# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1752 data_rphalh2 #------------------------------------------------------------------------------ _audit_creation_date '19100-08-23' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' ENTER CONTACT NAME HERE' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.3949(2) _cell_length_b 13.7790(3) _cell_length_c 14.2939(3) _cell_angle_alpha 90 _cell_angle_beta 99.330(2) _cell_angle_gamma 90 _cell_volume 1825.90(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 598.96 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H54 Al2 N2 P2 Si4 ' _chemical_formula_moiety 'C24 H54 Al2 N2 P2 Si4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 648.00 _exptl_absorpt_coefficient_mu 0.314 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'unknown' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4510 _reflns_number_total 12947 _reflns_number_gt 3554 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 35.41 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 108 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Al 0 4 0.056 0.052 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si 0 8 0.072 0.071 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom P(1) 0.61610(6) 0.13655(5) 0.86778(4) 0.0196(2) 1.000 . Uani d ? P(1*) 0.38392(7) -0.13646(5) 1.13221(5) 0.0196(2) 1.000 . Uani d ? Si(1) 0.52294(7) 0.32712(5) 0.77703(5) 0.0182(2) 1.000 . Uani d ? Si(1*) 0.47704(8) -0.32718(5) 1.22295(5) 0.0182(2) 1.000 . Uani d ? Si(2) 0.49581(7) 0.12068(5) 0.65823(5) 0.0188(2) 1.000 . Uani d ? Si(2*) 0.50427(8) -0.12065(5) 1.34176(5) 0.0186(2) 1.000 . Uani d ? Al(1*) 0.54484(8) -0.09272(5) 1.03148(5) 0.0158(2) 1.000 . Uani d ? Al(1) 0.45518(7) 0.09274(5) 0.96855(5) 0.0159(2) 1.000 . Uani d ? N(1) 0.2914(2) 0.1487(1) 0.8723(1) 0.0131(5) 1.000 . Uani d ? N(1*) 0.7086(2) -0.1485(1) 1.1277(1) 0.0134(5) 1.000 . Uani d ? C(1) 0.3214(2) 0.1844(2) 0.7891(2) 0.0154(6) 1.000 . Uani d ? C(1*) 0.6788(3) -0.1845(2) 1.2112(2) 0.0153(6) 1.000 . Uani d ? C(2) 0.2080(2) 0.2185(2) 0.7209(2) 0.0242(7) 1.000 . Uani d ? C(2*) 0.7917(3) -0.2186(2) 1.2789(2) 0.0238(7) 1.000 . Uani d ? C(3) 0.0684(3) 0.2170(2) 0.7386(2) 0.0281(7) 1.000 . Uani d ? C(3*) 0.9313(3) -0.2172(2) 1.2613(2) 0.0278(8) 1.000 . Uani d ? C(4*) 0.9600(3) -0.1806(2) 1.1761(2) 0.0231(7) 1.000 . Uani d ? C(4) 0.0411(2) 0.1807(2) 0.8238(2) 0.0231(7) 1.000 . Uani d ? C(5*) 0.8469(3) -0.1469(2) 1.1109(2) 0.0169(7) 1.000 . Uani d ? C(5) 0.1528(2) 0.1467(2) 0.8889(2) 0.0168(6) 1.000 . Uani d ? C(6*) 0.8750(3) -0.1055(2) 1.0183(2) 0.0243(8) 1.000 . Uani d ? C(6) 0.1249(3) 0.1057(2) 0.9818(2) 0.0244(7) 1.000 . Uani d ? C(7*) 0.5921(3) -0.4031(2) 1.3139(2) 0.0321(8) 1.000 . Uani d ? C(7) 0.4081(3) 0.4032(2) 0.6863(2) 0.0323(8) 1.000 . Uani d ? C(8*) 0.6062(4) -0.1700(3) 1.4558(2) 0.041(1) 1.000 . Uani d ? C(8) 0.3937(3) 0.1698(2) 0.5445(2) 0.0409(9) 1.000 . Uani d ? C(9) 0.7150(3) 0.3482(2) 0.7633(2) 0.0257(7) 1.000 . Uani d ? C(9*) 0.2851(3) -0.3483(2) 1.2366(2) 0.0252(7) 1.000 . Uani d ? C(10*) 0.3116(3) -0.1154(2) 1.3610(2) 0.0279(8) 1.000 . Uani d ? C(10) 0.6881(3) 0.1152(2) 0.6389(2) 0.0280(7) 1.000 . Uani d ? C(11*) 0.5100(3) -0.3724(2) 1.1049(2) 0.0311(8) 1.000 . Uani d ? C(11) 0.4906(3) 0.3727(2) 0.8950(2) 0.0311(7) 1.000 . Uani d ? C(12*) 0.5247(3) -0.1915(2) 1.2293(2) 0.0146(6) 1.000 . Uani d ? C(12) 0.4754(2) 0.1915(2) 0.7707(2) 0.0147(6) 1.000 . Uani d ? C(13*) 0.5764(3) 0.0037(2) 1.3290(2) 0.0342(9) 1.000 . Uani d ? C(13) 0.4230(3) -0.0036(2) 0.6712(2) 0.0350(8) 1.000 . Uani d ? H(1) 0.2275 0.2427 0.6622 0.029 1.000 . Uiso c ? H(1*) 0.7719 -0.2429 1.3376 0.029 1.000 . Uiso c ? H(2) -0.0080 0.2410 0.6928 0.034 1.000 . Uiso c ? H(2*) 1.0076 -0.2412 1.3073 0.033 1.000 . Uiso c ? H(3*) 1.0558 -0.1787 1.1629 0.028 1.000 . Uiso c ? H(3) -0.0550 0.1789 0.8368 0.028 1.000 . Uiso c ? H(4*) 0.9752 -0.1089 1.0157 0.029 1.000 . Uiso c ? H(4) 0.0246 0.1091 0.9845 0.029 1.000 . Uiso c ? H(5*) 0.8229 -0.1416 0.9674 0.029 1.000 . Uiso c ? H(5) 0.1769 0.1420 1.0326 0.029 1.000 . Uiso c ? H(6*) 0.8445 -0.0396 1.0135 0.029 1.000 . Uiso c ? H(6) 0.1553 0.0398 0.9868 0.029 1.000 . Uiso c ? H(7*) 0.6906 -0.3954 1.3075 0.038 1.000 . Uiso c ? H(7) 0.3095 0.3954 0.6927 0.039 1.000 . Uiso c ? H(8*) 0.5655 -0.4694 1.3048 0.038 1.000 . Uiso c ? H(8) 0.4346 0.4693 0.6955 0.039 1.000 . Uiso c ? H(9*) 0.5787 -0.3832 1.3754 0.038 1.000 . Uiso c ? H(9) 0.4213 0.3832 0.6247 0.039 1.000 . Uiso c ? H(10*) 0.7058 -0.1746 1.4512 0.050 1.000 . Uiso c ? H(10) 0.2946 0.1745 0.5492 0.049 1.000 . Uiso c ? H(11*) 0.5703 -0.2326 1.4673 0.050 1.000 . Uiso c ? H(11) 0.4301 0.2325 0.5331 0.049 1.000 . Uiso c ? H(12*) 0.5942 -0.1278 1.5065 0.050 1.000 . Uiso c ? H(12) 0.4061 0.1278 0.4938 0.049 1.000 . Uiso c ? H(13) 0.7380 0.4148 0.7736 0.032 1.000 . Uiso c ? H(13*) 0.2622 -0.4150 1.2263 0.030 1.000 . Uiso c ? H(14) 0.7282 0.3303 0.7011 0.032 1.000 . Uiso c ? H(14*) 0.2719 -0.3305 1.2988 0.030 1.000 . Uiso c ? H(15) 0.7763 0.3100 0.8083 0.032 1.000 . Uiso c ? H(15*) 0.2238 -0.3101 1.1916 0.030 1.000 . Uiso c ? H(16*) 0.2798 -0.1787 1.3737 0.033 1.000 . Uiso c ? H(16) 0.7198 0.1784 0.6262 0.034 1.000 . Uiso c ? H(17*) 0.3043 -0.0742 1.4133 0.033 1.000 . Uiso c ? H(17) 0.6948 0.0739 0.5865 0.034 1.000 . Uiso c ? H(18*) 0.2532 -0.0904 1.3057 0.033 1.000 . Uiso c ? H(18) 0.7462 0.0900 0.6941 0.034 1.000 . Uiso c ? H(19*) 0.5615 0.0422 1.3817 0.041 1.000 . Uiso c ? H(19) 0.4375 -0.0423 0.6185 0.043 1.000 . Uiso c ? H(20*) 0.5277 0.0323 1.2722 0.041 1.000 . Uiso c ? H(20) 0.4715 -0.0323 0.7280 0.043 1.000 . Uiso c ? H(21*) 0.6767 0.0000 1.3265 0.041 1.000 . Uiso c ? H(21) 0.3227 0.0003 0.6737 0.043 1.000 . Uiso c ? H(22) 0.5477 0.3363 0.9439 0.038 1.000 . Uiso c ? H(22*) 0.4537 -0.3358 1.0560 0.037 1.000 . Uiso c ? H(23) 0.3918 0.3655 0.8998 0.038 1.000 . Uiso c ? H(23*) 0.6093 -0.3654 1.1005 0.037 1.000 . Uiso c ? H(24) 0.5170 0.4392 0.9014 0.038 1.000 . Uiso c ? H(24*) 0.4838 -0.4389 1.0982 0.037 1.000 . Uiso c ? H(25) 0.6277 0.0489 0.8355 0.030 1.000 . Uiso c ? H(25*) 0.3723 -0.0489 1.1645 0.030 1.000 . Uiso c ? H(26) 0.4363 0.1548 1.0631 0.030 1.000 . Uiso c ? H(26*) 0.5637 -0.1548 0.9369 0.030 1.000 . Uiso c ? H(27) 0.3899 -0.0200 0.9566 0.030 1.000 . Uiso c ? H(27*) 0.6101 0.0200 1.0434 0.030 1.000 . Uiso c ? H(29) 0.2823 -0.1293 1.1268 0.023 1.000 . Uiso c ? H(30) 0.5374 -0.0621 0.9714 0.019 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P(1) 0.0114(3) 0.0260(4) 0.0205(3) 0.0027(3) -0.0001(2) 0.0100(3) P(1*) 0.0112(3) 0.0261(4) 0.0204(4) 0.0024(3) -0.0001(3) 0.0103(3) Si(1) 0.0165(3) 0.0159(3) 0.0225(4) 0.0017(3) 0.0039(3) 0.0040(3) Si(1*) 0.0167(4) 0.0157(4) 0.0224(4) 0.0017(3) 0.0038(3) 0.0039(3) Si(2) 0.0157(3) 0.0221(3) 0.0184(4) -0.0005(3) 0.0023(3) -0.0002(3) Si(2*) 0.0156(4) 0.0218(4) 0.0181(4) -0.0003(3) 0.0022(3) -0.0003(3) Al(1*) 0.0197(4) 0.0158(4) 0.0110(4) -0.0022(3) 0.0001(3) 0.0014(3) Al(1) 0.0196(4) 0.0171(3) 0.0104(4) -0.0020(3) 0.0000(3) 0.0028(3) N(1) 0.0132(9) 0.0123(9) 0.014(1) -0.0011(8) 0.0032(7) -0.0006(7) N(1*) 0.013(1) 0.013(1) 0.014(1) -0.0016(9) 0.0034(8) -0.0005(8) C(1) 0.014(1) 0.015(1) 0.017(1) 0.0002(9) 0.0026(9) 0.0017(9) C(1*) 0.014(1) 0.015(1) 0.017(1) 0.001(1) 0.003(1) 0.002(1) C(2) 0.017(1) 0.034(1) 0.021(1) 0.004(1) 0.003(1) 0.013(1) C(2*) 0.017(1) 0.033(2) 0.022(2) 0.002(1) 0.003(1) 0.013(1) C(3) 0.014(1) 0.037(1) 0.032(2) 0.002(1) -0.001(1) 0.012(1) C(3*) 0.015(1) 0.037(2) 0.030(2) 0.003(1) 0.000(1) 0.011(1) C(4*) 0.015(1) 0.026(1) 0.029(2) 0.000(1) 0.007(1) 0.002(1) C(4) 0.010(1) 0.028(1) 0.033(1) -0.001(1) 0.009(1) 0.002(1) C(5*) 0.017(1) 0.013(1) 0.023(1) -0.001(1) 0.007(1) -0.003(1) C(5) 0.018(1) 0.013(1) 0.021(1) -0.001(1) 0.0075(9) -0.0026(9) C(6*) 0.024(1) 0.029(2) 0.022(2) -0.002(1) 0.012(1) 0.000(1) C(6) 0.024(1) 0.030(1) 0.023(1) -0.002(1) 0.012(1) -0.001(1) C(7*) 0.033(2) 0.024(2) 0.040(2) 0.006(1) 0.007(1) 0.014(1) C(7) 0.033(2) 0.024(1) 0.040(2) 0.006(1) 0.007(1) 0.013(1) C(8*) 0.045(2) 0.056(2) 0.021(2) 0.009(2) -0.002(1) -0.005(1) C(8) 0.044(2) 0.055(2) 0.021(2) 0.009(2) -0.002(1) -0.005(1) C(9) 0.024(1) 0.020(1) 0.033(2) -0.005(1) 0.006(1) 0.004(1) C(9*) 0.023(1) 0.021(1) 0.032(2) -0.005(1) 0.005(1) 0.003(1) C(10*) 0.023(1) 0.034(2) 0.029(2) -0.003(1) 0.010(1) -0.004(1) C(10) 0.024(1) 0.033(1) 0.029(2) -0.003(1) 0.010(1) -0.005(1) C(11*) 0.032(2) 0.028(2) 0.033(2) -0.001(1) 0.006(1) -0.007(1) C(11) 0.033(1) 0.028(1) 0.033(2) 0.000(1) 0.007(1) -0.007(1) C(12*) 0.012(1) 0.018(1) 0.013(1) 0.002(1) 0.001(1) 0.006(1) C(12) 0.013(1) 0.017(1) 0.014(1) 0.0023(9) 0.0013(9) 0.0055(9) C(13*) 0.028(2) 0.028(2) 0.048(2) -0.005(1) 0.011(1) -0.010(1) C(13) 0.030(1) 0.028(1) 0.048(2) -0.005(1) 0.011(1) -0.010(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3554 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_all 0.0557 _refine_ls_wR_factor_ref 0.0512 _refine_ls_goodness_of_fit_all 3.242 _refine_ls_goodness_of_fit_ref 2.823 _refine_ls_shift/su_max 0.0051 _refine_ls_shift/su_mean 0.1342 _refine_diff_density_min -1.05 _refine_diff_density_max 0.42 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P(1) Al(1) 2.3304(1) . . yes P(1) C(12) 1.913(2) . . yes P(1) H(25) 1.303 . . no Si(1) C(7) 1.868(3) . . yes Si(1) C(9) 1.869(2) . . yes Si(1) C(11) 1.870(3) . . yes Si(1) C(12) 1.920(2) . . yes Si(2) C(8) 1.875(3) . . yes Si(2) C(10) 1.873(2) . . yes Si(2) C(12) 1.917(2) . . yes Si(2) C(13) 1.865(3) . . yes Al(1) N(1) 2.040(2) . . yes Al(1) H(26) 1.633 . . no Al(1) H(27) 1.668 . . no N(1) C(1) 1.359(3) . . yes N(1) C(5) 1.361(3) . . yes C(1) C(2) 1.403(3) . . yes C(1) C(12) 1.515(3) . . yes C(2) C(3) 1.376(3) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.379(4) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.367(3) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.505(3) . . yes C(6) H(4) 0.95 . . no C(6) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) H(7) 0.95 . . no C(7) H(8) 0.95 . . no C(7) H(9) 0.95 . . no C(8) H(10) 0.95 . . no C(8) H(11) 0.95 . . no C(8) H(12) 0.95 . . no C(9) H(13) 0.95 . . no C(9) H(14) 0.95 . . no C(9) H(15) 0.95 . . no C(10) H(16) 0.95 . . no C(10) H(17) 0.95 . . no C(10) H(18) 0.95 . . no C(11) H(22) 0.95 . . no C(11) H(23) 0.95 . . no C(11) H(24) 0.95 . . no C(13) H(19) 0.95 . . no C(13) H(20) 0.95 . . no C(13) H(21) 0.95 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Al(1) P(1) C(12) 96.29(8) . . . yes Al(1) P(1) H(25) 94.6 . . . no C(12) P(1) H(25) 101.4 . . . no C(7) Si(1) C(9) 107.4(1) . . . yes C(7) Si(1) C(11) 106.1(1) . . . yes C(7) Si(1) C(12) 114.2(1) . . . yes C(9) Si(1) C(11) 110.0(1) . . . yes C(9) Si(1) C(12) 111.6(1) . . . yes C(11) Si(1) C(12) 107.4(1) . . . yes C(8) Si(2) C(10) 104.9(1) . . . yes C(8) Si(2) C(12) 115.9(1) . . . yes C(8) Si(2) C(13) 105.9(1) . . . yes C(10) Si(2) C(12) 112.0(1) . . . yes C(10) Si(2) C(13) 110.8(1) . . . yes C(12) Si(2) C(13) 107.2(1) . . . yes P(1) Al(1) N(1) 88.85(6) . . . yes P(1) Al(1) H(26) 123.0 . . . no P(1) Al(1) H(27) 116.2 . . . no N(1) Al(1) H(26) 100.9 . . . no N(1) Al(1) H(27) 93.3 . . . no H(26) Al(1) H(27) 119.0 . . . no Al(1) N(1) C(1) 119.2(2) . . . yes Al(1) N(1) C(5) 120.9(2) . . . yes C(1) N(1) C(5) 119.9(2) . . . yes N(1) C(1) C(2) 119.2(2) . . . yes N(1) C(1) C(12) 120.9(2) . . . yes C(2) C(1) C(12) 119.8(2) . . . yes C(1) C(2) C(3) 120.4(2) . . . yes C(1) C(2) H(1) 119.9 . . . no C(3) C(2) H(1) 119.7 . . . no C(2) C(3) C(4) 119.2(2) . . . yes C(2) C(3) H(2) 120.3 . . . no C(4) C(3) H(2) 120.5 . . . no C(3) C(4) C(5) 119.6(2) . . . yes C(3) C(4) H(3) 120.0 . . . no C(5) C(4) H(3) 120.4 . . . no N(1) C(5) C(4) 121.7(2) . . . yes N(1) C(5) C(6) 118.0(2) . . . yes C(4) C(5) C(6) 120.3(2) . . . yes C(5) C(6) H(4) 109.4 . . . no C(5) C(6) H(5) 109.6 . . . no C(5) C(6) H(6) 109.4 . . . no H(4) C(6) H(5) 109.5 . . . no H(4) C(6) H(6) 109.4 . . . no H(5) C(6) H(6) 109.5 . . . no Si(1) C(7) H(7) 109.3 . . . no Si(1) C(7) H(8) 109.5 . . . no Si(1) C(7) H(9) 109.5 . . . no H(7) C(7) H(8) 109.4 . . . no H(7) C(7) H(9) 109.4 . . . no H(8) C(7) H(9) 109.7 . . . no Si(2) C(8) H(10) 109.5 . . . no Si(2) C(8) H(11) 109.2 . . . no Si(2) C(8) H(12) 109.4 . . . no H(10) C(8) H(11) 109.5 . . . no H(10) C(8) H(12) 109.9 . . . no H(11) C(8) H(12) 109.3 . . . no Si(1) C(9) H(13) 109.5 . . . no Si(1) C(9) H(14) 109.4 . . . no Si(1) C(9) H(15) 109.5 . . . no H(13) C(9) H(14) 109.5 . . . no H(13) C(9) H(15) 109.5 . . . no H(14) C(9) H(15) 109.4 . . . no Si(2) C(10) H(16) 109.4 . . . no Si(2) C(10) H(17) 109.2 . . . no Si(2) C(10) H(18) 109.3 . . . no H(16) C(10) H(17) 109.7 . . . no H(16) C(10) H(18) 109.8 . . . no H(17) C(10) H(18) 109.6 . . . no Si(1) C(11) H(22) 109.3 . . . no Si(1) C(11) H(23) 109.5 . . . no Si(1) C(11) H(24) 109.4 . . . no H(22) C(11) H(23) 109.5 . . . no H(22) C(11) H(24) 109.3 . . . no H(23) C(11) H(24) 109.8 . . . no P(1) C(12) Si(1) 102.9(1) . . . yes P(1) C(12) Si(2) 104.8(1) . . . yes P(1) C(12) C(1) 114.6(1) . . . yes Si(1) C(12) Si(2) 118.7(1) . . . yes Si(1) C(12) C(1) 106.0(1) . . . yes Si(2) C(12) C(1) 109.9(1) . . . yes Si(2) C(13) H(19) 109.5 . . . no Si(2) C(13) H(20) 109.5 . . . no Si(2) C(13) H(21) 109.5 . . . no H(19) C(13) H(20) 109.5 . . . no H(19) C(13) H(21) 109.4 . . . no H(20) C(13) H(21) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(5) C(7) 3.542(3) . 2_546 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag P(1) Al(1) N(1) C(1) . . . . 3.0(2) no P(1) Al(1) N(1) C(5) . . . . -179.9(2) no P(1) C(12) Si(1) C(7) . . . . 177.7(1) no P(1) C(12) Si(1) C(9) . . . . 55.7(1) no P(1) C(12) Si(1) C(11) . . . . -64.9(1) no P(1) C(12) Si(2) C(8) . . . . -170.4(1) no P(1) C(12) Si(2) C(10) . . . . -50.1(1) no P(1) C(12) Si(2) C(13) . . . . 71.7(1) no P(1) C(12) C(1) N(1) . . . . 5.1(3) no P(1) C(12) C(1) C(2) . . . . -177.3(2) no Si(1) C(12) P(1) Al(1) . . . . 112.30(9) no Si(1) C(12) Si(2) C(8) . . . . -56.2(2) no Si(1) C(12) Si(2) C(10) . . . . 64.0(2) no Si(1) C(12) Si(2) C(13) . . . . -174.2(1) no Si(1) C(12) C(1) N(1) . . . . -107.6(2) no Si(1) C(12) C(1) C(2) . . . . 70.0(2) no Si(2) C(12) P(1) Al(1) . . . . -122.87(9) no Si(2) C(12) Si(1) C(7) . . . . 62.5(2) no Si(2) C(12) Si(1) C(9) . . . . -59.4(2) no Si(2) C(12) Si(1) C(11) . . . . 179.9(1) no Si(2) C(12) C(1) N(1) . . . . 122.9(2) no Si(2) C(12) C(1) C(2) . . . . -59.5(2) no Al(1) P(1) C(12) C(1) . . . . -2.3(2) no Al(1) N(1) C(1) C(2) . . . . 176.9(2) no Al(1) N(1) C(1) C(12) . . . . -5.5(3) no Al(1) N(1) C(5) C(4) . . . . -177.7(2) no Al(1) N(1) C(5) C(6) . . . . 2.3(3) no N(1) Al(1) P(1) C(12) . . . . -0.14(9) no N(1) C(1) C(2) C(3) . . . . 0.9(4) no N(1) C(5) C(4) C(3) . . . . 0.7(4) no C(1) N(1) C(5) C(4) . . . . -0.5(3) no C(1) N(1) C(5) C(6) . . . . 179.5(2) no C(1) C(2) C(3) C(4) . . . . -0.7(4) no C(1) C(12) Si(1) C(7) . . . . -61.6(2) no C(1) C(12) Si(1) C(9) . . . . 176.4(1) no C(1) C(12) Si(1) C(11) . . . . 55.7(2) no C(1) C(12) Si(2) C(8) . . . . 66.0(2) no C(1) C(12) Si(2) C(10) . . . . -173.8(1) no C(1) C(12) Si(2) C(13) . . . . -52.0(2) no C(2) C(1) N(1) C(5) . . . . -0.3(3) no C(2) C(3) C(4) C(5) . . . . -0.1(4) no C(3) C(2) C(1) C(12) . . . . -176.7(2) no C(3) C(4) C(5) C(6) . . . . -179.3(2) no C(5) N(1) C(1) C(12) . . . . 177.3(2) no #------------------------------------------------------------------------------ data_rash2 #------------------------------------------------------------------------------ _audit_creation_date '19100-03-03' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' ENTER CONTACT NAME HERE' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.4334(2) _cell_length_b 13.7645(3) _cell_length_c 14.4634(2) _cell_angle_alpha 90 _cell_angle_beta 99.734(1) _cell_angle_gamma 90 _cell_volume 1850.97(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 355.44 _chemical_formula_analytical ? _chemical_formula_sum 'C13 H27 Al As N Si2 ' _chemical_formula_moiety 'C13 H27 Al As N Si2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 744.00 _exptl_absorpt_coefficient_mu 2.000 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'unknown' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 5445 _reflns_number_total 6178 _reflns_number_gt 4150 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As 0 4 -0.030 2.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si 0 8 0.072 0.071 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 52 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 108 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Al 0 4 0.056 0.052 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom As(1) 0.13077(2) 0.13593(1) 0.37010(1) 0.02354(6) 1.000 . Uani d ? As(1*) -0.13077(2) -0.13593(1) 0.62990(1) 0.02354(6) 1.000 . Uani d ? Si(1) 0.02602(5) 0.32761(4) 0.27057(3) 0.0199(1) 1.000 . Uani d ? Si(1*) -0.02602(5) -0.32761(4) 0.72943(3) 0.0199(1) 1.000 . Uani d ? Si(2) -0.00368(5) 0.11786(4) 0.15825(3) 0.0210(1) 1.000 . Uani d ? Si(2*) 0.00368(5) -0.11786(4) 0.84175(3) 0.0210(1) 1.000 . Uani d ? Al(1*) 0.04467(6) -0.09325(4) 0.53268(3) 0.0173(1) 1.000 . Uani d ? Al(1) -0.04467(6) 0.09325(4) 0.46732(3) 0.0173(1) 1.000 . Uani d ? N(1) -0.2043(1) 0.15025(9) 0.36922(9) 0.0144(3) 1.000 . Uani d ? N(1*) 0.2043(1) -0.15025(9) 0.63078(9) 0.0144(3) 1.000 . Uani d ? C(1) -0.3424(2) 0.1493(1) 0.3852(1) 0.0182(4) 1.000 . Uani d ? C(1*) 0.3424(2) -0.1493(1) 0.6148(1) 0.0182(4) 1.000 . Uani d ? C(2) -0.4550(2) 0.1831(1) 0.3196(1) 0.0259(5) 1.000 . Uani d ? C(2*) 0.4550(2) -0.1831(1) 0.6804(1) 0.0259(5) 1.000 . Uani d ? C(3) -0.4266(2) 0.2187(2) 0.2357(1) 0.0309(5) 1.000 . Uani d ? C(3*) 0.4266(2) -0.2187(2) 0.7643(1) 0.0309(5) 1.000 . Uani d ? C(4*) 0.2877(2) -0.2193(1) 0.7810(1) 0.0266(5) 1.000 . Uani d ? C(4) -0.2877(2) 0.2193(1) 0.2190(1) 0.0266(5) 1.000 . Uani d ? C(5*) 0.1742(2) -0.1856(1) 0.7134(1) 0.0165(4) 1.000 . Uani d ? C(5) -0.1742(2) 0.1856(1) 0.2866(1) 0.0165(4) 1.000 . Uani d ? C(6) -0.3712(2) 0.1095(1) 0.4770(1) 0.0256(5) 1.000 . Uani d ? C(6*) 0.3712(2) -0.1095(1) 0.5230(1) 0.0256(5) 1.000 . Uani d ? C(7) -0.0219(2) 0.1924(1) 0.2673(1) 0.0157(4) 1.000 . Uani d ? C(7*) 0.0219(2) -0.1924(1) 0.7327(1) 0.0157(4) 1.000 . Uani d ? C(8*) 0.0055(2) -0.3771(1) 0.6142(1) 0.0348(6) 1.000 . Uani d ? C(8) -0.0055(2) 0.3771(1) 0.3858(1) 0.0348(6) 1.000 . Uani d ? C(9*) 0.0876(2) -0.4022(1) 0.8215(2) 0.0356(6) 1.000 . Uani d ? C(9) -0.0876(2) 0.4022(1) 0.1785(2) 0.0356(6) 1.000 . Uani d ? C(10*) -0.2174(2) -0.3475(1) 0.7427(1) 0.0290(5) 1.000 . Uani d ? C(10) 0.2174(2) 0.3475(1) 0.2573(1) 0.0290(5) 1.000 . Uani d ? C(11*) 0.1070(3) -0.1637(2) 0.9552(1) 0.0464(7) 1.000 . Uani d ? C(11) -0.1070(3) 0.1637(2) 0.0448(1) 0.0464(7) 1.000 . Uani d ? C(12*) -0.1864(2) -0.1113(1) 0.8625(1) 0.0311(6) 1.000 . Uani d ? C(12) 0.1864(2) 0.1113(1) 0.1375(1) 0.0311(6) 1.000 . Uani d ? C(13*) 0.0757(2) 0.0065(2) 0.8248(2) 0.0376(6) 1.000 . Uani d ? C(13) -0.0757(2) -0.0065(2) 0.1752(2) 0.0376(6) 1.000 . Uani d ? H(1) -0.5506 0.1819 0.3321 0.031 1.000 . Uiso c ? H(1*) 0.5506 -0.1819 0.6679 0.031 1.000 . Uiso c ? H(2) -0.5026 0.2425 0.1897 0.037 1.000 . Uiso c ? H(2*) 0.5026 -0.2425 0.8103 0.037 1.000 . Uiso c ? H(3*) 0.2681 -0.2430 0.8393 0.032 1.000 . Uiso c ? H(3) -0.2681 0.2430 0.1607 0.032 1.000 . Uiso c ? H(4) -0.4713 0.1129 0.4786 0.031 1.000 . Uiso c ? H(4*) 0.4713 -0.1129 0.5214 0.031 1.000 . Uiso c ? H(5) -0.3403 0.0438 0.4832 0.031 1.000 . Uiso c ? H(5*) 0.3403 -0.0438 0.5168 0.031 1.000 . Uiso c ? H(6) -0.3200 0.1468 0.5271 0.031 1.000 . Uiso c ? H(6*) 0.3200 -0.1468 0.4729 0.031 1.000 . Uiso c ? H(7*) -0.0510 -0.3420 0.5646 0.042 1.000 . Uiso c ? H(7) 0.0510 0.3420 0.4354 0.042 1.000 . Uiso c ? H(8*) -0.0207 -0.4438 0.6097 0.042 1.000 . Uiso c ? H(8) 0.0207 0.4438 0.3903 0.042 1.000 . Uiso c ? H(9*) 0.1044 -0.3707 0.6097 0.042 1.000 . Uiso c ? H(9) -0.1044 0.3707 0.3903 0.042 1.000 . Uiso c ? H(10*) 0.0594 -0.4684 0.8144 0.043 1.000 . Uiso c ? H(10) -0.0594 0.4684 0.1856 0.043 1.000 . Uiso c ? H(11*) 0.0754 -0.3800 0.8819 0.043 1.000 . Uiso c ? H(11) -0.0754 0.3800 0.1181 0.043 1.000 . Uiso c ? H(12*) 0.1858 -0.3962 0.8151 0.043 1.000 . Uiso c ? H(12) -0.1858 0.3962 0.1849 0.043 1.000 . Uiso c ? H(13*) -0.2786 -0.3106 0.6967 0.035 1.000 . Uiso c ? H(13) 0.2786 0.3106 0.3033 0.035 1.000 . Uiso c ? H(14*) -0.2306 -0.3274 0.8035 0.035 1.000 . Uiso c ? H(14) 0.2306 0.3274 0.1965 0.035 1.000 . Uiso c ? H(15*) -0.2403 -0.4145 0.7346 0.035 1.000 . Uiso c ? H(15) 0.2403 0.4145 0.2654 0.035 1.000 . Uiso c ? H(16*) 0.0717 -0.2258 0.9686 0.056 1.000 . Uiso c ? H(16) -0.0717 0.2258 0.0314 0.056 1.000 . Uiso c ? H(17*) 0.0959 -0.1198 1.0042 0.056 1.000 . Uiso c ? H(17) -0.0959 0.1198 -0.0042 0.056 1.000 . Uiso c ? H(18*) 0.2060 -0.1686 0.9505 0.056 1.000 . Uiso c ? H(18) -0.2060 0.1686 0.0495 0.056 1.000 . Uiso c ? H(19*) -0.2465 -0.0890 0.8072 0.037 1.000 . Uiso c ? H(19) 0.2465 0.0890 0.1928 0.037 1.000 . Uiso c ? H(20*) -0.1922 -0.0675 0.9125 0.037 1.000 . Uiso c ? H(20) 0.1922 0.0675 0.0875 0.037 1.000 . Uiso c ? H(21*) -0.2169 -0.1739 0.8784 0.037 1.000 . Uiso c ? H(21) 0.2169 0.1739 0.1216 0.037 1.000 . Uiso c ? H(22*) 0.1754 0.0023 0.8221 0.045 1.000 . Uiso c ? H(22) -0.1754 -0.0023 0.1779 0.045 1.000 . Uiso c ? H(23*) 0.0620 0.0469 0.8758 0.045 1.000 . Uiso c ? H(23) -0.0620 -0.0469 0.1242 0.045 1.000 . Uiso c ? H(24*) 0.0261 0.0334 0.7679 0.045 1.000 . Uiso c ? H(24) -0.0261 -0.0334 0.2321 0.045 1.000 . Uiso c ? H(26*) 0.1099 0.0142 0.5431 0.036 1.000 . Uiso c ? H(26) -0.1099 -0.0142 0.4569 0.036 1.000 . Uiso c ? H(27) 0.1389 0.0323 0.3316 0.036 1.000 . Uiso c ? H(27*) -0.1389 -0.0323 0.6684 0.036 1.000 . Uiso c ? H(28) -0.0409 0.0627 0.5266 0.021 1.000 . Uiso c ? H(28*) 0.0409 -0.0627 0.4734 0.021 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0124(1) 0.0327(1) 0.0247(1) 0.00259(8) 0.00075(7) 0.01450(8) As(1*) 0.0124(1) 0.0327(1) 0.0247(1) 0.00259(8) 0.00075(7) 0.01450(8) Si(1) 0.0179(3) 0.0159(3) 0.0263(3) 0.0014(2) 0.0045(2) 0.0038(2) Si(1*) 0.0179(3) 0.0159(3) 0.0263(3) 0.0014(2) 0.0045(2) 0.0038(2) Si(2) 0.0185(3) 0.0217(3) 0.0224(3) -0.0004(2) 0.0024(2) -0.0004(2) Si(2*) 0.0185(3) 0.0217(3) 0.0224(3) -0.0004(2) 0.0024(2) -0.0004(2) Al(1*) 0.0184(3) 0.0185(3) 0.0142(2) -0.0023(2) 0.0008(2) 0.0020(2) Al(1) 0.0184(3) 0.0185(3) 0.0142(2) -0.0023(2) 0.0008(2) 0.0020(2) N(1) 0.0146(7) 0.0125(7) 0.0166(7) -0.0016(5) 0.0039(6) -0.0008(5) N(1*) 0.0146(7) 0.0125(7) 0.0166(7) -0.0016(5) 0.0039(6) -0.0008(5) C(1) 0.0175(9) 0.0149(9) 0.0234(9) -0.0014(7) 0.0072(7) -0.0025(7) C(1*) 0.0175(9) 0.0149(9) 0.0234(9) -0.0014(7) 0.0072(7) -0.0025(7) C(2) 0.0137(9) 0.028(1) 0.037(1) 0.0019(8) 0.0078(8) 0.0061(8) C(2*) 0.0137(9) 0.028(1) 0.037(1) 0.0019(8) 0.0078(8) 0.0061(8) C(3) 0.0146(9) 0.039(1) 0.037(1) 0.0031(8) 0.0002(8) 0.0146(9) C(3*) 0.0146(9) 0.039(1) 0.037(1) 0.0031(8) 0.0002(8) 0.0146(9) C(4*) 0.018(1) 0.035(1) 0.027(1) 0.0016(8) 0.0031(8) 0.0144(8) C(4) 0.018(1) 0.035(1) 0.027(1) 0.0016(8) 0.0031(8) 0.0144(8) C(5*) 0.0141(8) 0.0142(9) 0.0209(9) -0.0007(7) 0.0020(7) 0.0028(7) C(5) 0.0141(8) 0.0142(9) 0.0209(9) -0.0007(7) 0.0020(7) 0.0028(7) C(6) 0.023(1) 0.031(1) 0.026(1) -0.0037(8) 0.0114(8) -0.0016(8) C(6*) 0.023(1) 0.031(1) 0.026(1) -0.0037(8) 0.0114(8) -0.0016(8) C(7) 0.0126(8) 0.0167(9) 0.0169(8) -0.0002(7) 0.0003(7) 0.0054(7) C(7*) 0.0126(8) 0.0167(9) 0.0169(8) -0.0002(7) 0.0003(7) 0.0054(7) C(8*) 0.033(1) 0.032(1) 0.039(1) 0.0010(9) 0.006(1) -0.0089(9) C(8) 0.033(1) 0.032(1) 0.039(1) 0.0010(9) 0.006(1) -0.0089(9) C(9*) 0.036(1) 0.024(1) 0.046(1) 0.0060(9) 0.007(1) 0.0133(9) C(9) 0.036(1) 0.024(1) 0.046(1) 0.0060(9) 0.007(1) 0.0133(9) C(10*) 0.026(1) 0.022(1) 0.040(1) -0.0068(8) 0.0082(9) 0.0025(8) C(10) 0.026(1) 0.022(1) 0.040(1) -0.0068(8) 0.0082(9) 0.0025(8) C(11*) 0.052(2) 0.056(2) 0.027(1) 0.010(1) -0.005(1) -0.005(1) C(11) 0.052(2) 0.056(2) 0.027(1) 0.010(1) -0.005(1) -0.005(1) C(12*) 0.029(1) 0.034(1) 0.033(1) -0.0029(9) 0.0126(9) -0.0062(9) C(12) 0.029(1) 0.034(1) 0.033(1) -0.0029(9) 0.0126(9) -0.0062(9) C(13*) 0.031(1) 0.027(1) 0.057(1) -0.0067(9) 0.011(1) -0.010(1) C(13) 0.031(1) 0.027(1) 0.057(1) -0.0067(9) 0.011(1) -0.010(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4150 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_all 0.0300 _refine_ls_wR_factor_ref 0.0300 _refine_ls_goodness_of_fit_all 2.368 _refine_ls_goodness_of_fit_ref 2.368 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -0.62 _refine_diff_density_max 0.55 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) Al(1) 2.4184(5) . . yes As(1) C(7) 2.041(2) . . yes As(1) H(27) 1.54 . . no Si(1) C(7) 1.914(2) . . yes Si(1) C(8) 1.870(2) . . yes Si(1) C(9) 1.870(2) . . yes Si(1) C(10) 1.867(2) . . yes Si(2) C(7) 1.913(2) . . yes Si(2) C(11) 1.871(2) . . yes Si(2) C(12) 1.869(2) . . yes Si(2) C(13) 1.872(2) . . yes Al(1) Al(1) 2.815(1) . 3_556 yes Al(1) N(1) 2.043(1) . . yes Al(1) H(25) 1.52(2) . . yes Al(1) H(26) 1.60 . . no N(1) C(1) 1.362(2) . . yes N(1) C(5) 1.364(2) . . yes C(1) C(2) 1.381(2) . . yes C(1) C(6) 1.501(2) . . yes C(2) C(3) 1.376(3) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.372(3) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.401(2) . . yes C(4) H(3) 0.95 . . no C(5) C(7) 1.512(2) . . yes C(6) H(4) 0.95 . . no C(6) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(8) H(7) 0.95 . . no C(8) H(8) 0.95 . . no C(8) H(9) 0.95 . . no C(9) H(10) 0.95 . . no C(9) H(11) 0.95 . . no C(9) H(12) 0.95 . . no C(10) H(13) 0.95 . . no C(10) H(14) 0.95 . . no C(10) H(15) 0.95 . . no C(11) H(16) 0.95 . . no C(11) H(17) 0.95 . . no C(11) H(18) 0.95 . . no C(12) H(19) 0.95 . . no C(12) H(20) 0.95 . . no C(12) H(21) 0.95 . . no C(13) H(22) 0.95 . . no C(13) H(23) 0.95 . . no C(13) H(24) 0.95 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Al(1) As(1) C(7) 92.76(5) . . . yes Al(1) As(1) H(27) 93.8 . . . no C(7) As(1) H(27) 99.3 . . . no C(7) Si(1) C(8) 107.69(9) . . . yes C(7) Si(1) C(9) 114.31(8) . . . yes C(7) Si(1) C(10) 111.62(8) . . . yes C(8) Si(1) C(9) 106.0(1) . . . yes C(8) Si(1) C(10) 109.91(9) . . . yes C(9) Si(1) C(10) 107.10(9) . . . yes C(7) Si(2) C(11) 115.85(9) . . . yes C(7) Si(2) C(12) 112.39(8) . . . yes C(7) Si(2) C(13) 107.27(9) . . . yes C(11) Si(2) C(12) 104.3(1) . . . yes C(11) Si(2) C(13) 106.0(1) . . . yes C(12) Si(2) C(13) 110.82(9) . . . yes As(1) Al(1) Al(1) 102.79(3) . . 3_556 yes As(1) Al(1) N(1) 89.96(4) . . . yes As(1) Al(1) H(25) 120.2(7) . . . yes As(1) Al(1) H(26) 117.4 . . . no Al(1) Al(1) N(1) 136.65(5) 3_556 . . yes Al(1) Al(1) H(25) 106.4(7) 3_556 . . yes Al(1) Al(1) H(26) 43.7 3_556 . . no N(1) Al(1) H(25) 102.0(7) . . . yes N(1) Al(1) H(26) 93.6 . . . no H(25) Al(1) H(26) 119.9 . . . no Al(1) N(1) C(1) 119.5(1) . . . yes Al(1) N(1) C(5) 120.5(1) . . . yes C(1) N(1) C(5) 120.0(1) . . . yes N(1) C(1) C(2) 121.8(2) . . . yes N(1) C(1) C(6) 118.4(1) . . . yes C(2) C(1) C(6) 119.8(2) . . . yes C(1) C(2) C(3) 119.0(2) . . . yes C(1) C(2) H(1) 120.5 . . . no C(3) C(2) H(1) 120.5 . . . no C(2) C(3) C(4) 119.5(2) . . . yes C(2) C(3) H(2) 120.3 . . . no C(4) C(3) H(2) 120.3 . . . no C(3) C(4) C(5) 121.0(2) . . . yes C(3) C(4) H(3) 119.5 . . . no C(5) C(4) H(3) 119.5 . . . no N(1) C(5) C(4) 118.9(2) . . . yes N(1) C(5) C(7) 121.9(1) . . . yes C(4) C(5) C(7) 119.2(1) . . . yes C(1) C(6) H(4) 109.5 . . . no C(1) C(6) H(5) 109.5 . . . no C(1) C(6) H(6) 109.5 . . . no H(4) C(6) H(5) 109.5 . . . no H(4) C(6) H(6) 109.5 . . . no H(5) C(6) H(6) 109.5 . . . no As(1) C(7) Si(1) 102.54(7) . . . yes As(1) C(7) Si(2) 104.22(8) . . . yes As(1) C(7) C(5) 114.7(1) . . . yes Si(1) C(7) Si(2) 119.21(9) . . . yes Si(1) C(7) C(5) 106.4(1) . . . yes Si(2) C(7) C(5) 109.9(1) . . . yes Si(1) C(8) H(7) 109.5 . . . no Si(1) C(8) H(8) 109.5 . . . no Si(1) C(8) H(9) 109.5 . . . no H(7) C(8) H(8) 109.5 . . . no H(7) C(8) H(9) 109.5 . . . no H(8) C(8) H(9) 109.5 . . . no Si(1) C(9) H(10) 109.5 . . . no Si(1) C(9) H(11) 109.5 . . . no Si(1) C(9) H(12) 109.5 . . . no H(10) C(9) H(11) 109.5 . . . no H(10) C(9) H(12) 109.5 . . . no H(11) C(9) H(12) 109.5 . . . no Si(1) C(10) H(13) 109.5 . . . no Si(1) C(10) H(14) 109.5 . . . no Si(1) C(10) H(15) 109.5 . . . no H(13) C(10) H(14) 109.5 . . . no H(13) C(10) H(15) 109.5 . . . no H(14) C(10) H(15) 109.5 . . . no Si(2) C(11) H(16) 109.5 . . . no Si(2) C(11) H(17) 109.5 . . . no Si(2) C(11) H(18) 109.5 . . . no H(16) C(11) H(17) 109.5 . . . no H(16) C(11) H(18) 109.5 . . . no H(17) C(11) H(18) 109.5 . . . no Si(2) C(12) H(19) 109.5 . . . no Si(2) C(12) H(20) 109.5 . . . no Si(2) C(12) H(21) 109.5 . . . no H(19) C(12) H(20) 109.5 . . . no H(19) C(12) H(21) 109.5 . . . no H(20) C(12) H(21) 109.5 . . . no Si(2) C(13) H(22) 109.5 . . . no Si(2) C(13) H(23) 109.5 . . . no Si(2) C(13) H(24) 109.5 . . . no H(22) C(13) H(23) 109.5 . . . no H(22) C(13) H(24) 109.5 . . . no H(23) C(13) H(24) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(1) C(9) 3.556(2) . 2_445 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag As(1) Al(1) Al(1) As(1) . . 3_556 3_556 180.0000 no As(1) Al(1) Al(1) N(1) . . 3_556 3_556 76.16(7) no As(1) Al(1) N(1) C(1) . . . . -179.1(1) no As(1) Al(1) N(1) C(5) . . . . 3.5(1) no As(1) C(7) Si(1) C(8) . . . . -66.1(1) no As(1) C(7) Si(1) C(9) . . . . 176.43(8) no As(1) C(7) Si(1) C(10) . . . . 54.7(1) no As(1) C(7) Si(2) C(11) . . . . -170.1(1) no As(1) C(7) Si(2) C(12) . . . . -50.3(1) no As(1) C(7) Si(2) C(13) . . . . 71.8(1) no As(1) C(7) C(5) N(1) . . . . 4.1(2) no As(1) C(7) C(5) C(4) . . . . -177.9(1) no Si(1) C(7) As(1) Al(1) . . . . 113.79(6) no Si(1) C(7) Si(2) C(11) . . . . -56.6(1) no Si(1) C(7) Si(2) C(12) . . . . 63.2(1) no Si(1) C(7) Si(2) C(13) . . . . -174.7(1) no Si(1) C(7) C(5) N(1) . . . . -108.6(1) no Si(1) C(7) C(5) C(4) . . . . 69.5(2) no Si(2) C(7) As(1) Al(1) . . . . -121.30(6) no Si(2) C(7) Si(1) C(8) . . . . 179.6(1) no Si(2) C(7) Si(1) C(9) . . . . 62.0(1) no Si(2) C(7) Si(1) C(10) . . . . -59.7(1) no Si(2) C(7) C(5) N(1) . . . . 121.1(1) no Si(2) C(7) C(5) C(4) . . . . -60.9(2) no Al(1) As(1) C(7) C(5) . . . . -1.1(1) no Al(1) Al(1) As(1) C(7) . 3_556 3_556 3_556 -137.27(5) no Al(1) Al(1) N(1) C(1) . 3_556 3_556 3_556 -72.1(1) no Al(1) Al(1) N(1) C(5) . 3_556 3_556 3_556 105.3(1) no Al(1) N(1) C(1) C(2) . . . . -177.3(1) no Al(1) N(1) C(1) C(6) . . . . 2.4(2) no Al(1) N(1) C(5) C(4) . . . . 176.6(1) no Al(1) N(1) C(5) C(7) . . . . -5.3(2) no N(1) Al(1) As(1) C(7) . . . . -0.93(6) no N(1) Al(1) Al(1) N(1) . . 3_556 3_556 -180.0000 no N(1) C(1) C(2) C(3) . . . . 0.1(3) no N(1) C(5) C(4) C(3) . . . . 1.2(3) no C(1) N(1) C(5) C(4) . . . . -0.8(2) no C(1) N(1) C(5) C(7) . . . . 177.2(1) no C(1) C(2) C(3) C(4) . . . . 0.2(3) no C(2) C(1) N(1) C(5) . . . . 0.2(2) no C(2) C(3) C(4) C(5) . . . . -0.9(3) no C(3) C(2) C(1) C(6) . . . . -179.6(2) no C(3) C(4) C(5) C(7) . . . . -176.9(2) no C(5) N(1) C(1) C(6) . . . . 179.9(1) no C(5) C(7) Si(1) C(8) . . . . 54.7(1) no C(5) C(7) Si(1) C(9) . . . . -62.8(1) no C(5) C(7) Si(1) C(10) . . . . 175.4(1) no C(5) C(7) Si(2) C(11) . . . . 66.6(1) no C(5) C(7) Si(2) C(12) . . . . -173.6(1) no C(5) C(7) Si(2) C(13) . . . . -51.6(1) no #------------------------------------------------------------------------------