024(1) 0.024(1) 0.0231(9) -0.0038(8) 0.0028(8) 0.0045(8) C16 0.0229(9) 0.0203(9) 0.0225(9) 0.0001(7) 0.0064(8) -0.0010(8) C17 0.026(1) 0.028(1) 0.031(1) -0.0011(8) 0.0058(9) 0.0006(9) C18 0.028(1) 0.026(1) 0.048(1) -0.0056(9) 0.011(1) -0.007(1) C19 0.037(1) 0.022(1) 0.051(1) 0.0009(9) 0.024(1) 0.002(1) C20 0.041(1) 0.030(1) 0.035(1) 0.009(1) 0.020(1) 0.013(1) C21 0.028(1) 0.031(1) 0.0245(9) 0.0022(9) 0.0089(8) -0.0001(9) C22 0.0237(9) 0.019(1) 0.0155(8) -0.0019(6) 0.0042(7) -0.0021(6) C23 0.0243(8) 0.027(1) 0.0273(9) -0.007(1) 0.0027(7) -0.005(1) C24 0.0267(9) 0.036(1) 0.0304(9) -0.005(1) 0.0096(7) 0.005(1) C25 0.036(1) 0.031(1) 0.024(1) -0.0008(9) 0.0119(9) -0.000(1) C26 0.032(1) 0.028(1) 0.0191(9) -0.0013(8) 0.0021(8) -0.0021(8) C27 0.0225(9) 0.0235(9) 0.0204(9) -0.0031(7) 0.0020(7) -0.0036(8) #=========================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 3.00' _computing_molecular_graphics ? #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag As1 . C8 . 1.881(2) yes As1 . C10 . 1.945(2) yes As1 . C16 . 1.9376(19) yes As1 . C22 . 1.9297(18) yes O1 . C1 . 1.260(3) yes N1 . C9 . 1.149(3) yes C1 . C2 . 1.466(3) yes C1 . C7 . 1.427(3) yes C2 . C3 . 1.406(3) yes C2 . C8 . 1.407(3) yes C3 . C4 . 1.380(3) yes C3 . H1 . 1.039(3) no C4 . C5 . 1.388(3) yes C4 . H2 . 1.016(3) no C5 . C6 . 1.373(3) yes C5 . H3 . 0.955(3) no C6 . C7 . 1.388(3) yes C6 . H4 . 0.927(3) no C7 . H5 . 1.086(3) no C8 . C9 . 1.416(3) yes C10 . C11 . 1.397(3) yes C10 . C15 . 1.397(3) yes C11 . C12 . 1.388(3) yes C11 . H15 . 1.104(4) no C12 . C13 . 1.386(3) yes C12 . H14 . 0.880(3) no C13 . C14 . 1.399(3) yes C13 . H13 . 0.959(3) no C14 . C15 . 1.383(3) yes C14 . H12 . 1.002(4) no C15 . H11 . 0.860(3) no C16 . C17 . 1.391(3) yes C16 . C21 . 1.389(3) yes C17 . C18 . 1.384(3) yes C17 . H10 . 0.949(3) no C18 . C19 . 1.386(4) yes C18 . H9 . 0.948(3) no C19 . C20 . 1.388(4) yes C19 . H8 . 1.217(4) no C20 . C21 . 1.383(3) yes C20 . H7 . 0.855(3) no C21 . H6 . 0.919(3) no C22 . C23 . 1.397(3) yes C22 . C27 . 1.385(3) yes C23 . C24 . 1.388(3) yes C23 . H21 . 1.046(3) no C24 . C25 . 1.393(3) yes C24 . H19 . 0.903(3) no C25 . C26 . 1.389(3) yes C25 . H18 . 1.080(4) no C26 . C27 . 1.386(3) yes C26 . H17 . 1.020(3) no C27 . H16 . 1.005(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C8 . As1 . C10 . 99.78(8) yes C8 . As1 . C16 . 120.60(8) yes C10 . As1 . C16 . 100.44(8) yes C8 . As1 . C22 . 113.72(8) yes C10 . As1 . C22 . 103.70(8) yes C16 . As1 . C22 . 114.51(8) yes O1 . C1 . C2 . 116.3(2) yes O1 . C1 . C7 . 118.81(19) yes C2 . C1 . C7 . 124.9(2) yes C1 . C2 . C3 . 125.50(19) yes C1 . C2 . C8 . 114.0(2) yes C3 . C2 . C8 . 120.5(2) yes C2 . C3 . C4 . 132.4(2) yes C2 . C3 . H1 . 110.8(2) no C4 . C3 . H1 . 116.8(2) no C3 . C4 . C5 . 129.1(2) yes C3 . C4 . H2 . 127.0(3) no C5 . C4 . H2 . 103.8(3) no C4 . C5 . C6 . 126.9(2) yes C4 . C5 . H3 . 117.3(3) no C6 . C5 . H3 . 115.8(3) no C5 . C6 . C7 . 130.3(2) yes C5 . C6 . H4 . 113.8(3) no C7 . C6 . H4 . 115.8(3) no C1 . C7 . C6 . 130.9(2) yes C1 . C7 . H5 . 111.0(2) no C6 . C7 . H5 . 118.0(3) no As1 . C8 . C2 . 124.61(16) yes As1 . C8 . C9 . 115.51(14) yes C2 . C8 . C9 . 119.35(18) yes N1 . C9 . C8 . 176.9(2) yes As1 . C10 . C11 . 121.46(15) yes As1 . C10 . C15 . 118.04(15) yes C11 . C10 . C15 . 120.13(19) yes C10 . C11 . C12 . 119.52(19) yes C10 . C11 . H15 . 121.8(2) no C12 . C11 . H15 . 118.4(2) no C11 . C12 . C13 . 120.6(2) yes C11 . C12 . H14 . 122.8(3) no C13 . C12 . H14 . 116.6(3) no C12 . C13 . C14 . 119.7(2) yes C12 . C13 . H13 . 124.9(3) no C14 . C13 . H13 . 115.0(3) no C13 . C14 . C15 . 120.26(19) yes C13 . C14 . H12 . 120.9(3) no C15 . C14 . H12 . 118.8(3) no C10 . C15 . C14 . 119.76(19) yes C10 . C15 . H11 . 127.7(3) no C14 . C15 . H11 . 112.5(3) no As1 . C16 . C17 . 117.33(16) yes As1 . C16 . C21 . 122.10(16) yes C17 . C16 . C21 . 120.56(19) yes C16 . C17 . C18 . 119.4(2) yes C16 . C17 . H10 . 117.9(3) no C18 . C17 . H10 . 122.6(3) no C17 . C18 . C19 . 120.5(2) yes C17 . C18 . H9 . 123.0(3) no C19 . C18 . H9 . 116.5(3) no C18 . C19 . C20 . 119.5(2) yes C18 . C19 . H8 . 128.2(3) no C20 . C19 . H8 . 106.3(3) no C19 . C20 . C21 . 120.8(2) yes C19 . C20 . H7 . 110.9(3) no C21 . C20 . H7 . 128.2(3) no C16 . C21 . C20 . 119.2(2) yes C16 . C21 . H6 . 115.6(3) no C20 . C21 . H6 . 124.9(3) no As1 . C22 . C23 . 118.28(15) yes As1 . C22 . C27 . 120.94(15) yes C23 . C22 . C27 . 120.76(17) yes C22 . C23 . C24 . 119.51(19) yes C22 . C23 . H21 . 123.7(3) no C24 . C23 . H21 . 116.1(3) no C23 . C24 . C25 . 119.9(2) yes C23 . C24 . H19 . 115.1(3) no C25 . C24 . H19 . 124.2(3) no C24 . C25 . C26 . 119.93(18) yes C24 . C25 . H18 . 123.9(3) no C26 . C25 . H18 . 116.0(3) no C25 . C26 . C27 . 120.6(2) yes C25 . C26 . H17 . 116.1(3) no C27 . C26 . H17 . 122.8(3) no C22 . C27 . C26 . 119.30(19) yes C22 . C27 . H16 . 124.6(2) no C26 . C27 . H16 . 116.0(2) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_site_symmetry_1 _geom_torsion_atom_site_label_2 _geom_torsion_site_symmetry_2 _geom_torsion_atom_site_label_3 _geom_torsion_site_symmetry_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C10 . As1 . C8 . C2 . -174.3(3) yes C10 . As1 . C8 . C9 . 14.2(3) yes C16 . As1 . C8 . C2 . -65.9(4) yes C16 . As1 . C8 . C9 . 122.6(3) yes C22 . As1 . C8 . C2 . 76.0(4) yes C22 . As1 . C8 . C9 . -95.6(3) yes C8 . As1 . C10 . C11 . -102.2(3) yes C8 . As1 . C10 . C15 . 70.8(3) yes C16 . As1 . C10 . C11 . 133.9(3) yes C16 . As1 . C10 . C15 . -53.0(4) yes C22 . As1 . C10 . C11 . 15.3(4) yes C22 . As1 . C10 . C15 . -171.6(3) yes C8 . As1 . C16 . C17 . -157.7(3) yes C8 . As1 . C16 . C21 . 23.1(5) yes C10 . As1 . C16 . C17 . -49.7(4) yes C10 . As1 . C16 . C21 . 131.1(3) yes C22 . As1 . C16 . C17 . 60.7(4) yes C22 . As1 . C16 . C21 . -118.5(3) yes C8 . As1 . C22 . C23 . -12.9(4) yes C8 . As1 . C22 . C27 . 165.4(3) yes C10 . As1 . C22 . C23 . -120.2(3) yes C10 . As1 . C22 . C27 . 58.1(4) yes C16 . As1 . C22 . C23 . 131.3(3) yes C16 . As1 . C22 . C27 . -50.3(4) yes O1 . C1 . C2 . C3 . 178.6(3) yes O1 . C1 . C2 . C8 . -0.2(3) yes C7 . C1 . C2 . C3 . -0.7(5) yes C7 . C1 . C2 . C8 . -179.5(3) yes O1 . C1 . C7 . C6 . 179.9(3) yes C2 . C1 . C7 . C6 . -0.9(5) yes C1 . C2 . C3 . C4 . 0.9(5) yes C8 . C2 . C3 . C4 . 179.6(3) yes C1 . C2 . C8 . As1 . -2.2(4) yes C1 . C2 . C8 . C9 . 169.0(3) yes C3 . C2 . C8 . As1 . 178.9(2) yes C3 . C2 . C8 . C9 . -9.9(4) yes C2 . C3 . C4 . C5 . 0.3(6) yes C3 . C4 . C5 . C6 . -0.7(6) yes C4 . C5 . C6 . C7 . -0.6(6) yes C5 . C6 . C7 . C1 . 1.7(6) yes As1 . C8 . C9 . N1 . 146.2(5) yes C2 . C8 . C9 . N1 . -25.9(6) yes As1 . C10 . C11 . C12 . 171.5(2) yes C15 . C10 . C11 . C12 . -1.5(4) yes As1 . C10 . C15 . C14 . -171.0(2) yes C11 . C10 . C15 . C14 . 2.1(4) yes C10 . C11 . C12 . C13 . -0.4(4) yes C11 . C12 . C13 . C14 . 1.5(4) yes C12 . C13 . C14 . C15 . -0.9(4) yes C13 . C14 . C15 . C10 . -1.0(4) yes As1 . C16 . C17 . C18 . -176.2(2) yes C21 . C16 . C17 . C18 . 3.0(5) yes As1 . C16 . C21 . C20 . 177.3(2) yes C17 . C16 . C21 . C20 . -1.9(5) yes C16 . C17 . C18 . C19 . -1.8(5) yes C17 . C18 . C19 . C20 . -0.5(5) yes C18 . C19 . C20 . C21 . 1.6(5) yes C19 . C20 . C21 . C16 . -0.4(5) yes As1 . C22 . C23 . C24 . 177.2(2) yes C27 . C22 . C23 . C24 . -1.1(4) yes As1 . C22 . C27 . C26 . -178.2(2) yes C23 . C22 . C27 . C26 . 0.1(4) yes C22 . C23 . C24 . C25 . 2.1(4) yes C23 . C24 . C25 . C26 . -2.2(5) yes C24 . C25 . C26 . C27 . 1.1(5) yes C25 . C26 . C27 . C22 . -0.1(4) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag As1 . O1 . 2.3914(15) yes As1 . C1 . 3.079(2) yes As1 . C2 . 2.919(2) yes As1 . C8 . 1.881(2) yes As1 . C9 . 2.799(2) yes As1 . C10 . 1.945(2) yes As1 . C11 . 2.927(2) yes As1 . C15 . 2.879(2) yes As1 . C16 . 1.9376(19) yes As1 . C17 . 2.858(2) yes As1 . C21 . 2.923(2) yes As1 . C22 . 1.9297(18) yes As1 . C23 . 2.8685(18) yes As1 . C27 . 2.897(2) yes As1 . H6 . 2.937(7) no As1 . H10 . 2.864(9) no As1 . H11 . 3.03(1) no As1 . H15 . 3.09(1) no As1 . H16 . 3.064(9) no As1 . H21 . 3.012(9) no O1 . C1 . 1.260(3) yes O1 . C2 . 2.318(3) yes O1 . C7 . 2.315(3) yes O1 . C8 . 2.601(2) yes O1 . C12 2_657 3.404(3) yes O1 . C16 . 2.818(2) yes O1 . C21 . 2.830(3) yes O1 . C22 . 2.860(2) yes O1 . C23 . 2.993(3) yes O1 . H2 2_556 3.29(3) no O1 . H5 . 2.427(9) no O1 . H6 . 2.48(1) no O1 . H13 2_657 3.31(4) no O1 . H14 2_657 2.67(5) no O1 . H21 . 2.842(9) no N1 . C2 . 3.457(3) yes N1 . C3 . 3.503(3) yes N1 . C6 2_546 3.327(3) yes N1 . C8 . 2.563(3) yes N1 . C9 . 1.149(3) yes N1 . C10 . 3.426(3) yes N1 . C15 . 3.566(3) yes N1 . C20 2_646 3.580(3) yes N1 . C26 2_647 3.328(3) yes N1 . C27 2_647 3.181(3) yes N1 . H1 . 2.72(1) no N1 . H4 2_546 2.60(5) no N1 . H7 2_646 2.98(3) no N1 . H10 2_647 3.38(2) no N1 . H16 2_647 2.43(2) no N1 . H17 2_647 2.81(2) no C1 . C2 . 1.466(3) yes C1 . C3 . 2.553(3) yes C1 . C4 . 3.191(3) yes C1 . C5 . 3.212(3) yes C1 . C6 . 2.561(3) yes C1 . C7 . 1.427(3) yes C1 . C8 . 2.410(3) yes C1 . C21 . 3.505(3) yes C1 . C23 . 3.549(3) yes C1 . H1 . 3.40(1) no C1 . H4 . 3.33(2) no C1 . H5 . 2.081(7) no C1 . H6 . 2.85(1) no C1 . H11 1_455 3.50(2) no C1 . H12 1_455 3.59(3) no C1 . H18 1_554 2.99(2) no C1 . H21 . 3.014(9) no C2 . C3 . 1.406(3) yes C2 . C4 . 2.548(3) yes C2 . C5 . 3.202(3) yes C2 . C6 . 3.179(3) yes C2 . C7 . 2.565(3) yes C2 . C8 . 1.407(3) yes C2 . C9 . 2.436(3) yes C2 . H1 . 2.023(6) no C2 . H2 . 3.47(2) no C2 . H5 . 3.46(1) no C2 . H6 . 3.25(1) no C2 . H12 1_455 2.91(3) no C2 . H18 1_554 3.17(2) no C2 . H21 . 3.05(1) no C3 . C4 . 1.380(3) yes C3 . C5 . 2.499(3) yes C3 . C6 . 3.082(3) yes C3 . C7 . 3.099(3) yes C3 . C8 . 2.441(3) yes C3 . C9 . 2.822(3) yes C3 . H1 . 1.039(3) no C3 . H2 . 2.150(9) no C3 . H3 . 3.31(2) no C3 . H5 2_546 3.23(1) no C3 . H8 2_646 3.38(3) no C3 . H11 1_455 3.55(3) no C3 . H12 1_455 2.74(5) no C3 . H18 1_554 3.27(3) no C4 . C5 . 1.388(3) yes C4 . C6 . 2.469(4) yes C4 . C7 . 3.105(3) yes C4 . H1 . 2.068(7) no C4 . H2 . 1.016(3) no C4 . H3 . 2.014(8) no C4 . H4 . 3.24(1) no C4 . H5 2_546 3.41(1) no C4 . H7 2_546 3.54(3) no C4 . H11 1_455 3.39(5) no C4 . H12 1_455 3.25(7) no C4 . H14 1_454 3.3(1) no C4 . H18 1_554 3.29(5) no C4 . H19 1_554 3.56(2) no C5 . C6 . 1.373(3) yes C5 . C7 . 2.506(4) yes C5 . H1 . 3.38(1) no C5 . H2 . 1.905(7) no C5 . H3 . 0.955(3) no C5 . H4 . 1.942(7) no C5 . H5 . 3.43(1) no C5 . H7 2_546 3.48(3) no C5 . H11 1_455 3.21(6) no C5 . H15 1_454 3.5(1) no C5 . H18 1_554 3.16(7) no C5 . H19 1_554 3.31(3) no C6 . C7 . 1.388(3) yes C6 . H1 2_556 3.56(1) no C6 . H2 . 3.22(1) no C6 . H3 . 1.984(7) no C6 . H4 . 0.927(3) no C6 . H5 . 2.127(7) no C6 . H11 1_455 3.14(5) no C6 . H18 1_554 2.96(6) no C7 . H1 2_556 3.17(1) no C7 . H3 . 3.30(2) no C7 . H4 . 1.976(8) no C7 . H5 . 1.086(3) no C7 . H11 1_455 3.25(3) no C7 . H18 1_554 2.89(4) no C8 . C9 . 1.416(3) yes C8 . C10 . 2.926(3) yes C8 . C15 . 3.462(3) yes C8 . C16 . 3.317(3) yes C8 . C22 . 3.191(3) yes C8 . C23 . 3.400(3) yes C8 . H1 . 2.500(9) no C8 . H6 . 3.23(1) no C8 . H11 . 3.48(1) no C8 . H12 1_455 3.36(2) no C8 . H21 . 2.91(1) no C9 . C10 . 2.918(3) yes C9 . C11 . 3.571(3) yes C9 . C15 . 3.247(3) yes C9 . H1 . 2.32(1) no C9 . H4 2_546 3.46(4) no C9 . H7 2_646 3.07(2) no C9 . H11 . 3.42(1) no C9 . H12 1_455 3.47(1) no C9 . H16 2_647 3.45(2) no C10 . C11 . 1.397(3) yes C10 . C12 . 2.406(3) yes C10 . C13 . 2.782(3) yes C10 . C14 . 2.405(3) yes C10 . C15 . 1.397(3) yes C10 . C16 . 2.984(3) yes C10 . C17 . 3.272(3) yes C10 . C22 . 3.047(3) yes C10 . C27 . 3.498(3) yes C10 . H10 . 2.893(9) no C10 . H11 . 2.040(8) no C10 . H12 . 3.31(1) no C10 . H14 . 3.22(1) no C10 . H15 . 2.190(7) no C10 . H16 . 3.36(1) no C10 . H19 1_655 3.58(4) no C11 . C12 . 1.388(3) yes C11 . C13 . 2.409(3) yes C11 . C14 . 2.785(3) yes C11 . C15 . 2.421(3) yes C11 . C18 2_647 3.509(3) yes C11 . C22 . 3.229(3) yes C11 . C27 . 3.382(3) yes C11 . H3 1_656 3.2(1) no C11 . H10 . 3.59(1) no C11 . H11 . 3.23(1) no C11 . H13 . 3.30(1) no C11 . H14 . 2.007(7) no C11 . H15 . 1.104(4) no C11 . H16 . 3.32(1) no C11 . H19 1_655 3.29(2) no C12 . C13 . 1.386(3) yes C12 . C14 . 2.408(3) yes C12 . C15 . 2.782(3) yes C12 . C16 2_647 3.565(3) yes C12 . H2 1_656 3.1(1) no C12 . H3 1_656 3.4(2) no C12 . H12 . 3.32(2) no C12 . H13 . 2.088(8) no C12 . H14 . 0.880(3) no C12 . H15 . 2.146(7) no C12 . H19 1_655 3.17(3) no C13 . C14 . 1.399(3) yes C13 . C15 . 2.412(3) yes C13 . C22 2_647 3.567(3) yes C13 . C26 2_647 3.498(3) yes C13 . C27 2_647 3.407(3) yes C13 . H9 2_747 3.10(2) no C13 . H11 . 3.14(1) no C13 . H12 . 2.098(8) no C13 . H13 . 0.959(3) no C13 . H14 . 1.946(8) no C13 . H15 . 3.40(1) no C13 . H19 1_655 3.36(4) no C13 . H21 1_655 3.02(2) no C14 . C15 . 1.383(3) yes C14 . C26 2_647 3.546(3) yes C14 . H11 . 1.887(6) no C14 . H12 . 1.002(4) no C14 . H13 . 2.003(7) no C14 . H14 . 3.18(1) no C14 . H17 2_647 3.49(5) no C14 . H21 1_655 2.65(2) no C15 . C16 . 3.323(3) yes C15 . C17 . 3.560(3) yes C15 . H10 . 3.37(1) no C15 . H11 . 0.860(3) no C15 . H12 . 2.062(6) no C15 . H13 . 3.24(1) no C15 . H15 . 3.43(2) no C15 . H21 1_655 3.13(2) no C16 . C17 . 1.391(3) yes C16 . C18 . 2.397(3) yes C16 . C19 . 2.771(3) yes C16 . C20 . 2.390(3) yes C16 . C21 . 1.389(3) yes C16 . C22 . 3.253(3) yes C16 . H6 . 1.970(8) no C16 . H7 . 3.20(1) no C16 . H9 . 3.27(1) no C16 . H10 . 2.018(8) no C16 . H11 . 3.084(9) no C16 . H14 2_657 3.02(3) no C16 . H16 . 3.43(1) no C17 . C18 . 1.384(3) yes C17 . C19 . 2.404(3) yes C17 . C20 . 2.771(4) yes C17 . C21 . 2.415(3) yes C17 . H5 1_655 3.47(4) no C17 . H6 . 3.21(2) no C17 . H8 . 3.51(1) no C17 . H9 . 2.060(7) no C17 . H10 . 0.949(3) no C17 . H11 . 3.43(1) no C17 . H14 2_657 3.41(2) no C17 . H15 2_657 3.42(2) no C17 . H16 . 3.03(1) no C18 . C19 . 1.386(4) yes C18 . C20 . 2.396(4) yes C18 . C21 . 2.779(3) yes C18 . H5 1_655 2.92(4) no C18 . H7 . 3.11(2) no C18 . H8 . 2.343(9) no C18 . H9 . 0.948(3) no C18 . H10 . 2.058(7) no C18 . H13 2_757 3.33(2) no C18 . H15 2_657 2.89(2) no C19 . C20 . 1.388(4) yes C19 . C21 . 2.409(4) yes C19 . H1 2_656 3.27(3) no C19 . H3 2_556 3.49(8) no C19 . H5 1_655 2.77(3) no C19 . H6 . 3.26(1) no C19 . H7 . 1.872(9) no C19 . H8 . 1.217(4) no C19 . H9 . 1.998(9) no C19 . H10 . 3.27(1) no C19 . H15 2_657 2.88(3) no C20 . C21 . 1.383(3) yes C20 . H2 2_556 3.19(4) no C20 . H3 2_556 3.28(5) no C20 . H4 1_655 3.05(4) no C20 . H5 1_655 3.19(2) no C20 . H6 . 2.052(7) no C20 . H7 . 0.855(3) no C20 . H8 . 2.087(7) no C20 . H9 . 3.23(2) no C20 . H14 2_657 3.49(4) no C20 . H15 2_657 3.42(2) no C20 . H17 1_554 3.22(4) no C21 . H2 2_556 3.20(4) no C21 . H4 1_655 3.16(4) no C21 . H6 . 0.919(3) no C21 . H7 . 2.026(7) no C21 . H8 . 3.35(1) no C21 . H10 . 3.26(2) no C21 . H14 2_657 3.09(4) no C21 . H17 1_554 3.07(2) no C22 . C23 . 1.397(3) yes C22 . C24 . 2.406(3) yes C22 . C25 . 2.770(3) yes C22 . C26 . 2.391(3) yes C22 . C27 . 1.385(3) yes C22 . H10 . 3.43(1) no C22 . H13 2_657 3.18(2) no C22 . H15 . 2.695(9) no C22 . H16 . 2.123(8) no C22 . H17 . 3.33(1) no C22 . H19 . 3.19(1) no C22 . H21 . 2.161(7) no C23 . C24 . 1.388(3) yes C23 . C25 . 2.407(3) yes C23 . C26 . 2.777(3) yes C23 . C27 . 2.418(3) yes C23 . H9 2_647 3.14(3) no C23 . H13 2_657 3.11(2) no C23 . H15 . 3.50(1) no C23 . H16 . 3.35(1) no C23 . H18 . 3.41(1) no C23 . H19 . 1.951(7) no C23 . H21 . 1.046(3) no C24 . C25 . 1.393(3) yes C24 . C26 . 2.408(3) yes C24 . C27 . 2.789(3) yes C24 . H8 2_647 3.29(7) no C24 . H9 2_647 3.34(5) no C24 . H13 2_657 3.16(4) no C24 . H17 . 3.30(2) no C24 . H18 . 2.187(7) no C24 . H19 . 0.903(3) no C24 . H21 . 2.073(6) no C25 . C26 . 1.389(3) yes C25 . C27 . 2.410(3) yes C25 . H8 2_647 2.91(7) no C25 . H12 2_657 3.56(8) no C25 . H13 2_657 3.24(5) no C25 . H16 . 3.29(1) no C25 . H17 . 2.053(7) no C25 . H18 . 1.080(4) no C25 . H19 . 2.042(8) no C25 . H21 . 3.33(1) no C26 . C27 . 1.386(3) yes C26 . H3 1_656 3.5(1) no C26 . H4 1_656 3.5(1) no C26 . H6 1_556 3.33(2) no C26 . H8 2_647 2.95(5) no C26 . H12 2_657 3.57(6) no C26 . H13 2_657 3.31(4) no C26 . H15 . 3.44(1) no C26 . H16 . 2.037(8) no C26 . H17 . 1.020(3) no C26 . H18 . 2.101(9) no C26 . H19 . 3.24(1) no C27 . H3 1_656 3.4(1) no C27 . H8 2_647 3.39(4) no C27 . H10 . 3.12(1) no C27 . H13 2_657 3.28(3) no C27 . H15 . 2.665(8) no C27 . H16 . 1.005(3) no C27 . H17 . 2.119(6) no C27 . H18 . 3.36(2) no C27 . H21 . 3.38(2) no #========================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #========================================================================== # End of CIF #==========================================================================