Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Makoto Minato' 'Takashi Ito' 'Masaki Kakeya' 'Takaomi Matsumoto' 'Jun-ya Nishiuchi' 'Yoshitaka Yamaguchi' _publ_contact_author_name 'Makoto Minato' _publ_contact_author_address ; Department of Materials Chemistry Yokohama National University Graduate School of Engineering 79-5 Tokiwadai Hodogaya-ku Yokohama 240-8501 JAPAN ; _publ_contact_author_email 'MINATO@YNU.AC.JP' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Reactions of quadruply chelated silyl- and germyl-molybdenum hydrido complexes with isocyanides: observation of the trans-influence of the silyl ligand ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ data_nij121/ito_lab/YNU _database_code_CSD 194603 _audit_creation_date 'Tue Feb 27 16:27:52 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C70 H69 N Mo P4 Si ' _chemical_formula_moiety '?' _chemical_formula_weight 1172.24 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.42(2) _cell_length_b 17.611(5) _cell_length_c 13.275(4) _cell_angle_alpha 90.50(2) _cell_angle_beta 109.72(5) _cell_angle_gamma 76.78(7) _cell_volume 3081.4299 _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 218.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 9993 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.63 _diffrn_measured_fraction_theta_max 0.6976 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.6976 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 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 9993 _reflns_number_gt 8760 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1316 _refine_ls_wR_factor_ref 0.3214 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9993 _refine_ls_number_parameters 638 _refine_ls_goodness_of_fit_ref 3.384 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0040 _refine_diff_density_max 1.35 _refine_diff_density_min -2.44 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Mo' 'Mo' -1.683 0.686 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.67368(6) 0.24119(4) 0.91480(6) 0.0410(2) Uani 1.00 d . . . P(1) P 0.8275(2) 0.1438(1) 1.0070(2) 0.0481(7) Uani 1.00 d . . . P(2) P 0.6220(2) 0.1229(1) 0.8351(2) 0.0464(7) Uani 1.00 d . . . P(3) P 0.5085(2) 0.3346(1) 0.8374(2) 0.0454(7) Uani 1.00 d . . . P(4) P 0.7210(2) 0.3649(1) 0.9588(2) 0.0444(7) Uani 1.00 d . . . Si(1) Si 0.6880(2) 0.2489(1) 1.1089(2) 0.0439(7) Uani 1.00 d . . . N(1) N 0.7784(7) 0.2438(5) 0.7337(7) 0.063(3) Uani 1.00 d . . . C(1) C 0.7359(7) 0.2466(5) 0.7937(9) 0.056(3) Uani 1.00 d . . . C(2) C 0.8168(9) 0.2514(6) 0.6474(8) 0.061(3) Uani 1.00 d . . . C(3) C 0.917(2) 0.257(3) 0.686(2) 0.29(2) Uani 1.00 d . . . C(4) C 0.826(3) 0.176(1) 0.598(2) 0.22(1) Uani 1.00 d . . . C(5) C 0.746(2) 0.310(2) 0.572(3) 0.32(2) Uani 1.00 d . . . C(6) C 0.5796(8) 0.2658(6) 1.1670(8) 0.059(3) Uani 1.00 d . . . C(7) C 0.5301(8) 0.2042(6) 1.1648(10) 0.066(4) Uani 1.00 d . . . C(8) C 0.4470(9) 0.2147(9) 1.2028(9) 0.084(4) Uani 1.00 d . . . C(9) C 0.415(1) 0.286(1) 1.240(1) 0.119(6) Uani 1.00 d . . . C(10) C 0.461(1) 0.3500(9) 1.2364(9) 0.095(5) Uani 1.00 d . . . C(11) C 0.5445(9) 0.3374(7) 1.2028(9) 0.072(4) Uani 1.00 d . . . C(12) C 0.7771(7) 0.1549(5) 1.1887(7) 0.047(3) Uani 1.00 d . . . C(13) C 0.8419(7) 0.1088(5) 1.1445(7) 0.047(3) Uani 1.00 d . . . C(14) C 0.9141(8) 0.0438(6) 1.2002(9) 0.061(3) Uani 1.00 d . . . C(15) C 0.9190(8) 0.0203(6) 1.3018(9) 0.066(3) Uani 1.00 d . . . C(16) C 0.8559(8) 0.0643(6) 1.3503(8) 0.060(3) Uani 1.00 d . . . C(17) C 0.7832(8) 0.1311(5) 1.2920(8) 0.055(3) Uani 1.00 d . . . C(18) C 0.9582(8) 0.1514(5) 1.0273(8) 0.054(3) Uani 1.00 d . . . C(19) C 1.0252(9) 0.1663(7) 1.128(1) 0.074(4) Uani 1.00 d . . . C(20) C 1.1201(10) 0.1754(9) 1.136(1) 0.089(5) Uani 1.00 d . . . C(21) C 1.1538(9) 0.1689(8) 1.053(1) 0.083(4) Uani 1.00 d . . . C(22) C 1.0905(10) 0.1542(6) 0.956(1) 0.073(4) Uani 1.00 d . . . C(23) C 0.9937(8) 0.1453(6) 0.9415(8) 0.055(3) Uani 1.00 d . . . C(24) C 0.8236(7) 0.0515(5) 0.9360(8) 0.050(3) Uani 1.00 d . . . C(25) C 0.7194(8) 0.0362(5) 0.9100(7) 0.051(3) Uani 1.00 d . . . C(26) C 0.5077(7) 0.0926(5) 0.8331(7) 0.052(3) Uani 1.00 d . . . C(27) C 0.4639(9) 0.1173(7) 0.911(1) 0.072(4) Uani 1.00 d . . . C(28) C 0.381(1) 0.0893(8) 0.915(1) 0.078(4) Uani 1.00 d . . . C(29) C 0.3413(10) 0.0404(7) 0.8411(10) 0.073(4) Uani 1.00 d . . . C(30) C 0.382(1) 0.0162(8) 0.765(1) 0.081(5) Uani 1.00 d . . . C(31) C 0.4659(10) 0.0400(7) 0.7642(10) 0.074(4) Uani 1.00 d . . . C(32) C 0.6130(8) 0.1082(5) 0.6952(7) 0.051(3) Uani 1.00 d . . . C(33) C 0.5423(9) 0.1611(7) 0.6169(8) 0.067(4) Uani 1.00 d . . . C(34) C 0.527(1) 0.1563(8) 0.509(1) 0.096(5) Uani 1.00 d . . . C(35) C 0.586(1) 0.094(1) 0.479(1) 0.104(6) Uani 1.00 d . . . C(36) C 0.656(1) 0.0378(8) 0.553(1) 0.093(5) Uani 1.00 d . . . C(37) C 0.674(1) 0.0464(7) 0.6647(10) 0.075(4) Uani 1.00 d . . . C(38) C 0.3879(7) 0.3179(5) 0.8418(8) 0.052(3) Uani 1.00 d . . . C(39) C 0.3587(7) 0.3351(6) 0.9284(8) 0.054(3) Uani 1.00 d . . . C(40) C 0.2678(9) 0.3218(7) 0.932(1) 0.073(4) Uani 1.00 d . . . C(41) C 0.2056(9) 0.2899(8) 0.844(1) 0.078(4) Uani 1.00 d . . . C(42) C 0.2337(10) 0.2714(9) 0.757(1) 0.086(5) Uani 1.00 d . . . C(43) C 0.3254(9) 0.2856(8) 0.757(1) 0.078(4) Uani 1.00 d . . . C(44) C 0.4612(7) 0.3810(5) 0.6970(8) 0.049(3) Uani 1.00 d . . . C(45) C 0.3710(9) 0.4392(7) 0.6602(9) 0.072(4) Uani 1.00 d . . . C(46) C 0.3364(9) 0.4727(8) 0.558(1) 0.090(4) Uani 1.00 d . . . C(47) C 0.3891(10) 0.4530(8) 0.4876(9) 0.078(4) Uani 1.00 d . . . C(48) C 0.479(1) 0.3962(8) 0.5257(9) 0.086(5) Uani 1.00 d . . . C(49) C 0.5149(9) 0.3603(7) 0.6282(8) 0.072(4) Uani 1.00 d . . . C(50) C 0.5168(7) 0.4251(5) 0.9073(7) 0.047(3) Uani 1.00 d . . . C(51) C 0.6090(7) 0.4487(5) 0.9059(7) 0.048(3) Uani 1.00 d . . . C(52) C 0.7529(7) 0.3290(5) 1.1684(8) 0.051(3) Uani 1.00 d . . . C(53) C 0.7646(7) 0.3832(6) 1.1015(8) 0.054(3) Uani 1.00 d . . . C(54) C 0.8056(8) 0.4481(6) 1.1382(8) 0.056(3) Uani 1.00 d . . . C(55) C 0.8372(10) 0.4582(7) 1.2500(9) 0.070(4) Uani 1.00 d . . . C(56) C 0.8308(10) 0.4040(8) 1.317(1) 0.081(4) Uani 1.00 d . . . C(57) C 0.7868(10) 0.3415(7) 1.2809(9) 0.072(4) Uani 1.00 d . . . C(58) C 0.8172(7) 0.3967(5) 0.9195(7) 0.047(3) Uani 1.00 d . . . C(59) C 0.9204(9) 0.3595(7) 0.968(1) 0.076(4) Uani 1.00 d . . . C(60) C 0.995(1) 0.3818(9) 0.945(1) 0.094(5) Uani 1.00 d . . . C(61) C 0.976(1) 0.4436(8) 0.881(1) 0.086(5) Uani 1.00 d . . . C(62) C 0.874(1) 0.4849(10) 0.830(1) 0.117(7) Uani 1.00 d . . . C(63) C 0.7957(10) 0.4614(7) 0.848(1) 0.086(4) Uani 1.00 d . . . C(64) C 0.1398(10) 0.1932(7) 0.4612(9) 0.2018 Uiso 1.00 d G . . C(65) C 0.0651(9) 0.2476(9) 0.383(1) 0.2018 Uiso 1.00 d G . . C(69) C 0.2408(9) 0.1981(9) 0.494(1) 0.2018 Uiso 1.00 d G . . C(71) C 0.091(1) 0.3069(8) 0.337(1) 0.2018 Uiso 1.00 d G . . C(72) C 0.192(2) 0.3118(8) 0.370(1) 0.2018 Uiso 1.00 d G . . C(73) C 0.267(1) 0.257(1) 0.448(1) 0.2018 Uiso 1.00 d G . . C(74) C 0.111(2) 0.1278(10) 0.512(2) 0.2018 Uiso 1.00 d G . . H(1) H 0.9562 0.2150 0.7357 0.3505 Uiso 1.00 calc . . . H(2) H 0.9403 0.2562 0.6262 0.3505 Uiso 1.00 calc . . . H(3) H 0.9195 0.3054 0.7172 0.3505 Uiso 1.00 calc . . . H(4) H 0.7658 0.1599 0.5781 0.2545 Uiso 1.00 calc . . . H(5) H 0.8470 0.1800 0.5375 0.2545 Uiso 1.00 calc . . . H(6) H 0.8794 0.1367 0.6497 0.2545 Uiso 1.00 calc . . . H(7) H 0.7464 0.3595 0.6073 0.3798 Uiso 1.00 calc . . . H(8) H 0.7691 0.3146 0.5140 0.3798 Uiso 1.00 calc . . . H(9) H 0.6828 0.3011 0.5514 0.3798 Uiso 1.00 calc . . . H(10) H 0.5528 0.1558 1.1381 0.0796 Uiso 1.00 calc . . . H(11) H 0.4143 0.1735 1.2029 0.1003 Uiso 1.00 calc . . . H(12) H 0.3610 0.2939 1.2678 0.1434 Uiso 1.00 calc . . . H(13) H 0.4357 0.4001 1.2569 0.1131 Uiso 1.00 calc . . . H(14) H 0.5777 0.3784 1.2041 0.0858 Uiso 1.00 calc . . . H(15) H 0.9608 0.0151 1.1693 0.0731 Uiso 1.00 calc . . . H(16) H 0.9661 -0.0265 1.3382 0.0798 Uiso 1.00 calc . . . H(17) H 0.8612 0.0498 1.4213 0.0717 Uiso 1.00 calc . . . H(18) H 0.7376 0.1608 1.3234 0.0659 Uiso 1.00 calc . . . H(19) H 1.0048 0.1696 1.1889 0.0880 Uiso 1.00 calc . . . H(20) H 1.1632 0.1872 1.2034 0.1066 Uiso 1.00 calc . . . H(21) H 1.2201 0.1742 1.0619 0.0991 Uiso 1.00 calc . . . H(22) H 1.1136 0.1498 0.8963 0.0873 Uiso 1.00 calc . . . H(23) H 0.9515 0.1350 0.8729 0.0664 Uiso 1.00 calc . . . H(24) H 0.8370 0.0572 0.8714 0.0604 Uiso 1.00 calc . . . H(25) H 0.8732 0.0091 0.9808 0.0604 Uiso 1.00 calc . . . H(26) H 0.7090 0.0253 0.9748 0.0617 Uiso 1.00 calc . . . H(27) H 0.7147 -0.0074 0.8676 0.0617 Uiso 1.00 calc . . . H(28) H 0.4901 0.1528 0.9608 0.0858 Uiso 1.00 calc . . . H(29) H 0.3522 0.1045 0.9696 0.0931 Uiso 1.00 calc . . . H(30) H 0.2839 0.0231 0.8426 0.0876 Uiso 1.00 calc . . . H(31) H 0.3535 -0.0170 0.7129 0.0978 Uiso 1.00 calc . . . H(32) H 0.4966 0.0197 0.7135 0.0888 Uiso 1.00 calc . . . H(33) H 0.5007 0.2038 0.6379 0.0805 Uiso 1.00 calc . . . H(34) H 0.4789 0.1955 0.4564 0.1141 Uiso 1.00 calc . . . H(35) H 0.5761 0.0886 0.4054 0.1245 Uiso 1.00 calc . . . H(36) H 0.6923 -0.0067 0.5298 0.1124 Uiso 1.00 calc . . . H(37) H 0.7278 0.0103 0.7175 0.0902 Uiso 1.00 calc . . . H(38) H 0.4007 0.3565 0.9876 0.0650 Uiso 1.00 calc . . . H(39) H 0.2481 0.3340 0.9929 0.0873 Uiso 1.00 calc . . . H(40) H 0.1435 0.2812 0.8461 0.0941 Uiso 1.00 calc . . . H(41) H 0.1923 0.2497 0.6974 0.1035 Uiso 1.00 calc . . . H(42) H 0.3458 0.2725 0.6965 0.0943 Uiso 1.00 calc . . . H(43) H 0.3337 0.4555 0.7067 0.0870 Uiso 1.00 calc . . . H(44) H 0.2738 0.5111 0.5344 0.1072 Uiso 1.00 calc . . . H(45) H 0.3645 0.4774 0.4169 0.0939 Uiso 1.00 calc . . . H(46) H 0.5173 0.3812 0.4798 0.1031 Uiso 1.00 calc . . . H(47) H 0.5769 0.3212 0.6515 0.0865 Uiso 1.00 calc . . . H(48) H 0.4583 0.4655 0.8717 0.0563 Uiso 1.00 calc . . . H(49) H 0.5211 0.4161 0.9794 0.0563 Uiso 1.00 calc . . . H(50) H 0.6189 0.4913 0.9494 0.0574 Uiso 1.00 calc . . . H(51) H 0.6007 0.4641 0.8343 0.0574 Uiso 1.00 calc . . . H(52) H 0.8121 0.4840 1.0893 0.0665 Uiso 1.00 calc . . . H(53) H 0.8625 0.5023 1.2773 0.0842 Uiso 1.00 calc . . . H(54) H 0.8572 0.4086 1.3924 0.0969 Uiso 1.00 calc . . . H(55) H 0.7793 0.3071 1.3308 0.0856 Uiso 1.00 calc . . . H(56) H 0.9386 0.3168 1.0203 0.0902 Uiso 1.00 calc . . . H(57) H 1.0630 0.3520 0.9770 0.1116 Uiso 1.00 calc . . . H(58) H 1.0293 0.4599 0.8677 0.1032 Uiso 1.00 calc . . . H(59) H 0.8601 0.5302 0.7840 0.1402 Uiso 1.00 calc . . . H(60) H 0.7274 0.4886 0.8102 0.1042 Uiso 1.00 calc . . . 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 Mo(1) 0.0403(5) 0.0262(4) 0.0620(5) -0.0024(3) 0.0270(4) -0.0032(3) P(1) 0.041(1) 0.032(1) 0.075(2) -0.001(1) 0.028(1) -0.003(1) P(2) 0.047(1) 0.030(1) 0.068(2) -0.006(1) 0.028(1) -0.006(1) P(3) 0.040(1) 0.032(1) 0.067(1) -0.0018(10) 0.025(1) -0.005(1) P(4) 0.042(1) 0.029(1) 0.068(1) -0.0053(10) 0.026(1) -0.0038(10) Si(1) 0.048(1) 0.031(1) 0.058(1) -0.002(1) 0.029(1) -0.001(1) N(1) 0.064(6) 0.052(5) 0.097(6) -0.008(4) 0.059(5) -0.003(4) C(1) 0.044(6) 0.023(4) 0.096(7) 0.002(4) 0.023(5) 0.001(4) C(2) 0.076(7) 0.055(6) 0.073(7) -0.016(6) 0.049(6) -0.006(5) C(3) 0.16(2) 0.67(7) 0.16(2) -0.21(3) 0.13(2) -0.12(3) C(4) 0.40(4) 0.24(3) 0.18(2) -0.21(3) 0.22(2) -0.16(2) C(5) 0.31(3) 0.27(3) 0.41(4) 0.18(3) 0.32(4) 0.22(3) C(6) 0.050(6) 0.050(6) 0.080(7) 0.006(5) 0.038(5) 0.001(5) C(7) 0.056(6) 0.060(7) 0.097(8) -0.010(5) 0.046(6) 0.012(6) C(8) 0.072(8) 0.12(1) 0.060(7) -0.011(8) 0.031(6) 0.034(7) C(9) 0.09(1) 0.14(1) 0.11(1) 0.06(1) 0.077(9) 0.04(1) C(10) 0.10(1) 0.10(1) 0.068(7) 0.051(9) 0.059(7) 0.031(7) C(11) 0.067(7) 0.064(7) 0.080(7) 0.018(6) 0.040(6) 0.008(5) C(12) 0.044(5) 0.039(5) 0.061(5) -0.010(4) 0.020(4) -0.002(4) C(13) 0.041(5) 0.044(5) 0.060(5) -0.005(4) 0.024(4) -0.002(4) C(14) 0.056(6) 0.048(6) 0.079(7) 0.000(5) 0.030(5) 0.021(5) C(15) 0.058(7) 0.039(6) 0.088(7) 0.006(5) 0.015(6) 0.013(5) C(16) 0.055(6) 0.051(6) 0.071(6) -0.008(5) 0.018(5) 0.021(5) C(17) 0.054(6) 0.038(5) 0.075(6) -0.009(5) 0.026(5) 0.001(4) C(18) 0.055(6) 0.034(5) 0.079(7) -0.001(4) 0.036(5) -0.001(4) C(19) 0.059(7) 0.074(8) 0.097(9) -0.015(6) 0.036(7) -0.005(6) C(20) 0.056(8) 0.10(1) 0.11(1) -0.024(7) 0.026(7) -0.028(8) C(21) 0.047(7) 0.081(9) 0.12(1) -0.006(6) 0.030(7) 0.021(8) C(22) 0.074(8) 0.044(6) 0.119(10) 0.007(6) 0.069(8) 0.017(6) C(23) 0.049(6) 0.044(5) 0.080(7) -0.001(5) 0.036(5) -0.004(5) C(24) 0.053(6) 0.034(5) 0.066(6) -0.003(4) 0.028(5) 0.002(4) C(25) 0.063(6) 0.031(5) 0.060(5) 0.002(4) 0.028(5) -0.002(4) C(26) 0.057(6) 0.037(5) 0.061(6) 0.003(4) 0.028(5) 0.008(4) C(27) 0.066(7) 0.061(7) 0.116(9) -0.028(6) 0.057(7) -0.026(6) C(28) 0.084(9) 0.088(9) 0.089(8) -0.035(7) 0.054(7) -0.023(7) C(29) 0.079(8) 0.073(8) 0.089(8) -0.040(7) 0.042(7) -0.025(6) C(30) 0.086(9) 0.086(9) 0.100(9) -0.046(8) 0.050(8) -0.028(7) C(31) 0.080(8) 0.071(8) 0.097(8) -0.040(7) 0.048(7) -0.046(7) C(32) 0.067(6) 0.035(5) 0.060(6) -0.010(5) 0.033(5) -0.010(4) C(33) 0.093(9) 0.067(7) 0.046(6) -0.015(6) 0.033(5) -0.012(5) C(34) 0.15(1) 0.069(8) 0.086(9) -0.020(9) 0.061(9) -0.032(7) C(35) 0.12(1) 0.14(1) 0.068(8) -0.06(1) 0.041(8) -0.019(9) C(36) 0.13(1) 0.075(9) 0.078(8) -0.007(9) 0.049(8) -0.038(7) C(37) 0.095(9) 0.051(6) 0.093(8) -0.010(6) 0.053(7) -0.013(6) C(38) 0.041(5) 0.041(5) 0.072(6) 0.001(4) 0.023(5) 0.009(4) C(39) 0.052(6) 0.049(6) 0.073(6) -0.011(5) 0.035(5) -0.010(5) C(40) 0.056(7) 0.060(7) 0.12(1) -0.011(6) 0.060(7) -0.003(7) C(41) 0.063(8) 0.097(10) 0.104(9) -0.045(7) 0.047(7) -0.025(8) C(42) 0.069(8) 0.11(1) 0.108(10) -0.056(8) 0.048(7) -0.042(8) C(43) 0.066(8) 0.089(9) 0.099(9) -0.038(7) 0.038(7) -0.035(7) C(44) 0.042(5) 0.038(5) 0.067(6) -0.010(4) 0.018(4) -0.003(4) C(45) 0.064(7) 0.054(7) 0.084(8) 0.007(6) 0.019(6) 0.009(6) C(46) 0.054(7) 0.079(9) 0.11(1) 0.012(7) 0.017(7) 0.037(8) C(47) 0.072(8) 0.088(9) 0.062(7) 0.001(7) 0.017(6) 0.015(6) C(48) 0.11(1) 0.097(10) 0.064(7) -0.009(8) 0.056(7) -0.004(6) C(49) 0.069(7) 0.082(8) 0.060(6) 0.007(6) 0.032(5) -0.004(5) C(50) 0.049(5) 0.028(4) 0.065(5) 0.000(4) 0.026(4) -0.004(4) C(51) 0.060(6) 0.032(5) 0.052(5) -0.002(4) 0.025(4) -0.012(4) C(52) 0.046(5) 0.040(5) 0.071(6) -0.007(4) 0.026(5) -0.009(4) C(53) 0.046(5) 0.041(5) 0.076(6) 0.004(4) 0.030(5) 0.006(4) C(54) 0.061(7) 0.043(6) 0.067(6) -0.018(5) 0.023(5) -0.013(4) C(55) 0.095(9) 0.052(7) 0.064(7) -0.022(6) 0.023(6) -0.017(5) C(56) 0.073(8) 0.078(9) 0.086(8) -0.018(7) 0.020(7) -0.037(7) C(57) 0.086(9) 0.051(7) 0.082(8) -0.010(6) 0.038(7) -0.008(6) C(58) 0.048(5) 0.035(5) 0.061(5) -0.006(4) 0.023(4) -0.010(4) C(59) 0.053(7) 0.068(8) 0.113(9) 0.004(6) 0.049(7) 0.016(7) C(60) 0.067(8) 0.083(10) 0.15(1) -0.009(7) 0.070(9) 0.005(9) C(61) 0.10(1) 0.074(9) 0.13(1) -0.041(8) 0.078(9) -0.037(8) C(62) 0.10(1) 0.11(1) 0.17(2) -0.03(1) 0.07(1) 0.04(1) C(63) 0.066(8) 0.067(8) 0.13(1) -0.020(6) 0.036(8) 0.037(7) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Mo(1) P(1) 2.414(3) . . yes Mo(1) P(2) 2.480(3) . . yes Mo(1) P(3) 2.454(3) . . yes Mo(1) P(4) 2.438(3) . . yes Mo(1) Si(1) 2.519(3) . . yes Mo(1) C(1) 2.10(1) . . yes P(1) C(13) 1.86(1) . . yes P(1) C(18) 1.85(1) . . yes P(1) C(24) 1.875(10) . . yes P(2) C(25) 1.843(8) . . yes P(2) C(26) 1.84(1) . . yes P(2) C(32) 1.84(1) . . yes P(3) C(38) 1.85(1) . . yes P(3) C(44) 1.876(10) . . yes P(3) C(50) 1.846(9) . . yes P(4) C(51) 1.856(8) . . yes P(4) C(53) 1.83(1) . . yes P(4) C(58) 1.83(1) . . yes Si(1) C(6) 1.93(1) . . yes Si(1) C(12) 1.912(8) . . yes Si(1) C(52) 1.89(1) . . yes N(1) C(1) 1.15(2) . . yes N(1) C(2) 1.45(2) . . yes C(2) C(3) 1.39(3) . . yes C(2) C(4) 1.48(3) . . yes C(2) C(5) 1.40(3) . . yes C(6) C(7) 1.42(2) . . yes C(6) C(11) 1.39(2) . . yes C(7) C(8) 1.42(2) . . yes C(8) C(9) 1.39(2) . . yes C(9) C(10) 1.44(3) . . yes C(10) C(11) 1.39(2) . . yes C(12) C(13) 1.38(1) . . yes C(12) C(17) 1.40(2) . . yes C(13) C(14) 1.38(1) . . yes C(14) C(15) 1.39(2) . . yes C(15) C(16) 1.38(2) . . yes C(16) C(17) 1.41(1) . . yes C(18) C(19) 1.42(2) . . yes C(18) C(23) 1.39(2) . . yes C(19) C(20) 1.38(2) . . yes C(20) C(21) 1.34(2) . . yes C(21) C(22) 1.37(2) . . yes C(22) C(23) 1.39(2) . . yes C(24) C(25) 1.51(2) . . yes C(26) C(27) 1.40(2) . . yes C(26) C(31) 1.39(2) . . yes C(27) C(28) 1.42(2) . . yes C(28) C(29) 1.37(2) . . yes C(29) C(30) 1.35(2) . . yes C(30) C(31) 1.37(2) . . yes C(32) C(33) 1.36(1) . . yes C(32) C(37) 1.39(2) . . yes C(33) C(34) 1.38(2) . . yes C(34) C(35) 1.37(2) . . yes C(35) C(36) 1.35(2) . . yes C(36) C(37) 1.43(2) . . yes C(38) C(39) 1.36(2) . . yes C(38) C(43) 1.40(2) . . yes C(39) C(40) 1.40(2) . . yes C(40) C(41) 1.41(2) . . yes C(41) C(42) 1.37(2) . . yes C(42) C(43) 1.40(2) . . yes C(44) C(45) 1.40(1) . . yes C(44) C(49) 1.38(2) . . yes C(45) C(46) 1.36(2) . . yes C(46) C(47) 1.39(2) . . yes C(47) C(48) 1.38(2) . . yes C(48) C(49) 1.38(2) . . yes C(50) C(51) 1.49(2) . . yes C(52) C(53) 1.38(2) . . yes C(52) C(57) 1.44(2) . . yes C(53) C(54) 1.41(1) . . yes C(54) C(55) 1.42(2) . . yes C(55) C(56) 1.35(2) . . yes C(56) C(57) 1.40(2) . . yes C(58) C(59) 1.41(1) . . yes C(58) C(63) 1.40(2) . . yes C(59) C(60) 1.35(2) . . yes C(60) C(61) 1.31(2) . . yes C(61) C(62) 1.40(2) . . yes C(62) C(63) 1.38(3) . . yes C(64) C(65) 1.39(2) . . yes C(64) C(69) 1.39(2) . . yes C(64) C(74) 1.54(3) . . yes C(65) C(71) 1.39(3) . . yes C(71) C(72) 1.39(3) . . yes C(72) C(73) 1.39(2) . . yes C(73) C(69) 1.39(3) . . yes #------------------------------------------------------------------------------ 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 P(1) Mo(1) P(2) 80.72(9) . . . yes P(1) Mo(1) P(3) 172.7(1) . . . yes P(1) Mo(1) P(4) 103.81(10) . . . yes P(1) Mo(1) Si(1) 76.77(9) . . . yes P(1) Mo(1) C(1) 85.9(2) . . . yes P(2) Mo(1) P(3) 97.73(9) . . . yes P(2) Mo(1) P(4) 169.22(10) . . . yes P(2) Mo(1) Si(1) 113.72(10) . . . yes P(2) Mo(1) C(1) 86.9(3) . . . yes P(3) Mo(1) P(4) 78.97(10) . . . yes P(3) Mo(1) Si(1) 97.49(9) . . . yes P(3) Mo(1) C(1) 101.2(2) . . . yes P(4) Mo(1) Si(1) 76.98(9) . . . yes P(4) Mo(1) C(1) 83.7(3) . . . yes Si(1) Mo(1) C(1) 149.9(3) . . . yes Mo(1) P(1) C(13) 115.6(3) . . . yes Mo(1) P(1) C(18) 126.1(3) . . . yes Mo(1) P(1) C(24) 108.5(3) . . . yes C(13) P(1) C(18) 100.7(5) . . . yes C(13) P(1) C(24) 101.2(4) . . . yes C(18) P(1) C(24) 101.1(5) . . . yes Mo(1) P(2) C(25) 108.2(3) . . . yes Mo(1) P(2) C(26) 125.5(3) . . . yes Mo(1) P(2) C(32) 118.2(4) . . . yes C(25) P(2) C(26) 99.4(5) . . . yes C(25) P(2) C(32) 103.1(4) . . . yes C(26) P(2) C(32) 99.0(5) . . . yes Mo(1) P(3) C(38) 124.2(3) . . . yes Mo(1) P(3) C(44) 122.6(3) . . . yes Mo(1) P(3) C(50) 107.3(3) . . . yes C(38) P(3) C(44) 98.8(4) . . . yes C(38) P(3) C(50) 102.2(5) . . . yes C(44) P(3) C(50) 97.0(4) . . . yes Mo(1) P(4) C(51) 110.9(3) . . . yes Mo(1) P(4) C(53) 116.6(4) . . . yes Mo(1) P(4) C(58) 123.9(3) . . . yes C(51) P(4) C(53) 100.5(4) . . . yes C(51) P(4) C(58) 102.4(5) . . . yes C(53) P(4) C(58) 99.2(5) . . . yes Mo(1) Si(1) C(6) 127.6(3) . . . yes Mo(1) Si(1) C(12) 109.1(3) . . . yes Mo(1) Si(1) C(52) 109.8(4) . . . yes C(6) Si(1) C(12) 102.0(5) . . . yes C(6) Si(1) C(52) 101.3(5) . . . yes C(12) Si(1) C(52) 104.6(4) . . . yes C(1) N(1) C(2) 169.8(8) . . . yes Mo(1) C(1) N(1) 173.0(7) . . . yes N(1) C(2) C(3) 111(1) . . . yes N(1) C(2) C(4) 107(1) . . . yes N(1) C(2) C(5) 108(1) . . . yes C(3) C(2) C(4) 101(2) . . . yes C(3) C(2) C(5) 117(2) . . . yes C(4) C(2) C(5) 109(1) . . . yes Si(1) C(6) C(7) 118.0(8) . . . yes Si(1) C(6) C(11) 122.0(10) . . . yes C(7) C(6) C(11) 119(1) . . . yes C(6) C(7) C(8) 120(1) . . . yes C(7) C(8) C(9) 118(1) . . . yes C(8) C(9) C(10) 120(1) . . . yes C(9) C(10) C(11) 119(1) . . . yes C(6) C(11) C(10) 120(1) . . . yes Si(1) C(12) C(13) 118.4(7) . . . yes Si(1) C(12) C(17) 124.0(7) . . . yes C(13) C(12) C(17) 117.6(8) . . . yes P(1) C(13) C(12) 114.8(6) . . . yes P(1) C(13) C(14) 123.1(9) . . . yes C(12) C(13) C(14) 122.1(10) . . . yes C(13) C(14) C(15) 119(1) . . . yes C(14) C(15) C(16) 120.5(9) . . . yes C(15) C(16) C(17) 118(1) . . . yes C(12) C(17) C(16) 121(1) . . . yes P(1) C(18) C(19) 122(1) . . . yes P(1) C(18) C(23) 120.2(7) . . . yes C(19) C(18) C(23) 117(1) . . . yes C(18) C(19) C(20) 119(1) . . . yes C(19) C(20) C(21) 122(1) . . . yes C(20) C(21) C(22) 118(1) . . . yes C(21) C(22) C(23) 121(1) . . . yes C(18) C(23) C(22) 120(1) . . . yes P(1) C(24) C(25) 108.9(7) . . . yes P(2) C(25) C(24) 109.7(7) . . . yes P(2) C(26) C(27) 119.5(8) . . . yes P(2) C(26) C(31) 123.8(10) . . . yes C(27) C(26) C(31) 116(1) . . . yes C(26) C(27) C(28) 119(1) . . . yes C(27) C(28) C(29) 119(1) . . . yes C(28) C(29) C(30) 121(1) . . . yes C(29) C(30) C(31) 119(1) . . . yes C(26) C(31) C(30) 123(1) . . . yes P(2) C(32) C(33) 118.2(8) . . . yes P(2) C(32) C(37) 123.8(7) . . . yes C(33) C(32) C(37) 118.0(10) . . . yes C(32) C(33) C(34) 123(1) . . . yes C(33) C(34) C(35) 117(1) . . . yes C(34) C(35) C(36) 121(1) . . . yes C(35) C(36) C(37) 119(1) . . . yes C(32) C(37) C(36) 118.9(10) . . . yes P(3) C(38) C(39) 121.3(8) . . . yes P(3) C(38) C(43) 120.5(10) . . . yes C(39) C(38) C(43) 118(1) . . . yes C(38) C(39) C(40) 121.3(10) . . . yes C(39) C(40) C(41) 119(1) . . . yes C(40) C(41) C(42) 120(1) . . . yes C(41) C(42) C(43) 117(1) . . . yes C(38) C(43) C(42) 122(1) . . . yes P(3) C(44) C(45) 120.3(9) . . . yes P(3) C(44) C(49) 121.5(7) . . . yes C(45) C(44) C(49) 118.2(10) . . . yes C(44) C(45) C(46) 120(1) . . . yes C(45) C(46) C(47) 122(1) . . . yes C(46) C(47) C(48) 116(1) . . . yes C(47) C(48) C(49) 122(1) . . . yes C(44) C(49) C(48) 120(1) . . . yes P(3) C(50) C(51) 108.8(7) . . . yes P(4) C(51) C(50) 109.4(6) . . . yes Si(1) C(52) C(53) 119.8(7) . . . yes Si(1) C(52) C(57) 124.2(9) . . . yes C(53) C(52) C(57) 115.8(10) . . . yes P(4) C(53) C(52) 114.4(7) . . . yes P(4) C(53) C(54) 121.9(8) . . . yes C(52) C(53) C(54) 123.7(9) . . . yes C(53) C(54) C(55) 118(1) . . . yes C(54) C(55) C(56) 118(1) . . . yes C(55) C(56) C(57) 122(1) . . . yes C(52) C(57) C(56) 120(1) . . . yes P(4) C(58) C(59) 120.1(9) . . . yes P(4) C(58) C(63) 123.8(8) . . . yes C(59) C(58) C(63) 115(1) . . . yes C(58) C(59) C(60) 122(1) . . . yes C(59) C(60) C(61) 121(1) . . . yes C(60) C(61) C(62) 118(1) . . . yes C(61) C(62) C(63) 121(1) . . . yes C(58) C(63) C(62) 119(1) . . . yes C(65) C(64) C(69) 120(1) . . . yes C(65) C(64) C(74) 119(1) . . . yes C(69) C(64) C(74) 120(1) . . . yes C(64) C(65) C(71) 119(1) . . . yes C(65) C(71) C(72) 119(1) . . . yes C(71) C(72) C(73) 120(1) . . . yes C(72) C(73) C(69) 119(1) . . . yes C(64) C(69) C(73) 119(1) . . . yes #------------------------------------------------------------------------------ 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 Mo(1) P(1) C(13) C(12) -15.2(9) . . . . yes Mo(1) P(1) C(13) C(14) 167.3(8) . . . . yes Mo(1) P(1) C(18) C(19) 105.1(9) . . . . yes Mo(1) P(1) C(18) C(23) -72.6(8) . . . . yes Mo(1) P(1) C(24) C(25) -44.4(7) . . . . yes Mo(1) P(2) C(25) C(24) -39.9(8) . . . . yes Mo(1) P(2) C(26) C(27) -24.7(9) . . . . yes Mo(1) P(2) C(26) C(31) 161.5(7) . . . . yes Mo(1) P(2) C(32) C(33) -64(1) . . . . yes Mo(1) P(2) C(32) C(37) 115(1) . . . . yes Mo(1) P(3) C(38) C(39) 84.8(8) . . . . yes Mo(1) P(3) C(38) C(43) -93.7(8) . . . . yes Mo(1) P(3) C(44) C(45) -174.0(8) . . . . yes Mo(1) P(3) C(44) C(49) 4(1) . . . . yes Mo(1) P(3) C(50) C(51) 50.7(6) . . . . yes Mo(1) P(4) C(51) C(50) 32.3(7) . . . . yes Mo(1) P(4) C(53) C(52) -8.4(9) . . . . yes Mo(1) P(4) C(53) C(54) 172.2(7) . . . . yes Mo(1) P(4) C(58) C(59) -71.0(9) . . . . yes Mo(1) P(4) C(58) C(63) 114.3(9) . . . . yes Mo(1) Si(1) C(6) C(7) 70.8(8) . . . . yes Mo(1) Si(1) C(6) C(11) -104.3(8) . . . . yes Mo(1) Si(1) C(12) C(13) 18.5(9) . . . . yes Mo(1) Si(1) C(12) C(17) -163.8(8) . . . . yes Mo(1) Si(1) C(52) C(53) 13.8(9) . . . . yes Mo(1) Si(1) C(52) C(57) -170.3(8) . . . . yes Mo(1) C(1) N(1) C(2) -176(4) . . . . yes P(1) Mo(1) P(2) C(25) 9.8(4) . . . . yes P(1) Mo(1) P(2) C(26) 126.2(4) . . . . yes P(1) Mo(1) P(2) C(32) -106.9(4) . . . . yes P(1) Mo(1) P(3) C(38) -28.2(9) . . . . yes P(1) Mo(1) P(3) C(44) -159.0(7) . . . . yes P(1) Mo(1) P(3) C(50) 90.4(8) . . . . yes P(1) Mo(1) P(4) C(51) -174.6(4) . . . . yes P(1) Mo(1) P(4) C(53) -60.4(4) . . . . yes P(1) Mo(1) P(4) C(58) 63.1(3) . . . . yes P(1) Mo(1) Si(1) C(6) -142.3(4) . . . . yes P(1) Mo(1) Si(1) C(12) -19.2(4) . . . . yes P(1) Mo(1) Si(1) C(52) 95.0(3) . . . . yes P(1) Mo(1) C(1) N(1) 0(7) . . . . yes P(1) C(13) C(12) Si(1) -2(1) . . . . yes P(1) C(13) C(12) C(17) 179.2(8) . . . . yes P(1) C(13) C(14) C(15) -178.7(8) . . . . yes P(1) C(18) C(19) C(20) -176.6(9) . . . . yes P(1) C(18) C(23) C(22) 177.4(7) . . . . yes P(1) C(24) C(25) P(2) 54.0(8) . . . . yes P(2) Mo(1) P(1) C(13) -97.8(4) . . . . yes P(2) Mo(1) P(1) C(18) 134.9(5) . . . . yes P(2) Mo(1) P(1) C(24) 15.1(4) . . . . yes P(2) Mo(1) P(3) C(38) 49.1(4) . . . . yes P(2) Mo(1) P(3) C(44) -81.7(4) . . . . yes P(2) Mo(1) P(3) C(50) 167.7(4) . . . . yes P(2) Mo(1) P(4) C(51) 71.6(6) . . . . yes P(2) Mo(1) P(4) C(53) -174.2(5) . . . . yes P(2) Mo(1) P(4) C(58) -50.7(6) . . . . yes P(2) Mo(1) Si(1) C(6) -68.8(4) . . . . yes P(2) Mo(1) Si(1) C(12) 54.3(4) . . . . yes P(2) Mo(1) Si(1) C(52) 168.4(3) . . . . yes P(2) Mo(1) C(1) N(1) -81(7) . . . . yes P(2) C(26) C(27) C(28) -175.0(8) . . . . yes P(2) C(26) C(31) C(30) 178.3(9) . . . . yes P(2) C(32) C(33) C(34) -179(1) . . . . yes P(2) C(32) C(37) C(36) 175(1) . . . . yes P(3) Mo(1) P(1) C(13) -19.4(8) . . . . yes P(3) Mo(1) P(1) C(18) -146.7(7) . . . . yes P(3) Mo(1) P(1) C(24) 93.5(8) . . . . yes P(3) Mo(1) P(2) C(25) -163.0(4) . . . . yes P(3) Mo(1) P(2) C(26) -46.5(4) . . . . yes P(3) Mo(1) P(2) C(32) 80.4(4) . . . . yes P(3) Mo(1) P(4) C(51) -1.5(4) . . . . yes P(3) Mo(1) P(4) C(53) 112.7(4) . . . . yes P(3) Mo(1) P(4) C(58) -123.8(3) . . . . yes P(3) Mo(1) Si(1) C(6) 33.1(4) . . . . yes P(3) Mo(1) Si(1) C(12) 156.2(4) . . . . yes P(3) Mo(1) Si(1) C(52) -89.7(3) . . . . yes P(3) Mo(1) C(1) N(1) -178(7) . . . . yes P(3) C(38) C(39) C(40) -179.4(7) . . . . yes P(3) C(38) C(43) C(42) 179.7(10) . . . . yes P(3) C(44) C(45) C(46) -179(1) . . . . yes P(3) C(44) C(49) C(48) -179(1) . . . . yes P(3) C(50) C(51) P(4) -52.6(7) . . . . yes P(4) Mo(1) P(1) C(13) 92.2(4) . . . . yes P(4) Mo(1) P(1) C(18) -35.1(5) . . . . yes P(4) Mo(1) P(1) C(24) -154.9(4) . . . . yes P(4) Mo(1) P(2) C(25) 125.6(5) . . . . yes P(4) Mo(1) P(2) C(26) -118.0(5) . . . . yes P(4) Mo(1) P(2) C(32) 8.9(6) . . . . yes P(4) Mo(1) P(3) C(38) -141.3(4) . . . . yes P(4) Mo(1) P(3) C(44) 87.9(4) . . . . yes P(4) Mo(1) P(3) C(50) -22.7(4) . . . . yes P(4) Mo(1) Si(1) C(6) 109.9(4) . . . . yes P(4) Mo(1) Si(1) C(12) -127.0(4) . . . . yes P(4) Mo(1) Si(1) C(52) -12.9(3) . . . . yes P(4) Mo(1) C(1) N(1) 104(7) . . . . yes P(4) C(53) C(52) Si(1) -4(1) . . . . yes P(4) C(53) C(52) C(57) 179.8(8) . . . . yes P(4) C(53) C(54) C(55) 179.7(8) . . . . yes P(4) C(58) C(59) C(60) -177(1) . . . . yes P(4) C(58) C(63) C(62) 174(1) . . . . yes Si(1) Mo(1) P(1) C(13) 19.4(4) . . . . yes Si(1) Mo(1) P(1) C(18) -107.9(4) . . . . yes Si(1) Mo(1) P(1) C(24) 132.3(4) . . . . yes Si(1) Mo(1) P(2) C(25) -61.3(4) . . . . yes Si(1) Mo(1) P(2) C(26) 55.2(4) . . . . yes Si(1) Mo(1) P(2) C(32) -177.9(4) . . . . yes Si(1) Mo(1) P(3) C(38) -66.2(4) . . . . yes Si(1) Mo(1) P(3) C(44) 163.0(4) . . . . yes Si(1) Mo(1) P(3) C(50) 52.4(4) . . . . yes Si(1) Mo(1) P(4) C(51) -101.9(4) . . . . yes Si(1) Mo(1) P(4) C(53) 12.2(4) . . . . yes Si(1) Mo(1) P(4) C(58) 135.8(3) . . . . yes Si(1) Mo(1) C(1) N(1) 54(7) . . . . yes Si(1) C(6) C(7) C(8) -177.5(7) . . . . yes Si(1) C(6) C(11) C(10) 174.9(8) . . . . yes Si(1) C(12) C(13) C(14) 174.5(8) . . . . yes Si(1) C(12) C(17) C(16) -175.0(8) . . . . yes Si(1) C(52) C(53) C(54) 175.4(8) . . . . yes Si(1) C(52) C(57) C(56) -177.7(9) . . . . yes C(1) Mo(1) P(1) C(13) 174.7(4) . . . . yes C(1) Mo(1) P(1) C(18) 47.4(5) . . . . yes C(1) Mo(1) P(1) C(24) -72.5(5) . . . . yes C(1) Mo(1) P(2) C(25) 96.1(5) . . . . yes C(1) Mo(1) P(2) C(26) -147.4(4) . . . . yes C(1) Mo(1) P(2) C(32) -20.5(4) . . . . yes C(1) Mo(1) P(3) C(38) 137.5(5) . . . . yes C(1) Mo(1) P(3) C(44) 6.7(5) . . . . yes C(1) Mo(1) P(3) C(50) -103.9(5) . . . . yes C(1) Mo(1) P(4) C(51) 101.3(4) . . . . yes C(1) Mo(1) P(4) C(53) -144.6(4) . . . . yes C(1) Mo(1) P(4) C(58) -21.0(4) . . . . yes C(1) Mo(1) Si(1) C(6) 161.2(6) . . . . yes C(1) Mo(1) Si(1) C(12) -75.7(6) . . . . yes C(1) Mo(1) Si(1) C(52) 38.5(6) . . . . yes C(1) N(1) C(2) C(3) 130(5) . . . . yes C(1) N(1) C(2) C(4) -118(5) . . . . yes C(1) N(1) C(2) C(5) 0(6) . . . . yes C(6) Si(1) C(12) C(13) 155.8(8) . . . . yes C(6) Si(1) C(12) C(17) -26.5(10) . . . . yes C(6) Si(1) C(52) C(53) -123.4(8) . . . . yes C(6) Si(1) C(52) C(57) 52.5(9) . . . . yes C(6) C(7) C(8) C(9) 1(1) . . . . yes C(6) C(11) C(10) C(9) 3(1) . . . . yes C(7) C(6) Si(1) C(12) -55.2(8) . . . . yes C(7) C(6) Si(1) C(52) -163.0(7) . . . . yes C(7) C(6) C(11) C(10) 0(1) . . . . yes C(7) C(8) C(9) C(10) 2(1) . . . . yes C(8) C(7) C(6) C(11) -2(1) . . . . yes C(8) C(9) C(10) C(11) -4(1) . . . . yes C(11) C(6) Si(1) C(12) 129.7(8) . . . . yes C(11) C(6) Si(1) C(52) 21.9(9) . . . . yes C(12) Si(1) C(52) C(53) 130.9(8) . . . . yes C(12) Si(1) C(52) C(57) -53(1) . . . . yes C(12) C(13) P(1) C(18) 123.9(8) . . . . yes C(12) C(13) P(1) C(24) -132.3(8) . . . . yes C(12) C(13) C(14) C(15) 3(1) . . . . yes C(12) C(17) C(16) C(15) -2(1) . . . . yes C(13) P(1) C(18) C(19) -28.0(9) . . . . yes C(13) P(1) C(18) C(23) 154.3(8) . . . . yes C(13) P(1) C(24) C(25) 77.8(7) . . . . yes C(13) C(12) Si(1) C(52) -99.0(9) . . . . yes C(13) C(12) C(17) C(16) 2(1) . . . . yes C(13) C(14) C(15) C(16) -3(1) . . . . yes C(14) C(13) P(1) C(18) -53.5(10) . . . . yes C(14) C(13) P(1) C(24) 50.2(10) . . . . yes C(14) C(13) C(12) C(17) -3(1) . . . . yes C(14) C(15) C(16) C(17) 3(1) . . . . yes C(17) C(12) Si(1) C(52) 78.7(10) . . . . yes C(18) P(1) C(24) C(25) -178.8(6) . . . . yes C(18) C(19) C(20) C(21) -1(2) . . . . yes C(18) C(23) C(22) C(21) 0(1) . . . . yes C(19) C(18) P(1) C(24) -131.9(9) . . . . yes C(19) C(18) C(23) C(22) 0(1) . . . . yes C(19) C(20) C(21) C(22) 1(2) . . . . yes C(20) C(19) C(18) C(23) 1(1) . . . . yes C(20) C(21) C(22) C(23) 0(1) . . . . yes C(23) C(18) P(1) C(24) 50.4(8) . . . . yes C(24) C(25) P(2) C(26) -172.3(7) . . . . yes C(24) C(25) P(2) C(32) 86.1(8) . . . . yes C(25) P(2) C(26) C(27) 95.8(8) . . . . yes C(25) P(2) C(26) C(31) -78.1(9) . . . . yes C(25) P(2) C(32) C(33) 176(1) . . . . yes C(25) P(2) C(32) C(37) -3(1) . . . . yes C(26) P(2) C(32) C(33) 74(1) . . . . yes C(26) P(2) C(32) C(37) -105(1) . . . . yes C(26) C(27) C(28) C(29) -2(1) . . . . yes C(26) C(31) C(30) C(29) -4(1) . . . . yes C(27) C(26) P(2) C(32) -159.2(7) . . . . yes C(27) C(26) C(31) C(30) 4(1) . . . . yes C(27) C(28) C(29) C(30) 1(1) . . . . yes C(28) C(27) C(26) C(31) 0(1) . . . . yes C(28) C(29) C(30) C(31) 1(1) . . . . yes C(31) C(26) P(2) C(32) 27.0(9) . . . . yes C(32) C(33) C(34) C(35) 1(2) . . . . yes C(32) C(37) C(36) C(35) 5(2) . . . . yes C(33) C(32) C(37) C(36) -4(2) . . . . yes C(33) C(34) C(35) C(36) 0(2) . . . . yes C(34) C(33) C(32) C(37) 0(2) . . . . yes C(34) C(35) C(36) C(37) -3(2) . . . . yes C(38) P(3) C(44) C(45) 45.3(10) . . . . yes C(38) P(3) C(44) C(49) -136.1(10) . . . . yes C(38) P(3) C(50) C(51) -177.3(6) . . . . yes C(38) C(39) C(40) C(41) 0(1) . . . . yes C(38) C(43) C(42) C(41) 0(1) . . . . yes C(39) C(38) P(3) C(44) -135.4(8) . . . . yes C(39) C(38) P(3) C(50) -36.1(8) . . . . yes C(39) C(38) C(43) C(42) 1(1) . . . . yes C(39) C(40) C(41) C(42) 0(1) . . . . yes C(40) C(39) C(38) C(43) 0(1) . . . . yes C(40) C(41) C(42) C(43) 0(1) . . . . yes C(43) C(38) P(3) C(44) 46.2(9) . . . . yes C(43) C(38) P(3) C(50) 145.4(8) . . . . yes C(44) P(3) C(50) C(51) -76.7(6) . . . . yes C(44) C(45) C(46) C(47) -1(2) . . . . yes C(44) C(49) C(48) C(47) 0(2) . . . . yes C(45) C(44) P(3) C(50) -58.3(10) . . . . yes C(45) C(44) C(49) C(48) 0(1) . . . . yes C(45) C(46) C(47) C(48) 0(2) . . . . yes C(46) C(45) C(44) C(49) 1(1) . . . . yes C(46) C(47) C(48) C(49) 0(2) . . . . yes C(49) C(44) P(3) C(50) 120.4(10) . . . . yes C(50) C(51) P(4) C(53) -91.7(7) . . . . yes C(50) C(51) P(4) C(58) 166.4(6) . . . . yes C(51) P(4) C(53) C(52) 111.6(8) . . . . yes C(51) P(4) C(53) C(54) -67.9(9) . . . . yes C(51) P(4) C(58) C(59) 163.0(9) . . . . yes C(51) P(4) C(58) C(63) -11(1) . . . . yes C(52) C(53) P(4) C(58) -143.9(7) . . . . yes C(52) C(53) C(54) C(55) 0(1) . . . . yes C(52) C(57) C(56) C(55) 4(1) . . . . yes C(53) P(4) C(58) C(59) 60.0(9) . . . . yes C(53) P(4) C(58) C(63) -114.7(10) . . . . yes C(53) C(52) C(57) C(56) -1(1) . . . . yes C(53) C(54) C(55) C(56) 2(1) . . . . yes C(54) C(53) P(4) C(58) 36.7(9) . . . . yes C(54) C(53) C(52) C(57) 0(1) . . . . yes C(54) C(55) C(56) C(57) -5(1) . . . . yes C(58) C(59) C(60) C(61) 4(2) . . . . yes C(58) C(63) C(62) C(61) 1(2) . . . . yes C(59) C(58) C(63) C(62) 0(1) . . . . yes C(59) C(60) C(61) C(62) -3(2) . . . . yes C(60) C(59) C(58) C(63) -2(1) . . . . yes C(60) C(61) C(62) C(63) 0(2) . . . . yes C(64) C(65) C(71) C(72) 0(2) . . . . yes C(64) C(69) C(73) C(72) 0(2) . . . . yes C(65) C(64) C(69) C(73) 0(2) . . . . yes C(65) C(71) C(72) C(73) 0(2) . . . . yes C(71) C(65) C(64) C(69) 0(2) . . . . yes C(71) C(65) C(64) C(74) -180.0 . . . . yes C(71) C(72) C(73) C(69) 0(2) . . . . yes C(73) C(69) C(64) C(74) 180.0 . . . . yes C(73) C(69) C(64) C(74) 180.0 . . . . yes #------------------------------------------------------------------------------ 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 Mo(1) Si(1) 2.519(3) . . ? C(19) C(65) 3.59(2) . 1_656 ? C(20) C(71) 3.59(2) . 1_656 ? C(34) C(73) 3.59(2) . . ? #------------------------------------------------------------------------------ data_nij135/ito_lab _database_code_CSD 194604 _audit_creation_date 'Thu May 10 13:14:52 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C65 H63 N Mo P4 Si ' _chemical_formula_moiety 'C65 H63 N Mo P4 Si ' _chemical_formula_weight 1106.14 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.473(3) _cell_length_b 20.304(5) _cell_length_c 12.078(3) _cell_angle_alpha 98.56(2) _cell_angle_beta 112.41(2) _cell_angle_gamma 78.80(2) _cell_volume 2764(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 16798 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 30.00 _diffrn_measured_fraction_theta_max 1.0001 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.0001 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.61 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 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 16115 _reflns_number_gt 10591 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1563 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 16115 _refine_ls_number_parameters 653 _refine_ls_goodness_of_fit_ref 1.495 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0011 _refine_diff_density_max 1.18 _refine_diff_density_min -1.14 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Mo' 'Mo' -1.683 0.686 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.96805(2) 0.25585(1) 0.50084(2) 0.02968(6) Uani 1.00 d . . . P(1) P 1.10045(7) 0.15569(4) 0.57259(7) 0.0365(2) Uani 1.00 d . . . P(2) P 0.84586(7) 0.20450(4) 0.57213(7) 0.0360(2) Uani 1.00 d . . . P(3) P 0.84306(7) 0.36580(4) 0.45104(7) 0.0342(2) Uani 1.00 d . . . P(4) P 1.06005(7) 0.29746(4) 0.38560(7) 0.0346(2) Uani 1.00 d . . . Si(1) Si 1.14399(8) 0.29884(4) 0.66188(8) 0.0369(2) Uani 1.00 d . . . N(1) N 0.8766(3) 0.1584(2) 0.2584(3) 0.066(1) Uani 1.00 d . . . C(1) C 0.9040(3) 0.1950(2) 0.3415(3) 0.0404(8) Uani 1.00 d . . . C(2) C 0.8391(5) 0.1201(3) 0.1449(5) 0.090(2) Uani 1.00 d . . . C(3) C 0.875(1) 0.0520(5) 0.1493(9) 0.307(5) Uani 1.00 d . . . C(4) C 0.8323(10) 0.0096(5) 0.0321(9) 0.227(4) Uani 1.00 d . . . C(5) C 0.711(1) 0.0278(4) -0.0373(7) 0.172(4) Uani 1.00 d . . . C(6) C 0.6761(8) 0.0937(5) -0.0420(9) 0.219(4) Uani 1.00 d . . . C(7) C 0.7164(6) 0.1389(4) 0.0749(6) 0.143(3) Uani 1.00 d . . . C(8) C 1.1443(3) 0.3751(2) 0.7758(3) 0.0436(8) Uani 1.00 d . . . C(9) C 1.1007(4) 0.3707(2) 0.8653(4) 0.059(1) Uani 1.00 d . . . C(10) C 1.1020(5) 0.4225(3) 0.9532(4) 0.076(2) Uani 1.00 d . . . C(11) C 1.1448(5) 0.4792(2) 0.9551(4) 0.077(2) Uani 1.00 d . . . C(12) C 1.1874(4) 0.4859(2) 0.8684(4) 0.066(1) Uani 1.00 d . . . C(13) C 1.1879(4) 0.4335(2) 0.7802(3) 0.054(1) Uani 1.00 d . . . C(14) C 1.2302(3) 0.2305(2) 0.7680(3) 0.0425(8) Uani 1.00 d . . . C(15) C 1.2088(3) 0.1649(2) 0.7261(3) 0.0441(8) Uani 1.00 d . . . C(16) C 1.2705(4) 0.1110(2) 0.7959(4) 0.059(1) Uani 1.00 d . . . C(17) C 1.3519(4) 0.1229(2) 0.9089(4) 0.071(1) Uani 1.00 d . . . C(18) C 1.3744(4) 0.1869(3) 0.9521(4) 0.070(1) Uani 1.00 d . . . C(19) C 1.3148(4) 0.2406(2) 0.8830(3) 0.059(1) Uani 1.00 d . . . C(20) C 1.1977(3) 0.1049(2) 0.4992(3) 0.0436(9) Uani 1.00 d . . . C(21) C 1.3114(3) 0.1192(2) 0.5309(4) 0.061(1) Uani 1.00 d . . . C(22) C 1.3843(4) 0.0838(3) 0.4737(5) 0.077(2) Uani 1.00 d . . . C(23) C 1.3466(5) 0.0347(3) 0.3845(5) 0.076(2) Uani 1.00 d . . . C(24) C 1.2348(5) 0.0206(2) 0.3500(5) 0.075(2) Uani 1.00 d . . . C(25) C 1.1598(4) 0.0556(2) 0.4074(4) 0.055(1) Uani 1.00 d . . . C(26) C 1.0188(3) 0.0925(2) 0.5868(3) 0.0457(9) Uani 1.00 d . . . C(27) C 0.9349(3) 0.1286(2) 0.6491(3) 0.0439(9) Uani 1.00 d . . . C(28) C 0.7818(3) 0.2438(2) 0.6846(3) 0.0431(9) Uani 1.00 d . . . C(29) C 0.7062(4) 0.2129(2) 0.7131(4) 0.061(1) Uani 1.00 d . . . C(30) C 0.6628(4) 0.2427(3) 0.8014(4) 0.073(2) Uani 1.00 d . . . C(31) C 0.6913(5) 0.3033(3) 0.8610(4) 0.077(2) Uani 1.00 d . . . C(32) C 0.7643(4) 0.3354(2) 0.8323(4) 0.066(1) Uani 1.00 d . . . C(33) C 0.8091(4) 0.3064(2) 0.7444(3) 0.051(1) Uani 1.00 d . . . C(34) C 0.7182(3) 0.1705(2) 0.4579(3) 0.0429(9) Uani 1.00 d . . . C(35) C 0.6208(3) 0.2162(2) 0.4007(4) 0.056(1) Uani 1.00 d . . . C(36) C 0.5220(4) 0.1940(3) 0.3116(4) 0.072(1) Uani 1.00 d . . . C(37) C 0.5202(4) 0.1264(3) 0.2791(4) 0.072(1) Uani 1.00 d . . . C(38) C 0.6156(4) 0.0806(2) 0.3349(4) 0.068(1) Uani 1.00 d . . . C(39) C 0.7134(3) 0.1028(2) 0.4239(4) 0.053(1) Uani 1.00 d . . . C(40) C 0.7856(3) 0.4228(2) 0.5558(3) 0.0379(8) Uani 1.00 d . . . C(41) C 0.8559(3) 0.4629(2) 0.6464(3) 0.0478(9) Uani 1.00 d . . . C(42) C 0.8135(4) 0.5058(2) 0.7251(4) 0.060(1) Uani 1.00 d . . . C(43) C 0.6979(4) 0.5084(2) 0.7152(4) 0.061(1) Uani 1.00 d . . . C(44) C 0.6265(3) 0.4692(2) 0.6268(4) 0.057(1) Uani 1.00 d . . . C(45) C 0.6700(3) 0.4261(2) 0.5474(3) 0.0491(10) Uani 1.00 d . . . C(46) C 0.7117(3) 0.3782(2) 0.3107(3) 0.0394(8) Uani 1.00 d . . . C(47) C 0.6517(3) 0.4421(2) 0.2811(4) 0.056(1) Uani 1.00 d . . . C(48) C 0.5546(4) 0.4504(2) 0.1742(4) 0.067(1) Uani 1.00 d . . . C(49) C 0.5187(4) 0.3960(3) 0.0974(4) 0.073(1) Uani 1.00 d . . . C(50) C 0.5774(4) 0.3325(3) 0.1255(4) 0.069(1) Uani 1.00 d . . . C(51) C 0.6749(3) 0.3237(2) 0.2313(3) 0.0518(10) Uani 1.00 d . . . C(52) C 0.9341(3) 0.4196(2) 0.4251(3) 0.0420(8) Uani 1.00 d . . . C(53) C 0.9827(3) 0.3813(2) 0.3329(3) 0.0442(9) Uani 1.00 d . . . C(54) C 1.2494(3) 0.3158(2) 0.5917(3) 0.0413(8) Uani 1.00 d . . . C(55) C 1.2089(3) 0.3161(2) 0.4680(3) 0.0405(8) Uani 1.00 d . . . C(56) C 1.2775(3) 0.3332(2) 0.4102(4) 0.054(1) Uani 1.00 d . . . C(57) C 1.3884(3) 0.3481(2) 0.4781(4) 0.065(1) Uani 1.00 d . . . C(58) C 1.4322(3) 0.3457(2) 0.6009(4) 0.065(1) Uani 1.00 d . . . C(59) C 1.3637(3) 0.3302(2) 0.6577(4) 0.055(1) Uani 1.00 d . . . C(60) C 1.0718(3) 0.2519(2) 0.2460(3) 0.0416(8) Uani 1.00 d . . . C(61) C 1.1649(4) 0.2005(2) 0.2525(3) 0.059(1) Uani 1.00 d . . . C(62) C 1.1765(4) 0.1655(3) 0.1499(4) 0.077(1) Uani 1.00 d . . . C(63) C 1.0964(5) 0.1810(3) 0.0385(4) 0.083(2) Uani 1.00 d . . . C(64) C 1.0039(5) 0.2283(3) 0.0312(4) 0.095(2) Uani 1.00 d . . . C(65) C 0.9898(4) 0.2635(3) 0.1332(4) 0.078(1) Uani 1.00 d . . . H(1) H 0.8793 0.1334 0.1011 0.1076 Uiso 1.00 calc . . . H(2) H 0.9578 0.0442 0.1794 0.3679 Uiso 1.00 calc . . . H(3) H 0.8472 0.0373 0.2036 0.3679 Uiso 1.00 calc . . . H(4) H 0.8769 0.0141 -0.0141 0.2727 Uiso 1.00 calc . . . H(5) H 0.8448 -0.0361 0.0491 0.2727 Uiso 1.00 calc . . . H(6) H 0.6969 0.0080 -0.1170 0.2060 Uiso 1.00 calc . . . H(7) H 0.6663 0.0104 -0.0034 0.2060 Uiso 1.00 calc . . . H(8) H 0.7033 0.1081 -0.0967 0.2633 Uiso 1.00 calc . . . H(9) H 0.5928 0.1007 -0.0725 0.2633 Uiso 1.00 calc . . . H(10) H 0.6713 0.1354 0.1213 0.1719 Uiso 1.00 calc . . . H(11) H 0.7039 0.1842 0.0559 0.1719 Uiso 1.00 calc . . . H(12) H 1.0699 0.3314 0.8653 0.0713 Uiso 1.00 calc . . . H(13) H 1.0725 0.4184 1.0133 0.0913 Uiso 1.00 calc . . . H(14) H 1.1454 0.5144 1.0165 0.0920 Uiso 1.00 calc . . . H(15) H 1.2162 0.5260 0.8688 0.0791 Uiso 1.00 calc . . . H(16) H 1.2189 0.4379 0.7215 0.0648 Uiso 1.00 calc . . . H(17) H 1.2563 0.0664 0.7655 0.0711 Uiso 1.00 calc . . . H(18) H 1.3927 0.0865 0.9571 0.0854 Uiso 1.00 calc . . . H(19) H 1.4313 0.1946 1.0299 0.0846 Uiso 1.00 calc . . . H(20) H 1.3314 0.2848 0.9139 0.0708 Uiso 1.00 calc . . . H(21) H 1.3386 0.1537 0.5924 0.0728 Uiso 1.00 calc . . . H(22) H 1.4617 0.0937 0.4968 0.0928 Uiso 1.00 calc . . . H(23) H 1.3977 0.0103 0.3461 0.0916 Uiso 1.00 calc . . . H(24) H 1.2082 -0.0132 0.2867 0.0903 Uiso 1.00 calc . . . H(25) H 1.0825 0.0454 0.3832 0.0665 Uiso 1.00 calc . . . H(26) H 0.9757 0.0734 0.5095 0.0548 Uiso 1.00 calc . . . H(27) H 1.0719 0.0579 0.6336 0.0548 Uiso 1.00 calc . . . H(28) H 0.9790 0.1418 0.7302 0.0526 Uiso 1.00 calc . . . H(29) H 0.8841 0.0988 0.6471 0.0526 Uiso 1.00 calc . . . H(30) H 0.6842 0.1712 0.6717 0.0735 Uiso 1.00 calc . . . H(31) H 0.6124 0.2207 0.8209 0.0880 Uiso 1.00 calc . . . H(32) H 0.6613 0.3231 0.9216 0.0922 Uiso 1.00 calc . . . H(33) H 0.7838 0.3777 0.8732 0.0794 Uiso 1.00 calc . . . H(34) H 0.8584 0.3292 0.7247 0.0616 Uiso 1.00 calc . . . H(35) H 0.6216 0.2631 0.4225 0.0667 Uiso 1.00 calc . . . H(36) H 0.4558 0.2258 0.2733 0.0860 Uiso 1.00 calc . . . H(37) H 0.4529 0.1114 0.2180 0.0868 Uiso 1.00 calc . . . H(38) H 0.6145 0.0337 0.3125 0.0811 Uiso 1.00 calc . . . H(39) H 0.7788 0.0707 0.4626 0.0640 Uiso 1.00 calc . . . H(40) H 0.9353 0.4609 0.6546 0.0573 Uiso 1.00 calc . . . H(41) H 0.8631 0.5335 0.7859 0.0718 Uiso 1.00 calc . . . H(42) H 0.6687 0.5375 0.7699 0.0730 Uiso 1.00 calc . . . H(43) H 0.5473 0.4714 0.6194 0.0683 Uiso 1.00 calc . . . H(44) H 0.6202 0.3985 0.4867 0.0589 Uiso 1.00 calc . . . H(45) H 0.6767 0.4804 0.3337 0.0670 Uiso 1.00 calc . . . H(46) H 0.5135 0.4942 0.1551 0.0810 Uiso 1.00 calc . . . H(47) H 0.4532 0.4019 0.0244 0.0878 Uiso 1.00 calc . . . H(48) H 0.5514 0.2945 0.0726 0.0832 Uiso 1.00 calc . . . H(49) H 0.7164 0.2798 0.2489 0.0622 Uiso 1.00 calc . . . H(50) H 0.8875 0.4607 0.3959 0.0504 Uiso 1.00 calc . . . H(51) H 0.9966 0.4289 0.4980 0.0504 Uiso 1.00 calc . . . H(52) H 1.0361 0.4056 0.3234 0.0530 Uiso 1.00 calc . . . H(53) H 0.9203 0.3757 0.2581 0.0530 Uiso 1.00 calc . . . H(54) H 1.2476 0.3345 0.3254 0.0647 Uiso 1.00 calc . . . H(55) H 1.4349 0.3600 0.4397 0.0775 Uiso 1.00 calc . . . H(56) H 1.5095 0.3548 0.6468 0.0785 Uiso 1.00 calc . . . H(57) H 1.3943 0.3292 0.7426 0.0664 Uiso 1.00 calc . . . H(58) H 1.2215 0.1894 0.3289 0.0713 Uiso 1.00 calc . . . H(59) H 1.2406 0.1303 0.1562 0.0922 Uiso 1.00 calc . . . H(60) H 1.1067 0.1583 -0.0323 0.0997 Uiso 1.00 calc . . . H(61) H 0.9466 0.2380 -0.0455 0.1141 Uiso 1.00 calc . . . H(62) H 0.9222 0.2962 0.1253 0.0933 Uiso 1.00 calc . . . H(63) H 0.990(3) 0.282(2) 0.644(3) 0.043(9) Uiso 1.00 calc . . . 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 Mo(1) 0.0276(1) 0.0283(1) 0.0322(1) -0.00320(8) 0.00891(9) 0.00467(8) P(1) 0.0328(4) 0.0315(4) 0.0423(4) -0.0011(3) 0.0101(3) 0.0072(3) P(2) 0.0342(4) 0.0364(4) 0.0396(4) -0.0054(3) 0.0134(3) 0.0075(3) P(3) 0.0300(4) 0.0303(4) 0.0419(4) -0.0023(3) 0.0122(3) 0.0055(3) P(4) 0.0294(4) 0.0379(4) 0.0373(4) -0.0030(3) 0.0117(3) 0.0075(3) Si(1) 0.0341(4) 0.0370(4) 0.0362(4) -0.0066(3) 0.0071(3) 0.0046(3) N(1) 0.073(2) 0.070(2) 0.057(2) -0.027(2) 0.025(2) -0.018(2) C(1) 0.039(2) 0.040(2) 0.044(2) -0.007(1) 0.016(1) 0.002(1) C(2) 0.087(4) 0.086(4) 0.074(3) -0.022(3) 0.014(3) -0.033(3) C(3) 0.29(1) 0.134(7) 0.197(9) 0.102(8) -0.141(9) -0.108(7) C(4) 0.21(1) 0.145(7) 0.155(8) 0.072(7) -0.045(7) -0.096(6) C(5) 0.25(1) 0.107(6) 0.107(6) -0.083(7) -0.008(7) -0.021(5) C(6) 0.148(8) 0.152(8) 0.186(9) 0.023(6) -0.074(6) -0.087(7) C(7) 0.099(5) 0.125(6) 0.119(5) 0.022(4) -0.014(4) -0.059(4) C(8) 0.039(2) 0.044(2) 0.040(2) -0.005(1) 0.005(1) 0.004(1) C(9) 0.064(2) 0.063(2) 0.050(2) -0.016(2) 0.019(2) -0.007(2) C(10) 0.087(3) 0.088(3) 0.053(2) -0.016(3) 0.030(2) -0.016(2) C(11) 0.093(4) 0.060(3) 0.065(3) -0.011(3) 0.023(3) -0.017(2) C(12) 0.075(3) 0.041(2) 0.066(3) -0.010(2) 0.007(2) 0.000(2) C(13) 0.057(2) 0.043(2) 0.053(2) -0.005(2) 0.010(2) 0.005(2) C(14) 0.036(2) 0.046(2) 0.039(2) -0.002(1) 0.006(1) 0.011(1) C(15) 0.038(2) 0.044(2) 0.045(2) -0.002(1) 0.007(1) 0.014(1) C(16) 0.054(2) 0.046(2) 0.065(2) 0.001(2) 0.004(2) 0.020(2) C(17) 0.062(3) 0.068(3) 0.064(3) 0.002(2) -0.004(2) 0.030(2) C(18) 0.058(2) 0.081(3) 0.052(2) -0.009(2) -0.008(2) 0.022(2) C(19) 0.054(2) 0.061(2) 0.048(2) -0.015(2) -0.003(2) 0.010(2) C(20) 0.039(2) 0.038(2) 0.054(2) 0.006(1) 0.018(1) 0.014(1) C(21) 0.044(2) 0.076(3) 0.060(2) -0.001(2) 0.017(2) 0.008(2) C(22) 0.050(2) 0.105(4) 0.082(3) 0.014(2) 0.032(2) 0.031(3) C(23) 0.074(3) 0.077(3) 0.088(3) 0.024(3) 0.050(3) 0.026(3) C(24) 0.110(4) 0.045(2) 0.084(3) -0.005(2) 0.053(3) -0.001(2) C(25) 0.066(2) 0.041(2) 0.068(2) -0.006(2) 0.034(2) 0.003(2) C(26) 0.043(2) 0.035(2) 0.057(2) -0.003(1) 0.013(1) 0.012(1) C(27) 0.044(2) 0.040(2) 0.051(2) -0.006(1) 0.017(1) 0.014(1) C(28) 0.041(2) 0.052(2) 0.040(2) -0.004(1) 0.017(1) 0.010(1) C(29) 0.063(2) 0.069(3) 0.066(2) -0.015(2) 0.033(2) 0.012(2) C(30) 0.068(3) 0.099(4) 0.074(3) -0.005(3) 0.044(2) 0.024(3) C(31) 0.080(3) 0.099(4) 0.056(2) 0.016(3) 0.040(2) 0.016(2) C(32) 0.079(3) 0.067(3) 0.049(2) 0.006(2) 0.028(2) 0.003(2) C(33) 0.060(2) 0.049(2) 0.046(2) 0.001(2) 0.023(2) 0.007(2) C(34) 0.039(2) 0.050(2) 0.045(2) -0.012(1) 0.017(1) 0.006(1) C(35) 0.044(2) 0.054(2) 0.062(2) -0.004(2) 0.010(2) 0.010(2) C(36) 0.049(2) 0.082(3) 0.071(3) -0.008(2) 0.003(2) 0.016(2) C(37) 0.052(2) 0.099(4) 0.063(3) -0.031(3) 0.011(2) -0.003(2) C(38) 0.059(3) 0.068(3) 0.079(3) -0.026(2) 0.025(2) -0.011(2) C(39) 0.048(2) 0.049(2) 0.063(2) -0.011(2) 0.017(2) 0.002(2) C(40) 0.036(2) 0.033(1) 0.043(2) -0.001(1) 0.014(1) 0.004(1) C(41) 0.041(2) 0.049(2) 0.053(2) -0.006(1) 0.017(1) 0.000(2) C(42) 0.065(3) 0.058(2) 0.053(2) -0.011(2) 0.022(2) -0.010(2) C(43) 0.070(3) 0.055(2) 0.060(2) 0.003(2) 0.035(2) -0.004(2) C(44) 0.046(2) 0.061(2) 0.067(2) -0.001(2) 0.028(2) 0.004(2) C(45) 0.040(2) 0.052(2) 0.055(2) -0.005(1) 0.018(2) 0.001(2) C(46) 0.030(1) 0.045(2) 0.044(2) -0.001(1) 0.013(1) 0.012(1) C(47) 0.048(2) 0.053(2) 0.062(2) 0.001(2) 0.013(2) 0.017(2) C(48) 0.053(2) 0.072(3) 0.072(3) 0.015(2) 0.017(2) 0.034(2) C(49) 0.051(2) 0.102(4) 0.051(2) 0.003(2) 0.001(2) 0.020(2) C(50) 0.059(3) 0.076(3) 0.056(2) -0.010(2) 0.004(2) 0.000(2) C(51) 0.046(2) 0.055(2) 0.047(2) -0.003(2) 0.008(2) 0.007(2) C(52) 0.039(2) 0.033(1) 0.058(2) -0.005(1) 0.018(1) 0.010(1) C(53) 0.040(2) 0.041(2) 0.056(2) 0.000(1) 0.020(1) 0.018(1) C(54) 0.032(1) 0.040(2) 0.050(2) -0.008(1) 0.011(1) 0.004(1) C(55) 0.029(1) 0.044(2) 0.049(2) -0.005(1) 0.013(1) 0.009(1) C(56) 0.038(2) 0.067(2) 0.062(2) -0.012(2) 0.019(2) 0.014(2) C(57) 0.041(2) 0.079(3) 0.085(3) -0.016(2) 0.026(2) 0.021(2) C(58) 0.031(2) 0.079(3) 0.085(3) -0.020(2) 0.009(2) 0.017(2) C(59) 0.038(2) 0.067(2) 0.057(2) -0.015(2) 0.007(2) 0.009(2) C(60) 0.037(2) 0.051(2) 0.038(2) 0.001(1) 0.014(1) 0.012(1) C(61) 0.061(2) 0.059(2) 0.044(2) 0.015(2) 0.013(2) 0.008(2) C(62) 0.070(3) 0.081(3) 0.060(3) 0.025(2) 0.021(2) -0.001(2) C(63) 0.092(4) 0.097(4) 0.046(2) 0.014(3) 0.026(2) -0.003(2) C(64) 0.100(4) 0.111(4) 0.037(2) 0.037(3) 0.008(2) 0.006(2) C(65) 0.066(3) 0.098(4) 0.042(2) 0.029(2) 0.008(2) 0.006(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Mo(1) P(1) 2.3964(8) . . yes Mo(1) P(2) 2.4568(9) . . yes Mo(1) P(3) 2.4715(8) . . yes Mo(1) P(4) 2.4315(8) . . yes Mo(1) Si(1) 2.5188(9) . . yes Mo(1) C(1) 2.091(3) . . yes P(1) C(15) 1.839(3) . . yes P(1) C(20) 1.839(3) . . yes P(1) C(26) 1.849(3) . . yes P(2) C(27) 1.856(3) . . yes P(2) C(28) 1.837(3) . . yes P(2) C(34) 1.839(3) . . yes P(3) C(40) 1.840(3) . . yes P(3) C(46) 1.863(3) . . yes P(3) C(52) 1.854(3) . . yes P(4) C(53) 1.858(3) . . yes P(4) C(55) 1.826(3) . . yes P(4) C(60) 1.842(3) . . yes Si(1) C(8) 1.911(4) . . yes Si(1) C(14) 1.904(3) . . yes Si(1) C(54) 1.918(3) . . yes N(1) C(1) 1.136(4) . . yes N(1) C(2) 1.429(5) . . yes C(2) C(3) 1.37(1) . . yes C(2) C(7) 1.444(8) . . yes C(3) C(4) 1.506(10) . . yes C(4) C(5) 1.42(1) . . yes C(5) C(6) 1.33(1) . . yes C(6) C(7) 1.531(9) . . yes C(8) C(9) 1.403(5) . . yes C(8) C(13) 1.384(5) . . yes C(9) C(10) 1.376(6) . . yes C(10) C(11) 1.354(7) . . yes C(11) C(12) 1.376(7) . . yes C(12) C(13) 1.390(5) . . yes C(14) C(15) 1.391(5) . . yes C(14) C(19) 1.402(5) . . yes C(15) C(16) 1.397(5) . . yes C(16) C(17) 1.375(6) . . yes C(17) C(18) 1.367(6) . . yes C(18) C(19) 1.385(6) . . yes C(20) C(21) 1.397(5) . . yes C(20) C(25) 1.382(5) . . yes C(21) C(22) 1.379(6) . . yes C(22) C(23) 1.360(8) . . yes C(23) C(24) 1.370(7) . . yes C(24) C(25) 1.397(6) . . yes C(26) C(27) 1.528(5) . . yes C(28) C(29) 1.394(5) . . yes C(28) C(33) 1.401(5) . . yes C(29) C(30) 1.384(6) . . yes C(30) C(31) 1.367(7) . . yes C(31) C(32) 1.383(7) . . yes C(32) C(33) 1.388(5) . . yes C(34) C(35) 1.388(5) . . yes C(34) C(39) 1.381(5) . . yes C(35) C(36) 1.392(6) . . yes C(36) C(37) 1.373(7) . . yes C(37) C(38) 1.371(7) . . yes C(38) C(39) 1.385(6) . . yes C(40) C(41) 1.382(5) . . yes C(40) C(45) 1.395(4) . . yes C(41) C(42) 1.378(5) . . yes C(42) C(43) 1.392(6) . . yes C(43) C(44) 1.365(6) . . yes C(44) C(45) 1.394(5) . . yes C(46) C(47) 1.388(5) . . yes C(46) C(51) 1.378(5) . . yes C(47) C(48) 1.397(6) . . yes C(48) C(49) 1.361(7) . . yes C(49) C(50) 1.373(7) . . yes C(50) C(51) 1.394(5) . . yes C(52) C(53) 1.512(5) . . yes C(54) C(55) 1.383(4) . . yes C(54) C(59) 1.406(4) . . yes C(55) C(56) 1.408(5) . . yes C(56) C(57) 1.378(5) . . yes C(57) C(58) 1.377(6) . . yes C(58) C(59) 1.384(6) . . yes C(60) C(61) 1.388(5) . . yes C(60) C(65) 1.377(5) . . yes C(61) C(62) 1.378(6) . . yes C(62) C(63) 1.373(6) . . yes C(63) C(64) 1.334(7) . . yes C(64) C(65) 1.383(6) . . yes #------------------------------------------------------------------------------ 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 P(1) Mo(1) P(2) 80.48(3) . . . yes P(1) Mo(1) P(3) 173.11(3) . . . yes P(1) Mo(1) P(4) 102.33(3) . . . yes P(1) Mo(1) Si(1) 75.87(3) . . . yes P(1) Mo(1) C(1) 84.32(9) . . . yes P(2) Mo(1) P(3) 99.78(3) . . . yes P(2) Mo(1) P(4) 166.98(3) . . . yes P(2) Mo(1) Si(1) 115.69(3) . . . yes P(2) Mo(1) C(1) 85.77(9) . . . yes P(3) Mo(1) P(4) 78.97(3) . . . yes P(3) Mo(1) Si(1) 97.98(3) . . . yes P(3) Mo(1) C(1) 102.57(9) . . . yes P(4) Mo(1) Si(1) 77.24(3) . . . yes P(4) Mo(1) C(1) 81.90(9) . . . yes Si(1) Mo(1) C(1) 147.20(9) . . . yes Mo(1) P(1) C(15) 115.7(1) . . . yes Mo(1) P(1) C(20) 125.3(1) . . . yes Mo(1) P(1) C(26) 110.0(1) . . . yes C(15) P(1) C(20) 98.7(2) . . . yes C(15) P(1) C(26) 101.7(2) . . . yes C(20) P(1) C(26) 102.4(2) . . . yes Mo(1) P(2) C(27) 108.7(1) . . . yes Mo(1) P(2) C(28) 125.8(1) . . . yes Mo(1) P(2) C(34) 117.4(1) . . . yes C(27) P(2) C(28) 99.0(2) . . . yes C(27) P(2) C(34) 102.4(2) . . . yes C(28) P(2) C(34) 100.0(2) . . . yes Mo(1) P(3) C(40) 124.1(1) . . . yes Mo(1) P(3) C(46) 123.7(1) . . . yes Mo(1) P(3) C(52) 106.4(1) . . . yes C(40) P(3) C(46) 98.6(1) . . . yes C(40) P(3) C(52) 100.6(1) . . . yes C(46) P(3) C(52) 98.7(1) . . . yes Mo(1) P(4) C(53) 111.3(1) . . . yes Mo(1) P(4) C(55) 116.2(1) . . . yes Mo(1) P(4) C(60) 122.2(1) . . . yes C(53) P(4) C(55) 100.8(2) . . . yes C(53) P(4) C(60) 101.3(2) . . . yes C(55) P(4) C(60) 102.2(2) . . . yes Mo(1) Si(1) C(8) 127.3(1) . . . yes Mo(1) Si(1) C(14) 109.5(1) . . . yes Mo(1) Si(1) C(54) 110.0(1) . . . yes C(8) Si(1) C(14) 100.1(1) . . . yes C(8) Si(1) C(54) 102.6(1) . . . yes C(14) Si(1) C(54) 105.4(1) . . . yes C(1) N(1) C(2) 172.3(5) . . . yes Mo(1) C(1) N(1) 174.7(3) . . . yes N(1) C(2) C(3) 114.8(6) . . . yes N(1) C(2) C(7) 112.9(5) . . . yes C(3) C(2) C(7) 114.2(7) . . . yes C(2) C(3) C(4) 116.3(8) . . . yes C(3) C(4) C(5) 113.8(8) . . . yes C(4) C(5) C(6) 114.3(8) . . . yes C(5) C(6) C(7) 118.1(9) . . . yes C(2) C(7) C(6) 111.9(6) . . . yes Si(1) C(8) C(9) 117.5(3) . . . yes Si(1) C(8) C(13) 125.5(3) . . . yes C(9) C(8) C(13) 117.0(3) . . . yes C(8) C(9) C(10) 121.0(4) . . . yes C(9) C(10) C(11) 120.8(5) . . . yes C(10) C(11) C(12) 120.3(4) . . . yes C(11) C(12) C(13) 119.3(4) . . . yes C(8) C(13) C(12) 121.7(4) . . . yes Si(1) C(14) C(15) 116.8(2) . . . yes Si(1) C(14) C(19) 125.5(3) . . . yes C(15) C(14) C(19) 117.7(3) . . . yes P(1) C(15) C(14) 114.9(2) . . . yes P(1) C(15) C(16) 124.1(3) . . . yes C(14) C(15) C(16) 121.0(3) . . . yes C(15) C(16) C(17) 119.8(4) . . . yes C(16) C(17) C(18) 120.3(4) . . . yes C(17) C(18) C(19) 120.4(4) . . . yes C(14) C(19) C(18) 120.8(4) . . . yes P(1) C(20) C(21) 119.5(3) . . . yes P(1) C(20) C(25) 122.1(3) . . . yes C(21) C(20) C(25) 118.2(3) . . . yes C(20) C(21) C(22) 120.6(4) . . . yes C(21) C(22) C(23) 120.6(5) . . . yes C(22) C(23) C(24) 120.0(4) . . . yes C(23) C(24) C(25) 120.3(5) . . . yes C(20) C(25) C(24) 120.2(4) . . . yes P(1) C(26) C(27) 107.6(2) . . . yes P(2) C(27) C(26) 110.6(2) . . . yes P(2) C(28) C(29) 121.9(3) . . . yes P(2) C(28) C(33) 119.8(3) . . . yes C(29) C(28) C(33) 118.3(3) . . . yes C(28) C(29) C(30) 120.5(4) . . . yes C(29) C(30) C(31) 120.9(4) . . . yes C(30) C(31) C(32) 119.6(4) . . . yes C(31) C(32) C(33) 120.5(4) . . . yes C(28) C(33) C(32) 120.2(4) . . . yes P(2) C(34) C(35) 117.6(3) . . . yes P(2) C(34) C(39) 124.5(3) . . . yes C(35) C(34) C(39) 117.8(3) . . . yes C(34) C(35) C(36) 120.7(4) . . . yes C(35) C(36) C(37) 120.1(4) . . . yes C(36) C(37) C(38) 120.0(4) . . . yes C(37) C(38) C(39) 119.7(4) . . . yes C(34) C(39) C(38) 121.7(4) . . . yes P(3) C(40) C(41) 121.2(2) . . . yes P(3) C(40) C(45) 121.0(2) . . . yes C(41) C(40) C(45) 117.9(3) . . . yes C(40) C(41) C(42) 121.5(3) . . . yes C(41) C(42) C(43) 119.7(4) . . . yes C(42) C(43) C(44) 120.0(3) . . . yes C(43) C(44) C(45) 119.9(4) . . . yes C(40) C(45) C(44) 121.0(3) . . . yes P(3) C(46) C(47) 121.3(3) . . . yes P(3) C(46) C(51) 120.1(3) . . . yes C(47) C(46) C(51) 118.5(3) . . . yes C(46) C(47) C(48) 120.4(4) . . . yes C(47) C(48) C(49) 120.4(4) . . . yes C(48) C(49) C(50) 119.9(4) . . . yes C(49) C(50) C(51) 120.3(4) . . . yes C(46) C(51) C(50) 120.6(4) . . . yes P(3) C(52) C(53) 107.5(2) . . . yes P(4) C(53) C(52) 108.8(2) . . . yes Si(1) C(54) C(55) 117.7(2) . . . yes Si(1) C(54) C(59) 124.4(3) . . . yes C(55) C(54) C(59) 117.8(3) . . . yes P(4) C(55) C(54) 116.5(2) . . . yes P(4) C(55) C(56) 122.2(3) . . . yes C(54) C(55) C(56) 121.3(3) . . . yes C(55) C(56) C(57) 119.3(4) . . . yes C(56) C(57) C(58) 120.5(4) . . . yes C(57) C(58) C(59) 120.1(3) . . . yes C(54) C(59) C(58) 121.1(4) . . . yes P(4) C(60) C(61) 119.4(3) . . . yes P(4) C(60) C(65) 123.7(3) . . . yes C(61) C(60) C(65) 116.8(3) . . . yes C(60) C(61) C(62) 120.9(4) . . . yes C(61) C(62) C(63) 120.6(4) . . . yes C(62) C(63) C(64) 119.0(4) . . . yes C(63) C(64) C(65) 121.2(4) . . . yes C(60) C(65) C(64) 121.3(4) . . . yes #------------------------------------------------------------------------------ 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 Mo(1) P(1) C(15) C(14) -21.4(3) . . . . yes Mo(1) P(1) C(15) C(16) 161.5(3) . . . . yes Mo(1) P(1) C(20) C(21) 90.8(3) . . . . yes Mo(1) P(1) C(20) C(25) -84.8(3) . . . . yes Mo(1) P(1) C(26) C(27) -45.7(3) . . . . yes Mo(1) P(2) C(27) C(26) -35.8(3) . . . . yes Mo(1) P(2) C(28) C(29) 175.1(3) . . . . yes Mo(1) P(2) C(28) C(33) -5.1(3) . . . . yes Mo(1) P(2) C(34) C(35) -75.0(3) . . . . yes Mo(1) P(2) C(34) C(39) 104.0(3) . . . . yes Mo(1) P(3) C(40) C(41) 78.0(3) . . . . yes Mo(1) P(3) C(40) C(45) -100.9(3) . . . . yes Mo(1) P(3) C(46) C(47) -173.2(2) . . . . yes Mo(1) P(3) C(46) C(51) 4.3(3) . . . . yes Mo(1) P(3) C(52) C(53) 53.1(2) . . . . yes Mo(1) P(4) C(53) C(52) 32.5(3) . . . . yes Mo(1) P(4) C(55) C(54) -10.3(3) . . . . yes Mo(1) P(4) C(55) C(56) 172.7(3) . . . . yes Mo(1) P(4) C(60) C(61) -84.8(3) . . . . yes Mo(1) P(4) C(60) C(65) 92.1(4) . . . . yes Mo(1) Si(1) C(8) C(9) 68.9(3) . . . . yes Mo(1) Si(1) C(8) C(13) -113.7(3) . . . . yes Mo(1) Si(1) C(14) C(15) 18.3(3) . . . . yes Mo(1) Si(1) C(14) C(19) -163.1(3) . . . . yes Mo(1) Si(1) C(54) C(55) 12.5(3) . . . . yes Mo(1) Si(1) C(54) C(59) -169.8(3) . . . . yes Mo(1) C(1) N(1) C(2) -132(3) . . . . yes P(1) Mo(1) P(2) C(27) 6.1(1) . . . . yes P(1) Mo(1) P(2) C(28) 122.7(1) . . . . yes P(1) Mo(1) P(2) C(34) -109.4(1) . . . . yes P(1) Mo(1) P(3) C(40) -38.7(3) . . . . yes P(1) Mo(1) P(3) C(46) -170.5(2) . . . . yes P(1) Mo(1) P(3) C(52) 76.8(3) . . . . yes P(1) Mo(1) P(4) C(53) -173.6(1) . . . . yes P(1) Mo(1) P(4) C(55) -59.1(1) . . . . yes P(1) Mo(1) P(4) C(60) 66.9(1) . . . . yes P(1) Mo(1) Si(1) C(8) -141.9(1) . . . . yes P(1) Mo(1) Si(1) C(14) -21.8(1) . . . . yes P(1) Mo(1) Si(1) C(54) 93.5(1) . . . . yes P(1) Mo(1) C(1) N(1) -12(3) . . . . yes P(1) C(15) C(14) Si(1) 0.7(4) . . . . yes P(1) C(15) C(14) C(19) -178.0(3) . . . . yes P(1) C(15) C(16) C(17) 178.4(4) . . . . yes P(1) C(20) C(21) C(22) -177.3(3) . . . . yes P(1) C(20) C(25) C(24) 176.7(3) . . . . yes P(1) C(26) C(27) P(2) 51.5(3) . . . . yes P(2) Mo(1) P(1) C(15) -95.9(1) . . . . yes P(2) Mo(1) P(1) C(20) 141.0(1) . . . . yes P(2) Mo(1) P(1) C(26) 18.5(1) . . . . yes P(2) Mo(1) P(3) C(40) 52.9(1) . . . . yes P(2) Mo(1) P(3) C(46) -79.0(1) . . . . yes P(2) Mo(1) P(3) C(52) 168.4(1) . . . . yes P(2) Mo(1) P(4) C(53) 85.2(2) . . . . yes P(2) Mo(1) P(4) C(55) -160.3(2) . . . . yes P(2) Mo(1) P(4) C(60) -34.3(2) . . . . yes P(2) Mo(1) Si(1) C(8) -70.0(1) . . . . yes P(2) Mo(1) Si(1) C(14) 50.1(1) . . . . yes P(2) Mo(1) Si(1) C(54) 165.4(1) . . . . yes P(2) Mo(1) C(1) N(1) -93(3) . . . . yes P(2) C(28) C(29) C(30) 177.6(3) . . . . yes P(2) C(28) C(33) C(32) -177.8(3) . . . . yes P(2) C(34) C(35) C(36) 178.7(4) . . . . yes P(2) C(34) C(39) C(38) -178.2(3) . . . . yes P(3) Mo(1) P(1) C(15) -3.1(3) . . . . yes P(3) Mo(1) P(1) C(20) -126.3(3) . . . . yes P(3) Mo(1) P(1) C(26) 111.3(3) . . . . yes P(3) Mo(1) P(2) C(27) -167.0(1) . . . . yes P(3) Mo(1) P(2) C(28) -50.3(1) . . . . yes P(3) Mo(1) P(2) C(34) 77.6(1) . . . . yes P(3) Mo(1) P(4) C(53) -0.5(1) . . . . yes P(3) Mo(1) P(4) C(55) 114.0(1) . . . . yes P(3) Mo(1) P(4) C(60) -120.0(1) . . . . yes P(3) Mo(1) Si(1) C(8) 34.9(1) . . . . yes P(3) Mo(1) Si(1) C(14) 155.1(1) . . . . yes P(3) Mo(1) Si(1) C(54) -89.6(1) . . . . yes P(3) Mo(1) C(1) N(1) 167(3) . . . . yes P(3) C(40) C(41) C(42) 179.9(3) . . . . yes P(3) C(40) C(45) C(44) 180.0(3) . . . . yes P(3) C(46) C(47) C(48) 178.8(3) . . . . yes P(3) C(46) C(51) C(50) -179.4(3) . . . . yes P(3) C(52) C(53) P(4) -54.3(3) . . . . yes P(4) Mo(1) P(1) C(15) 97.1(1) . . . . yes P(4) Mo(1) P(1) C(20) -26.1(1) . . . . yes P(4) Mo(1) P(1) C(26) -148.5(1) . . . . yes P(4) Mo(1) P(2) C(27) 109.7(2) . . . . yes P(4) Mo(1) P(2) C(28) -133.7(2) . . . . yes P(4) Mo(1) P(2) C(34) -5.8(2) . . . . yes P(4) Mo(1) P(3) C(40) -140.3(1) . . . . yes P(4) Mo(1) P(3) C(46) 87.9(1) . . . . yes P(4) Mo(1) P(3) C(52) -24.8(1) . . . . yes P(4) Mo(1) Si(1) C(8) 111.6(1) . . . . yes P(4) Mo(1) Si(1) C(14) -128.2(1) . . . . yes P(4) Mo(1) Si(1) C(54) -12.9(1) . . . . yes P(4) Mo(1) C(1) N(1) 90(3) . . . . yes P(4) C(55) C(54) Si(1) -2.0(4) . . . . yes P(4) C(55) C(54) C(59) -179.8(3) . . . . yes P(4) C(55) C(56) C(57) 178.7(3) . . . . yes P(4) C(60) C(61) C(62) -179.9(4) . . . . yes P(4) C(60) C(65) C(64) 179.1(5) . . . . yes Si(1) Mo(1) P(1) C(15) 23.8(1) . . . . yes Si(1) Mo(1) P(1) C(20) -99.3(1) . . . . yes Si(1) Mo(1) P(1) C(26) 138.3(1) . . . . yes Si(1) Mo(1) P(2) C(27) -63.1(1) . . . . yes Si(1) Mo(1) P(2) C(28) 53.5(1) . . . . yes Si(1) Mo(1) P(2) C(34) -178.6(1) . . . . yes Si(1) Mo(1) P(3) C(40) -65.0(1) . . . . yes Si(1) Mo(1) P(3) C(46) 163.1(1) . . . . yes Si(1) Mo(1) P(3) C(52) 50.5(1) . . . . yes Si(1) Mo(1) P(4) C(53) -101.4(1) . . . . yes Si(1) Mo(1) P(4) C(55) 13.1(1) . . . . yes Si(1) Mo(1) P(4) C(60) 139.1(1) . . . . yes Si(1) Mo(1) C(1) N(1) 39(3) . . . . yes Si(1) C(8) C(9) C(10) 177.6(4) . . . . yes Si(1) C(8) C(13) C(12) -178.2(3) . . . . yes Si(1) C(14) C(15) C(16) 177.9(3) . . . . yes Si(1) C(14) C(19) C(18) -178.6(4) . . . . yes Si(1) C(54) C(55) C(56) 175.1(3) . . . . yes Si(1) C(54) C(59) C(58) -176.2(3) . . . . yes N(1) C(2) C(3) C(4) 177(1) . . . . yes N(1) C(2) C(7) C(6) -175.7(8) . . . . yes C(1) Mo(1) P(1) C(15) 177.5(2) . . . . yes C(1) Mo(1) P(1) C(20) 54.3(2) . . . . yes C(1) Mo(1) P(1) C(26) -68.1(2) . . . . yes C(1) Mo(1) P(2) C(27) 91.0(2) . . . . yes C(1) Mo(1) P(2) C(28) -152.4(2) . . . . yes C(1) Mo(1) P(2) C(34) -24.5(2) . . . . yes C(1) Mo(1) P(3) C(40) 140.7(2) . . . . yes C(1) Mo(1) P(3) C(46) 8.8(2) . . . . yes C(1) Mo(1) P(3) C(52) -103.8(1) . . . . yes C(1) Mo(1) P(4) C(53) 104.0(2) . . . . yes C(1) Mo(1) P(4) C(55) -141.4(2) . . . . yes C(1) Mo(1) P(4) C(60) -15.5(1) . . . . yes C(1) Mo(1) Si(1) C(8) 163.5(2) . . . . yes C(1) Mo(1) Si(1) C(14) -76.4(2) . . . . yes C(1) Mo(1) Si(1) C(54) 38.9(2) . . . . yes C(1) N(1) C(2) C(3) 160(3) . . . . yes C(1) N(1) C(2) C(7) -66(3) . . . . yes C(2) C(3) C(4) C(5) -44(1) . . . . yes C(2) C(7) C(6) C(5) 43(1) . . . . yes C(3) C(2) C(7) C(6) -42(1) . . . . yes C(3) C(4) C(5) C(6) 43(1) . . . . yes C(4) C(3) C(2) C(7) 44(1) . . . . yes C(4) C(5) C(6) C(7) -44(1) . . . . yes C(8) Si(1) C(14) C(15) 154.0(3) . . . . yes C(8) Si(1) C(14) C(19) -27.5(4) . . . . yes C(8) Si(1) C(54) C(55) -125.3(3) . . . . yes C(8) Si(1) C(54) C(59) 52.4(3) . . . . yes C(8) C(9) C(10) C(11) 0.4(8) . . . . yes C(8) C(13) C(12) C(11) 1.4(6) . . . . yes C(9) C(8) Si(1) C(14) -55.2(3) . . . . yes C(9) C(8) Si(1) C(54) -163.6(3) . . . . yes C(9) C(8) C(13) C(12) -0.8(6) . . . . yes C(9) C(10) C(11) C(12) 0.3(8) . . . . yes C(10) C(9) C(8) C(13) -0.1(6) . . . . yes C(10) C(11) C(12) C(13) -1.1(8) . . . . yes C(13) C(8) Si(1) C(14) 122.3(3) . . . . yes C(13) C(8) Si(1) C(54) 13.9(3) . . . . yes C(14) Si(1) C(54) C(55) 130.4(3) . . . . yes C(14) Si(1) C(54) C(59) -51.9(3) . . . . yes C(14) C(15) P(1) C(20) 114.8(3) . . . . yes C(14) C(15) P(1) C(26) -140.5(3) . . . . yes C(14) C(15) C(16) C(17) 1.4(7) . . . . yes C(14) C(19) C(18) C(17) 0.2(8) . . . . yes C(15) P(1) C(20) C(21) -39.4(3) . . . . yes C(15) P(1) C(20) C(25) 145.0(3) . . . . yes C(15) P(1) C(26) C(27) 77.4(3) . . . . yes C(15) C(14) Si(1) C(54) -99.9(3) . . . . yes C(15) C(14) C(19) C(18) -0.1(6) . . . . yes C(15) C(16) C(17) C(18) -1.4(8) . . . . yes C(16) C(15) P(1) C(20) -62.3(4) . . . . yes C(16) C(15) P(1) C(26) 42.4(4) . . . . yes C(16) C(15) C(14) C(19) -0.7(6) . . . . yes C(16) C(17) C(18) C(19) 0.5(8) . . . . yes C(19) C(14) Si(1) C(54) 78.6(4) . . . . yes C(20) P(1) C(26) C(27) 179.2(2) . . . . yes C(20) C(21) C(22) C(23) 0.7(7) . . . . yes C(20) C(25) C(24) C(23) 0.2(7) . . . . yes C(21) C(20) P(1) C(26) -143.5(3) . . . . yes C(21) C(20) C(25) C(24) 1.0(6) . . . . yes C(21) C(22) C(23) C(24) 0.6(8) . . . . yes C(22) C(21) C(20) C(25) -1.5(6) . . . . yes C(22) C(23) C(24) C(25) -1.1(8) . . . . yes C(25) C(20) P(1) C(26) 40.9(3) . . . . yes C(26) C(27) P(2) C(28) -168.6(2) . . . . yes C(26) C(27) P(2) C(34) 89.1(3) . . . . yes C(27) P(2) C(28) C(29) -64.0(3) . . . . yes C(27) P(2) C(28) C(33) 115.9(3) . . . . yes C(27) P(2) C(34) C(35) 166.1(3) . . . . yes C(27) P(2) C(34) C(39) -14.9(3) . . . . yes C(28) P(2) C(34) C(35) 64.5(3) . . . . yes C(28) P(2) C(34) C(39) -116.5(3) . . . . yes C(28) C(29) C(30) C(31) 1.1(7) . . . . yes C(28) C(33) C(32) C(31) -0.7(6) . . . . yes C(29) C(28) P(2) C(34) 40.4(3) . . . . yes C(29) C(28) C(33) C(32) 2.0(6) . . . . yes C(29) C(30) C(31) C(32) 0.2(8) . . . . yes C(30) C(29) C(28) C(33) -2.2(6) . . . . yes C(30) C(31) C(32) C(33) -0.5(7) . . . . yes C(33) C(28) P(2) C(34) -139.7(3) . . . . yes C(34) C(35) C(36) C(37) -0.2(7) . . . . yes C(34) C(39) C(38) C(37) -0.6(7) . . . . yes C(35) C(34) C(39) C(38) 0.7(6) . . . . yes C(35) C(36) C(37) C(38) 0.3(8) . . . . yes C(36) C(35) C(34) C(39) -0.3(6) . . . . yes C(36) C(37) C(38) C(39) 0.1(7) . . . . yes C(40) P(3) C(46) C(47) 45.4(3) . . . . yes C(40) P(3) C(46) C(51) -137.1(3) . . . . yes C(40) P(3) C(52) C(53) -176.4(2) . . . . yes C(40) C(41) C(42) C(43) 1.0(6) . . . . yes C(40) C(45) C(44) C(43) -0.8(6) . . . . yes C(41) C(40) P(3) C(46) -140.8(3) . . . . yes C(41) C(40) P(3) C(52) -40.3(3) . . . . yes C(41) C(40) C(45) C(44) 1.0(5) . . . . yes C(41) C(42) C(43) C(44) -0.8(7) . . . . yes C(42) C(41) C(40) C(45) -1.1(6) . . . . yes C(42) C(43) C(44) C(45) 0.7(7) . . . . yes C(45) C(40) P(3) C(46) 40.2(3) . . . . yes C(45) C(40) P(3) C(52) 140.8(3) . . . . yes C(46) P(3) C(52) C(53) -75.9(2) . . . . yes C(46) C(47) C(48) C(49) -0.7(7) . . . . yes C(46) C(51) C(50) C(49) 1.8(7) . . . . yes C(47) C(46) P(3) C(52) -56.8(3) . . . . yes C(47) C(46) C(51) C(50) -1.9(6) . . . . yes C(47) C(48) C(49) C(50) 0.7(8) . . . . yes C(48) C(47) C(46) C(51) 1.3(6) . . . . yes C(48) C(49) C(50) C(51) -1.2(8) . . . . yes C(51) C(46) P(3) C(52) 120.7(3) . . . . yes C(52) C(53) P(4) C(55) -91.2(2) . . . . yes C(52) C(53) P(4) C(60) 163.9(2) . . . . yes C(53) P(4) C(55) C(54) 110.1(3) . . . . yes C(53) P(4) C(55) C(56) -67.0(3) . . . . yes C(53) P(4) C(60) C(61) 151.0(3) . . . . yes C(53) P(4) C(60) C(65) -32.1(4) . . . . yes C(54) C(55) P(4) C(60) -145.8(3) . . . . yes C(54) C(55) C(56) C(57) 1.8(6) . . . . yes C(54) C(59) C(58) C(57) 0.8(7) . . . . yes C(55) P(4) C(60) C(61) 47.2(3) . . . . yes C(55) P(4) C(60) C(65) -135.9(4) . . . . yes C(55) C(54) C(59) C(58) 1.5(6) . . . . yes C(55) C(56) C(57) C(58) 0.6(7) . . . . yes C(56) C(55) P(4) C(60) 37.2(3) . . . . yes C(56) C(55) C(54) C(59) -2.7(5) . . . . yes C(56) C(57) C(58) C(59) -1.8(7) . . . . yes C(60) C(61) C(62) C(63) 0.5(9) . . . . yes C(60) C(65) C(64) C(63) 1(1) . . . . yes C(61) C(60) C(65) C(64) -3.9(8) . . . . yes C(61) C(62) C(63) C(64) -3.2(10) . . . . yes C(62) C(61) C(60) C(65) 3.0(7) . . . . yes C(62) C(63) C(64) C(65) 2(1) . . . . yes C(62) C(63) C(64) C(65) 2(1) . . . . yes #------------------------------------------------------------------------------ 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 Mo(1) Si(1) 2.5188(9) . . ? C(30) C(58) 3.517(7) . 1_455 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_nij134/ito_lab/YNU _database_code_CSD 194605 _audit_creation_date 'Tue Jan 23 15:12:34 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C67 H61 N Mo P4 Si ' _chemical_formula_moiety 'C67 H61 N Mo P4 Si ' _chemical_formula_weight 1128.15 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.298(6) _cell_length_b 17.097(9) _cell_length_c 12.788(4) _cell_angle_alpha 104.04(4) _cell_angle_beta 113.30(3) _cell_angle_gamma 90.16(5) _cell_volume 2768(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 12.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 13141 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0001 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0001 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 16.64 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 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 12717 _reflns_number_gt 7186 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1273 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 12717 _refine_ls_number_parameters 667 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0356 _refine_diff_density_max 0.50 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Mo' 'Mo' -1.683 0.686 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.22534(2) 0.26028(2) 0.28652(2) 0.02479(7) Uani 1.00 d . . . P(1) P 0.36077(6) 0.32735(5) 0.47590(7) 0.0293(2) Uani 1.00 d . . . P(2) P 0.19014(7) 0.40473(5) 0.30224(8) 0.0322(2) Uani 1.00 d . . . P(3) P 0.08726(6) 0.18921(5) 0.09593(8) 0.0326(2) Uani 1.00 d . . . P(4) P 0.27447(6) 0.12402(5) 0.27313(8) 0.0300(2) Uani 1.00 d . . . Si(1) Si 0.17719(7) 0.21374(5) 0.43620(8) 0.0281(2) Uani 1.00 d . . . N(1) N 0.3666(3) 0.2710(2) 0.1440(3) 0.050(1) Uani 1.00 d . . . C(1) C 0.3165(2) 0.2693(2) 0.1971(3) 0.0327(8) Uani 1.00 d . . . C(2) C 0.4230(3) 0.2719(2) 0.0766(3) 0.043(1) Uani 1.00 d . . . C(3) C 0.3874(3) 0.2197(3) -0.0364(4) 0.051(1) Uani 1.00 d . . . C(4) C 0.4419(4) 0.2240(3) -0.1038(4) 0.064(1) Uani 1.00 d . . . C(5) C 0.5285(4) 0.2781(4) -0.0607(5) 0.072(2) Uani 1.00 d . . . C(6) C 0.5637(3) 0.3266(3) 0.0520(5) 0.064(2) Uani 1.00 d . . . C(7) C 0.5146(3) 0.3240(3) 0.1255(4) 0.053(1) Uani 1.00 d . . . C(8) C 0.2932(4) 0.1604(4) -0.0844(5) 0.078(2) Uani 1.00 d . . . C(9) C 0.5565(4) 0.3729(3) 0.2505(5) 0.079(2) Uani 1.00 d . . . C(10) C 0.0438(2) 0.1838(2) 0.4256(3) 0.0346(9) Uani 1.00 d . . . C(11) C 0.0107(3) 0.1071(3) 0.4232(4) 0.051(1) Uani 1.00 d . . . C(12) C -0.0861(4) 0.0891(3) 0.4202(4) 0.068(2) Uani 1.00 d . . . C(13) C -0.1498(3) 0.1480(4) 0.4202(4) 0.069(2) Uani 1.00 d . . . C(14) C -0.1205(3) 0.2239(3) 0.4203(4) 0.062(1) Uani 1.00 d . . . C(15) C -0.0240(3) 0.2419(3) 0.4229(3) 0.047(1) Uani 1.00 d . . . C(16) C 0.2385(2) 0.2925(2) 0.5841(3) 0.0315(8) Uani 1.00 d . . . C(17) C 0.3264(2) 0.3407(2) 0.6030(3) 0.0318(8) Uani 1.00 d . . . C(18) C 0.3839(3) 0.3937(2) 0.7128(3) 0.0439(10) Uani 1.00 d . . . C(19) C 0.3529(3) 0.4015(3) 0.8042(3) 0.052(1) Uani 1.00 d . . . C(20) C 0.2669(3) 0.3562(3) 0.7875(3) 0.050(1) Uani 1.00 d . . . C(21) C 0.2106(3) 0.3017(2) 0.6797(3) 0.041(1) Uani 1.00 d . . . C(22) C 0.4911(2) 0.2974(2) 0.5447(3) 0.0362(9) Uani 1.00 d . . . C(23) C 0.5036(3) 0.2345(2) 0.5991(4) 0.049(1) Uani 1.00 d . . . C(24) C 0.5987(4) 0.2084(3) 0.6494(4) 0.064(1) Uani 1.00 d . . . C(25) C 0.6822(4) 0.2456(3) 0.6449(5) 0.081(2) Uani 1.00 d . . . C(26) C 0.6719(3) 0.3071(3) 0.5930(5) 0.079(2) Uani 1.00 d . . . C(27) C 0.5765(3) 0.3336(3) 0.5425(4) 0.055(1) Uani 1.00 d . . . C(28) C 0.3870(3) 0.4347(2) 0.4828(3) 0.0377(9) Uani 1.00 d . . . C(29) C 0.2844(3) 0.4692(2) 0.4468(3) 0.0406(10) Uani 1.00 d . . . C(30) C 0.0688(3) 0.4380(2) 0.3081(3) 0.0395(10) Uani 1.00 d . . . C(31) C -0.0170(3) 0.3831(2) 0.2545(4) 0.053(1) Uani 1.00 d . . . C(32) C -0.1106(3) 0.4053(3) 0.2553(5) 0.068(2) Uani 1.00 d . . . C(33) C -0.1167(4) 0.4825(3) 0.3118(5) 0.068(2) Uani 1.00 d . . . C(34) C -0.0326(4) 0.5381(3) 0.3629(5) 0.074(2) Uani 1.00 d . . . C(35) C 0.0603(4) 0.5167(3) 0.3629(5) 0.067(1) Uani 1.00 d . . . C(36) C 0.2074(3) 0.4624(2) 0.2044(3) 0.0399(10) Uani 1.00 d . . . C(37) C 0.1327(4) 0.5064(3) 0.1440(4) 0.066(2) Uani 1.00 d . . . C(38) C 0.1496(5) 0.5475(3) 0.0703(5) 0.084(2) Uani 1.00 d . . . C(39) C 0.2391(5) 0.5459(3) 0.0568(5) 0.077(2) Uani 1.00 d . . . C(40) C 0.3140(4) 0.5025(3) 0.1161(4) 0.069(2) Uani 1.00 d . . . C(41) C 0.2970(3) 0.4617(2) 0.1891(4) 0.052(1) Uani 1.00 d . . . C(42) C -0.0477(3) 0.1754(2) 0.0771(3) 0.0384(9) Uani 1.00 d . . . C(43) C -0.1226(3) 0.2181(3) 0.0130(4) 0.062(1) Uani 1.00 d . . . C(44) C -0.2210(3) 0.2112(4) 0.0055(5) 0.076(2) Uani 1.00 d . . . C(45) C -0.2476(3) 0.1608(3) 0.0607(5) 0.069(1) Uani 1.00 d . . . C(46) C -0.1769(3) 0.1171(3) 0.1227(4) 0.057(1) Uani 1.00 d . . . C(47) C -0.0767(3) 0.1247(2) 0.1313(3) 0.044(1) Uani 1.00 d . . . C(48) C 0.0597(3) 0.2165(2) -0.0439(3) 0.0413(10) Uani 1.00 d . . . C(49) C 0.0058(4) 0.1617(3) -0.1535(4) 0.064(1) Uani 1.00 d . . . C(50) C -0.0255(4) 0.1865(4) -0.2559(4) 0.076(2) Uani 1.00 d . . . C(51) C -0.0038(4) 0.2654(4) -0.2505(4) 0.069(2) Uani 1.00 d . . . C(52) C 0.0502(4) 0.3205(3) -0.1448(4) 0.063(1) Uani 1.00 d . . . C(53) C 0.0826(3) 0.2952(3) -0.0408(3) 0.050(1) Uani 1.00 d . . . C(54) C 0.1132(3) 0.0819(2) 0.0528(3) 0.0379(9) Uani 1.00 d . . . C(55) C 0.1661(3) 0.0495(2) 0.1596(3) 0.0380(9) Uani 1.00 d . . . C(56) C 0.2489(2) 0.1226(2) 0.4716(3) 0.0323(8) Uani 1.00 d . . . C(57) C 0.2976(3) 0.0847(2) 0.4010(3) 0.0332(9) Uani 1.00 d . . . C(58) C 0.3561(3) 0.0214(2) 0.4277(4) 0.048(1) Uani 1.00 d . . . C(59) C 0.3665(3) -0.0040(3) 0.5265(4) 0.058(1) Uani 1.00 d . . . C(60) C 0.3189(3) 0.0329(3) 0.5968(4) 0.053(1) Uani 1.00 d . . . C(61) C 0.2591(3) 0.0952(2) 0.5695(3) 0.042(1) Uani 1.00 d . . . C(62) C 0.3839(3) 0.0955(2) 0.2348(3) 0.0350(9) Uani 1.00 d . . . C(63) C 0.3840(3) 0.0238(3) 0.1559(4) 0.052(1) Uani 1.00 d . . . C(64) C 0.4679(4) 0.0084(3) 0.1281(4) 0.066(2) Uani 1.00 d . . . C(65) C 0.5522(3) 0.0636(3) 0.1778(4) 0.059(1) Uani 1.00 d . . . C(66) C 0.5550(3) 0.1342(3) 0.2584(4) 0.054(1) Uani 1.00 d . . . C(67) C 0.4724(3) 0.1497(2) 0.2874(3) 0.043(1) Uani 1.00 d . . . H(1) H 0.4184 0.1888 -0.1828 0.0758 Uiso 1.00 calc . . . H(2) H 0.5638 0.2819 -0.1105 0.0854 Uiso 1.00 calc . . . H(3) H 0.6251 0.3641 0.0827 0.0764 Uiso 1.00 calc . . . H(4) H 0.2642 0.1644 -0.0278 0.0934 Uiso 1.00 calc . . . H(5) H 0.2421 0.1702 -0.1545 0.0934 Uiso 1.00 calc . . . H(6) H 0.3094 0.1059 -0.1043 0.0934 Uiso 1.00 calc . . . H(7) H 0.6230 0.3599 0.2942 0.0957 Uiso 1.00 calc . . . H(8) H 0.5610 0.4298 0.2552 0.0957 Uiso 1.00 calc . . . H(9) H 0.5123 0.3630 0.2874 0.0957 Uiso 1.00 calc . . . H(10) H 0.0554 0.0643 0.4213 0.0617 Uiso 1.00 calc . . . H(11) H -0.1079 0.0348 0.4179 0.0829 Uiso 1.00 calc . . . H(12) H -0.2157 0.1370 0.4219 0.0796 Uiso 1.00 calc . . . H(13) H -0.1661 0.2662 0.4180 0.0739 Uiso 1.00 calc . . . H(14) H -0.0038 0.2961 0.4238 0.0577 Uiso 1.00 calc . . . H(15) H 0.4451 0.4249 0.7243 0.0529 Uiso 1.00 calc . . . H(16) H 0.3911 0.4402 0.8792 0.0608 Uiso 1.00 calc . . . H(17) H 0.2459 0.3621 0.8522 0.0629 Uiso 1.00 calc . . . H(18) H 0.1513 0.2688 0.6694 0.0500 Uiso 1.00 calc . . . H(19) H 0.4445 0.2093 0.6020 0.0579 Uiso 1.00 calc . . . H(20) H 0.6060 0.1649 0.6877 0.0765 Uiso 1.00 calc . . . H(21) H 0.7481 0.2266 0.6758 0.0977 Uiso 1.00 calc . . . H(22) H 0.7307 0.3350 0.5938 0.0924 Uiso 1.00 calc . . . H(23) H 0.5691 0.3766 0.5037 0.0674 Uiso 1.00 calc . . . H(24) H 0.4333 0.4640 0.5605 0.0449 Uiso 1.00 calc . . . H(25) H 0.4176 0.4388 0.4292 0.0449 Uiso 1.00 calc . . . H(26) H 0.2933 0.5232 0.4413 0.0492 Uiso 1.00 calc . . . H(27) H 0.2593 0.4711 0.5066 0.0492 Uiso 1.00 calc . . . H(28) H -0.0125 0.3285 0.2145 0.0639 Uiso 1.00 calc . . . H(29) H -0.1710 0.3651 0.2154 0.0809 Uiso 1.00 calc . . . H(30) H -0.1794 0.4982 0.3181 0.0833 Uiso 1.00 calc . . . H(31) H -0.0373 0.5929 0.4022 0.0848 Uiso 1.00 calc . . . H(32) H 0.1202 0.5577 0.3987 0.0809 Uiso 1.00 calc . . . H(33) H 0.0691 0.5088 0.1535 0.0778 Uiso 1.00 calc . . . H(34) H 0.0960 0.5762 0.0270 0.0977 Uiso 1.00 calc . . . H(35) H 0.2487 0.5752 0.0053 0.0868 Uiso 1.00 calc . . . H(36) H 0.3772 0.4996 0.1043 0.0823 Uiso 1.00 calc . . . H(37) H 0.3503 0.4319 0.2300 0.0630 Uiso 1.00 calc . . . H(38) H -0.1043 0.2531 -0.0280 0.0759 Uiso 1.00 calc . . . H(39) H -0.2714 0.2423 -0.0388 0.0900 Uiso 1.00 calc . . . H(40) H -0.3163 0.1562 0.0568 0.0824 Uiso 1.00 calc . . . H(41) H -0.1962 0.0816 0.1604 0.0676 Uiso 1.00 calc . . . H(42) H -0.0273 0.0936 0.1751 0.0537 Uiso 1.00 calc . . . H(43) H -0.0109 0.1063 -0.1561 0.0787 Uiso 1.00 calc . . . H(44) H -0.0630 0.1482 -0.3317 0.0897 Uiso 1.00 calc . . . H(45) H -0.0261 0.2829 -0.3223 0.0828 Uiso 1.00 calc . . . H(46) H 0.0673 0.3763 -0.1410 0.0747 Uiso 1.00 calc . . . H(47) H 0.1207 0.3336 0.0346 0.0621 Uiso 1.00 calc . . . H(48) H 0.0499 0.0487 0.0025 0.0451 Uiso 1.00 calc . . . H(49) H 0.1557 0.0785 0.0104 0.0451 Uiso 1.00 calc . . . H(50) H 0.1915 -0.0005 0.1361 0.0451 Uiso 1.00 calc . . . H(51) H 0.1184 0.0400 0.1908 0.0451 Uiso 1.00 calc . . . H(52) H 0.3885 -0.0050 0.3767 0.0573 Uiso 1.00 calc . . . H(53) H 0.4075 -0.0472 0.5456 0.0667 Uiso 1.00 calc . . . H(54) H 0.3267 0.0156 0.6656 0.0619 Uiso 1.00 calc . . . H(55) H 0.2240 0.1200 0.6180 0.0499 Uiso 1.00 calc . . . H(56) H 0.3239 -0.0158 0.1200 0.0627 Uiso 1.00 calc . . . H(57) H 0.4653 -0.0424 0.0714 0.0772 Uiso 1.00 calc . . . H(58) H 0.6093 0.0528 0.1551 0.0710 Uiso 1.00 calc . . . H(59) H 0.6157 0.1730 0.2963 0.0677 Uiso 1.00 calc . . . H(60) H 0.4753 0.1993 0.3445 0.0529 Uiso 1.00 calc . . . 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 Mo(1) 0.0238(1) 0.0225(1) 0.0271(1) 0.00097(9) 0.0094(1) 0.00661(10) P(1) 0.0254(4) 0.0287(4) 0.0299(4) -0.0018(3) 0.0082(3) 0.0063(3) P(2) 0.0330(4) 0.0265(4) 0.0370(5) 0.0035(3) 0.0135(4) 0.0095(4) P(3) 0.0279(4) 0.0315(4) 0.0324(4) -0.0012(3) 0.0076(4) 0.0061(4) P(4) 0.0294(4) 0.0260(4) 0.0345(4) 0.0036(3) 0.0139(4) 0.0064(3) Si(1) 0.0268(4) 0.0279(4) 0.0311(4) 0.0023(3) 0.0128(4) 0.0090(4) N(1) 0.057(2) 0.055(2) 0.062(2) 0.022(2) 0.044(2) 0.027(2) C(1) 0.031(2) 0.033(2) 0.033(2) 0.003(1) 0.011(1) 0.010(1) C(2) 0.046(2) 0.048(2) 0.053(2) 0.019(2) 0.033(2) 0.025(2) C(3) 0.045(2) 0.063(3) 0.054(2) 0.016(2) 0.027(2) 0.022(2) C(4) 0.055(3) 0.096(4) 0.049(2) 0.026(3) 0.028(2) 0.023(2) C(5) 0.050(3) 0.123(5) 0.067(3) 0.029(3) 0.039(2) 0.041(3) C(6) 0.038(2) 0.088(3) 0.078(3) 0.007(2) 0.031(2) 0.032(3) C(7) 0.050(2) 0.058(3) 0.059(3) 0.014(2) 0.028(2) 0.018(2) C(8) 0.076(3) 0.093(4) 0.064(3) -0.006(3) 0.037(3) 0.003(3) C(9) 0.071(3) 0.078(4) 0.083(4) 0.000(3) 0.038(3) -0.001(3) C(10) 0.028(2) 0.045(2) 0.031(2) 0.000(1) 0.010(1) 0.012(1) C(11) 0.037(2) 0.059(3) 0.055(2) -0.006(2) 0.011(2) 0.025(2) C(12) 0.047(3) 0.087(4) 0.070(3) -0.020(2) 0.012(2) 0.039(3) C(13) 0.032(2) 0.120(4) 0.059(3) -0.007(3) 0.017(2) 0.033(3) C(14) 0.037(2) 0.094(4) 0.055(3) 0.015(2) 0.019(2) 0.016(2) C(15) 0.039(2) 0.056(2) 0.044(2) 0.005(2) 0.019(2) 0.007(2) C(16) 0.030(2) 0.031(2) 0.033(2) 0.007(1) 0.012(1) 0.009(1) C(17) 0.031(2) 0.033(2) 0.029(2) 0.004(1) 0.011(1) 0.008(1) C(18) 0.045(2) 0.044(2) 0.034(2) -0.004(2) 0.011(2) 0.004(2) C(19) 0.057(2) 0.056(2) 0.029(2) 0.004(2) 0.009(2) 0.003(2) C(20) 0.058(2) 0.058(2) 0.037(2) 0.015(2) 0.023(2) 0.009(2) C(21) 0.041(2) 0.046(2) 0.042(2) 0.009(2) 0.022(2) 0.012(2) C(22) 0.027(2) 0.038(2) 0.034(2) 0.000(1) 0.004(1) 0.005(1) C(23) 0.042(2) 0.048(2) 0.052(2) 0.008(2) 0.013(2) 0.017(2) C(24) 0.053(3) 0.058(3) 0.069(3) 0.017(2) 0.012(2) 0.020(2) C(25) 0.041(3) 0.068(3) 0.109(4) 0.018(2) 0.009(3) 0.018(3) C(26) 0.032(2) 0.082(4) 0.117(5) 0.001(2) 0.024(3) 0.029(3) C(27) 0.031(2) 0.055(2) 0.077(3) -0.003(2) 0.019(2) 0.018(2) C(28) 0.037(2) 0.029(2) 0.039(2) -0.008(1) 0.010(2) 0.005(1) C(29) 0.050(2) 0.024(2) 0.045(2) 0.002(1) 0.017(2) 0.009(1) C(30) 0.042(2) 0.038(2) 0.044(2) 0.015(2) 0.020(2) 0.016(2) C(31) 0.040(2) 0.042(2) 0.069(3) 0.011(2) 0.016(2) 0.013(2) C(32) 0.042(2) 0.069(3) 0.094(4) 0.013(2) 0.026(2) 0.027(3) C(33) 0.058(3) 0.084(4) 0.084(4) 0.036(3) 0.041(3) 0.037(3) C(34) 0.072(3) 0.063(3) 0.081(4) 0.033(3) 0.036(3) 0.003(3) C(35) 0.061(3) 0.044(2) 0.086(3) 0.012(2) 0.028(3) 0.003(2) C(36) 0.049(2) 0.030(2) 0.042(2) 0.003(2) 0.018(2) 0.014(1) C(37) 0.058(3) 0.078(3) 0.081(3) 0.021(2) 0.031(3) 0.051(3) C(38) 0.091(4) 0.092(4) 0.087(4) 0.025(3) 0.029(3) 0.069(3) C(39) 0.089(4) 0.083(4) 0.072(3) -0.002(3) 0.034(3) 0.045(3) C(40) 0.064(3) 0.087(4) 0.069(3) -0.002(3) 0.033(3) 0.035(3) C(41) 0.056(2) 0.047(2) 0.055(2) 0.002(2) 0.020(2) 0.022(2) C(42) 0.032(2) 0.038(2) 0.035(2) -0.005(1) 0.009(1) 0.001(1) C(43) 0.040(2) 0.067(3) 0.080(3) 0.012(2) 0.019(2) 0.033(3) C(44) 0.037(2) 0.095(4) 0.093(4) 0.020(2) 0.018(2) 0.035(3) C(45) 0.034(2) 0.081(3) 0.076(3) -0.006(2) 0.022(2) -0.005(3) C(46) 0.044(2) 0.068(3) 0.054(2) -0.012(2) 0.024(2) 0.001(2) C(47) 0.038(2) 0.051(2) 0.038(2) 0.001(2) 0.014(2) 0.005(2) C(48) 0.034(2) 0.053(2) 0.033(2) 0.002(2) 0.010(2) 0.012(2) C(49) 0.066(3) 0.072(3) 0.036(2) -0.009(2) 0.005(2) 0.007(2) C(50) 0.074(3) 0.106(4) 0.032(2) 0.006(3) 0.009(2) 0.012(3) C(51) 0.060(3) 0.113(4) 0.043(3) 0.013(3) 0.020(2) 0.039(3) C(52) 0.063(3) 0.076(3) 0.063(3) 0.012(2) 0.027(2) 0.039(3) C(53) 0.049(2) 0.060(3) 0.041(2) 0.002(2) 0.014(2) 0.019(2) C(54) 0.036(2) 0.032(2) 0.037(2) -0.002(1) 0.012(2) 0.001(1) C(55) 0.034(2) 0.026(2) 0.049(2) 0.000(1) 0.015(2) 0.004(1) C(56) 0.030(2) 0.029(2) 0.038(2) 0.003(1) 0.013(1) 0.013(1) C(57) 0.034(2) 0.027(2) 0.040(2) 0.005(1) 0.015(1) 0.012(1) C(58) 0.054(2) 0.041(2) 0.063(3) 0.021(2) 0.032(2) 0.024(2) C(59) 0.057(3) 0.051(2) 0.079(3) 0.024(2) 0.028(2) 0.041(2) C(60) 0.054(2) 0.058(3) 0.056(2) 0.013(2) 0.021(2) 0.035(2) C(61) 0.045(2) 0.040(2) 0.046(2) 0.008(2) 0.019(2) 0.022(2) C(62) 0.037(2) 0.036(2) 0.037(2) 0.012(1) 0.018(1) 0.012(1) C(63) 0.048(2) 0.051(2) 0.054(2) 0.005(2) 0.026(2) 0.002(2) C(64) 0.069(3) 0.073(3) 0.059(3) 0.022(3) 0.038(2) 0.004(2) C(65) 0.051(3) 0.086(3) 0.062(3) 0.028(2) 0.036(2) 0.033(3) C(66) 0.035(2) 0.063(3) 0.069(3) 0.011(2) 0.019(2) 0.027(2) C(67) 0.031(2) 0.046(2) 0.050(2) 0.007(2) 0.015(2) 0.011(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Mo(1) P(1) 2.4207(9) . . yes Mo(1) P(2) 2.4978(9) . . yes Mo(1) P(3) 2.4612(9) . . yes Mo(1) P(4) 2.4210(9) . . yes Mo(1) Si(1) 2.5593(9) . . yes Mo(1) C(1) 2.072(3) . . yes P(1) C(17) 1.840(3) . . yes P(1) C(22) 1.854(4) . . yes P(1) C(28) 1.847(3) . . yes P(2) C(29) 1.866(4) . . yes P(2) C(30) 1.851(4) . . yes P(2) C(36) 1.855(4) . . yes P(3) C(42) 1.854(4) . . yes P(3) C(48) 1.849(4) . . yes P(3) C(54) 1.867(4) . . yes P(4) C(55) 1.856(3) . . yes P(4) C(57) 1.827(3) . . yes P(4) C(62) 1.849(3) . . yes Si(1) C(10) 1.917(3) . . yes Si(1) C(16) 1.899(3) . . yes Si(1) C(56) 1.915(3) . . yes N(1) C(1) 1.171(4) . . yes N(1) C(2) 1.396(4) . . yes C(2) C(3) 1.391(6) . . yes C(2) C(7) 1.405(6) . . yes C(3) C(4) 1.384(6) . . yes C(3) C(8) 1.503(7) . . yes C(4) C(5) 1.378(7) . . yes C(5) C(6) 1.365(7) . . yes C(6) C(7) 1.386(6) . . yes C(7) C(9) 1.485(7) . . yes C(10) C(11) 1.383(5) . . yes C(10) C(15) 1.386(5) . . yes C(11) C(12) 1.401(6) . . yes C(12) C(13) 1.359(7) . . yes C(13) C(14) 1.363(7) . . yes C(14) C(15) 1.399(6) . . yes C(16) C(17) 1.405(4) . . yes C(16) C(21) 1.405(5) . . yes C(17) C(18) 1.391(5) . . yes C(18) C(19) 1.384(5) . . yes C(19) C(20) 1.365(6) . . yes C(20) C(21) 1.383(5) . . yes C(22) C(23) 1.392(5) . . yes C(22) C(27) 1.380(5) . . yes C(23) C(24) 1.383(6) . . yes C(24) C(25) 1.379(7) . . yes C(25) C(26) 1.353(7) . . yes C(26) C(27) 1.391(6) . . yes C(28) C(29) 1.521(5) . . yes C(30) C(31) 1.368(5) . . yes C(30) C(35) 1.388(5) . . yes C(31) C(32) 1.395(6) . . yes C(32) C(33) 1.363(7) . . yes C(33) C(34) 1.360(7) . . yes C(34) C(35) 1.378(7) . . yes C(36) C(37) 1.391(5) . . yes C(36) C(41) 1.369(6) . . yes C(37) C(38) 1.393(6) . . yes C(38) C(39) 1.357(7) . . yes C(39) C(40) 1.381(7) . . yes C(40) C(41) 1.384(6) . . yes C(42) C(43) 1.396(5) . . yes C(42) C(47) 1.386(5) . . yes C(43) C(44) 1.375(6) . . yes C(44) C(45) 1.375(7) . . yes C(45) C(46) 1.366(7) . . yes C(46) C(47) 1.397(5) . . yes C(48) C(49) 1.393(5) . . yes C(48) C(53) 1.373(5) . . yes C(49) C(50) 1.380(6) . . yes C(50) C(51) 1.361(7) . . yes C(51) C(52) 1.365(7) . . yes C(52) C(53) 1.400(6) . . yes C(54) C(55) 1.515(5) . . yes C(56) C(57) 1.391(5) . . yes C(56) C(61) 1.396(4) . . yes C(57) C(58) 1.396(5) . . yes C(58) C(59) 1.387(6) . . yes C(59) C(60) 1.370(6) . . yes C(60) C(61) 1.392(5) . . yes C(62) C(63) 1.386(5) . . yes C(62) C(67) 1.390(5) . . yes C(63) C(64) 1.389(6) . . yes C(64) C(65) 1.358(7) . . yes C(65) C(66) 1.372(6) . . yes C(66) C(67) 1.379(5) . . yes #------------------------------------------------------------------------------ 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 P(1) Mo(1) P(2) 79.00(3) . 1_555 1_555 yes P(1) Mo(1) P(3) 178.57(3) . 1_555 1_555 yes P(1) Mo(1) P(4) 98.25(3) . 1_555 1_555 yes P(1) Mo(1) Si(1) 75.75(3) . 1_555 1_555 yes P(1) Mo(1) C(1) 92.49(9) . 1_555 1_555 yes P(2) Mo(1) P(3) 102.15(3) . 1_555 1_555 yes P(2) Mo(1) P(4) 174.93(3) . 1_555 1_555 yes P(2) Mo(1) Si(1) 107.32(3) . 1_555 1_555 yes P(2) Mo(1) C(1) 91.84(9) . 1_555 1_555 yes P(3) Mo(1) P(4) 80.67(3) . 1_555 1_555 yes P(3) Mo(1) Si(1) 103.03(3) . 1_555 1_555 yes P(3) Mo(1) C(1) 88.33(9) . 1_555 1_555 yes P(4) Mo(1) Si(1) 75.89(3) . 1_555 1_555 yes P(4) Mo(1) C(1) 83.99(9) . 1_555 1_555 yes Si(1) Mo(1) C(1) 154.76(9) . 1_555 1_555 yes Mo(1) P(1) C(17) 115.1(1) . 1_555 1_555 yes Mo(1) P(1) C(22) 127.7(1) . 1_555 1_555 yes Mo(1) P(1) C(28) 109.7(1) . 1_555 1_555 yes C(17) P(1) C(22) 98.0(2) . 1_555 1_555 yes C(17) P(1) C(28) 99.7(2) . 1_555 1_555 yes C(22) P(1) C(28) 102.6(2) . 1_555 1_555 yes Mo(1) P(2) C(29) 108.9(1) . 1_555 1_555 yes Mo(1) P(2) C(30) 121.1(1) . 1_555 1_555 yes Mo(1) P(2) C(36) 122.5(1) . 1_555 1_555 yes C(29) P(2) C(30) 100.3(2) . 1_555 1_555 yes C(29) P(2) C(36) 98.6(2) . 1_555 1_555 yes C(30) P(2) C(36) 101.2(2) . 1_555 1_555 yes Mo(1) P(3) C(42) 122.0(1) . 1_555 1_555 yes Mo(1) P(3) C(48) 124.0(1) . 1_555 1_555 yes Mo(1) P(3) C(54) 109.2(1) . 1_555 1_555 yes C(42) P(3) C(48) 96.6(2) . 1_555 1_555 yes C(42) P(3) C(54) 101.4(2) . 1_555 1_555 yes C(48) P(3) C(54) 99.6(2) . 1_555 1_555 yes Mo(1) P(4) C(55) 110.1(1) . 1_555 1_555 yes Mo(1) P(4) C(57) 116.7(1) . 1_555 1_555 yes Mo(1) P(4) C(62) 120.6(1) . 1_555 1_555 yes C(55) P(4) C(57) 99.7(2) . 1_555 1_555 yes C(55) P(4) C(62) 103.7(2) . 1_555 1_555 yes C(57) P(4) C(62) 103.5(2) . 1_555 1_555 yes Mo(1) Si(1) C(10) 128.8(1) . 1_555 1_555 yes Mo(1) Si(1) C(16) 108.5(1) . 1_555 1_555 yes Mo(1) Si(1) C(56) 108.5(1) . 1_555 1_555 yes C(10) Si(1) C(16) 103.6(1) . 1_555 1_555 yes C(10) Si(1) C(56) 103.0(1) . 1_555 1_555 yes C(16) Si(1) C(56) 101.1(1) . 1_555 1_555 yes C(1) N(1) C(2) 177.7(4) . 1_555 1_555 yes Mo(1) C(1) N(1) 177.1(3) . 1_555 1_555 yes N(1) C(2) C(3) 118.6(4) . 1_555 1_555 yes N(1) C(2) C(7) 119.3(4) . 1_555 1_555 yes C(3) C(2) C(7) 122.1(3) . 1_555 1_555 yes C(2) C(3) C(4) 117.8(4) . 1_555 1_555 yes C(2) C(3) C(8) 121.4(4) . 1_555 1_555 yes C(4) C(3) C(8) 120.8(4) . 1_555 1_555 yes C(3) C(4) C(5) 121.3(4) . 1_555 1_555 yes C(4) C(5) C(6) 119.6(4) . 1_555 1_555 yes C(5) C(6) C(7) 122.1(4) . 1_555 1_555 yes C(2) C(7) C(6) 116.8(4) . 1_555 1_555 yes C(2) C(7) C(9) 121.0(4) . 1_555 1_555 yes C(6) C(7) C(9) 122.1(4) . 1_555 1_555 yes Si(1) C(10) C(11) 123.8(3) . 1_555 1_555 yes Si(1) C(10) C(15) 119.3(3) . 1_555 1_555 yes C(11) C(10) C(15) 116.9(3) . 1_555 1_555 yes C(10) C(11) C(12) 121.6(4) . 1_555 1_555 yes C(11) C(12) C(13) 119.9(4) . 1_555 1_555 yes C(12) C(13) C(14) 120.1(4) . 1_555 1_555 yes C(13) C(14) C(15) 120.0(4) . 1_555 1_555 yes C(10) C(15) C(14) 121.5(4) . 1_555 1_555 yes Si(1) C(16) C(17) 116.3(2) . 1_555 1_555 yes Si(1) C(16) C(21) 126.2(3) . 1_555 1_555 yes C(17) C(16) C(21) 117.2(3) . 1_555 1_555 yes P(1) C(17) C(16) 116.1(2) . 1_555 1_555 yes P(1) C(17) C(18) 123.0(3) . 1_555 1_555 yes C(16) C(17) C(18) 120.9(3) . 1_555 1_555 yes C(17) C(18) C(19) 120.0(3) . 1_555 1_555 yes C(18) C(19) C(20) 120.2(3) . 1_555 1_555 yes C(19) C(20) C(21) 120.4(3) . 1_555 1_555 yes C(16) C(21) C(20) 121.3(3) . 1_555 1_555 yes P(1) C(22) C(23) 118.8(3) . 1_555 1_555 yes P(1) C(22) C(27) 122.9(3) . 1_555 1_555 yes C(23) C(22) C(27) 118.3(3) . 1_555 1_555 yes C(22) C(23) C(24) 121.2(4) . 1_555 1_555 yes C(23) C(24) C(25) 119.0(4) . 1_555 1_555 yes C(24) C(25) C(26) 120.7(4) . 1_555 1_555 yes C(25) C(26) C(27) 120.4(4) . 1_555 1_555 yes C(22) C(27) C(26) 120.3(4) . 1_555 1_555 yes P(1) C(28) C(29) 106.8(2) . 1_555 1_555 yes P(2) C(29) C(28) 110.6(2) . 1_555 1_555 yes P(2) C(30) C(31) 118.7(3) . 1_555 1_555 yes P(2) C(30) C(35) 123.0(3) . 1_555 1_555 yes C(31) C(30) C(35) 118.3(4) . 1_555 1_555 yes C(30) C(31) C(32) 121.0(4) . 1_555 1_555 yes C(31) C(32) C(33) 119.8(4) . 1_555 1_555 yes C(32) C(33) C(34) 119.7(4) . 1_555 1_555 yes C(33) C(34) C(35) 120.9(4) . 1_555 1_555 yes C(30) C(35) C(34) 120.2(4) . 1_555 1_555 yes P(2) C(36) C(37) 123.1(3) . 1_555 1_555 yes P(2) C(36) C(41) 119.2(3) . 1_555 1_555 yes C(37) C(36) C(41) 117.7(4) . 1_555 1_555 yes C(36) C(37) C(38) 120.4(4) . 1_555 1_555 yes C(37) C(38) C(39) 120.8(5) . 1_555 1_555 yes C(38) C(39) C(40) 119.5(4) . 1_555 1_555 yes C(39) C(40) C(41) 119.6(4) . 1_555 1_555 yes C(36) C(41) C(40) 122.0(4) . 1_555 1_555 yes P(3) C(42) C(43) 121.7(3) . 1_555 1_555 yes P(3) C(42) C(47) 120.7(3) . 1_555 1_555 yes C(43) C(42) C(47) 117.5(3) . 1_555 1_555 yes C(42) C(43) C(44) 121.3(4) . 1_555 1_555 yes C(43) C(44) C(45) 120.0(4) . 1_555 1_555 yes C(44) C(45) C(46) 120.4(4) . 1_555 1_555 yes C(45) C(46) C(47) 119.6(4) . 1_555 1_555 yes C(42) C(47) C(46) 121.1(4) . 1_555 1_555 yes P(3) C(48) C(49) 121.9(3) . 1_555 1_555 yes P(3) C(48) C(53) 119.4(3) . 1_555 1_555 yes C(49) C(48) C(53) 118.3(4) . 1_555 1_555 yes C(48) C(49) C(50) 120.7(5) . 1_555 1_555 yes C(49) C(50) C(51) 120.0(4) . 1_555 1_555 yes C(50) C(51) C(52) 120.9(4) . 1_555 1_555 yes C(51) C(52) C(53) 119.1(4) . 1_555 1_555 yes C(48) C(53) C(52) 121.0(4) . 1_555 1_555 yes P(3) C(54) C(55) 111.7(2) . 1_555 1_555 yes P(4) C(55) C(54) 109.7(2) . 1_555 1_555 yes Si(1) C(56) C(57) 119.0(2) . 1_555 1_555 yes Si(1) C(56) C(61) 122.6(3) . 1_555 1_555 yes C(57) C(56) C(61) 118.4(3) . 1_555 1_555 yes P(4) C(57) C(56) 114.0(2) . 1_555 1_555 yes P(4) C(57) C(58) 125.0(3) . 1_555 1_555 yes C(56) C(57) C(58) 121.0(3) . 1_555 1_555 yes C(57) C(58) C(59) 119.6(3) . 1_555 1_555 yes C(58) C(59) C(60) 120.0(4) . 1_555 1_555 yes C(59) C(60) C(61) 120.6(4) . 1_555 1_555 yes C(56) C(61) C(60) 120.4(3) . 1_555 1_555 yes P(4) C(62) C(63) 124.7(3) . 1_555 1_555 yes P(4) C(62) C(67) 118.2(3) . 1_555 1_555 yes C(63) C(62) C(67) 117.0(3) . 1_555 1_555 yes C(62) C(63) C(64) 121.2(4) . 1_555 1_555 yes C(63) C(64) C(65) 120.6(4) . 1_555 1_555 yes C(64) C(65) C(66) 119.4(4) . 1_555 1_555 yes C(65) C(66) C(67) 120.5(4) . 1_555 1_555 yes C(62) C(67) C(66) 121.3(4) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Mo(1) P(1) C(17) C(16) 16.9(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(1) C(17) C(18) -164.3(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(1) C(22) C(23) -78.7(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(1) C(22) C(27) 99.9(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(1) C(28) C(29) 50.9(2) 1_555 1_555 1_555 1_555 yes Mo(1) P(2) C(29) C(28) 33.1(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(2) C(30) C(31) -28.2(4) 1_555 1_555 1_555 1_555 yes Mo(1) P(2) C(30) C(35) 152.9(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(2) C(36) C(37) 130.2(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(2) C(36) C(41) -49.2(4) 1_555 1_555 1_555 1_555 yes Mo(1) P(3) C(42) C(43) 108.5(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(3) C(42) C(47) -68.5(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(3) C(48) C(49) 158.8(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(3) C(48) C(53) -28.6(4) 1_555 1_555 1_555 1_555 yes Mo(1) P(3) C(54) C(55) 33.4(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(4) C(55) C(54) 41.2(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(4) C(57) C(56) 23.0(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(4) C(57) C(58) -158.4(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(4) C(62) C(63) -136.4(3) 1_555 1_555 1_555 1_555 yes Mo(1) P(4) C(62) C(67) 42.9(3) 1_555 1_555 1_555 1_555 yes Mo(1) Si(1) C(10) C(11) 116.7(3) 1_555 1_555 1_555 1_555 yes Mo(1) Si(1) C(10) C(15) -65.0(3) 1_555 1_555 1_555 1_555 yes Mo(1) Si(1) C(16) C(17) -24.7(3) 1_555 1_555 1_555 1_555 yes Mo(1) Si(1) C(16) C(21) 162.0(3) 1_555 1_555 1_555 1_555 yes Mo(1) Si(1) C(56) C(57) -12.2(3) 1_555 1_555 1_555 1_555 yes Mo(1) Si(1) C(56) C(61) 164.2(3) 1_555 1_555 1_555 1_555 yes Mo(1) C(1) N(1) C(2) 57(13) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(2) C(29) -1.9(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(2) C(30) -117.1(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(2) C(36) 112.1(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(3) C(42) 70(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(3) C(48) -163(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(3) C(54) -47(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(4) C(55) 163.2(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(4) C(57) 50.5(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) P(4) C(62) -76.2(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) Si(1) C(10) 150.3(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) Si(1) C(16) 24.4(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) Si(1) C(56) -84.6(1) 1_555 1_555 1_555 1_555 yes P(1) Mo(1) C(1) N(1) 132(5) 1_555 1_555 1_555 1_555 yes P(1) C(17) C(16) Si(1) 6.2(3) 1_555 1_555 1_555 1_555 yes P(1) C(17) C(16) C(21) -179.9(3) 1_555 1_555 1_555 1_555 yes P(1) C(17) C(18) C(19) 179.1(3) 1_555 1_555 1_555 1_555 yes P(1) C(22) C(23) C(24) 178.4(3) 1_555 1_555 1_555 1_555 yes P(1) C(22) C(27) C(26) -178.3(4) 1_555 1_555 1_555 1_555 yes P(1) C(28) C(29) P(2) -52.8(3) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(1) C(17) 88.0(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(1) C(22) -148.2(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(1) C(28) -23.4(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(3) C(42) -72.9(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(3) C(48) 52.9(2) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(3) C(54) 169.4(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(4) C(55) -140.0(4) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(4) C(57) 107.4(4) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) P(4) C(62) -19.4(4) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) Si(1) C(10) 76.9(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) Si(1) C(16) -49.0(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) Si(1) C(56) -158.1(1) 1_555 1_555 1_555 1_555 yes P(2) Mo(1) C(1) N(1) -148(5) 1_555 1_555 1_555 1_555 yes P(2) C(30) C(31) C(32) -179.4(4) 1_555 1_555 1_555 1_555 yes P(2) C(30) C(35) C(34) 179.1(4) 1_555 1_555 1_555 1_555 yes P(2) C(36) C(37) C(38) -179.0(4) 1_555 1_555 1_555 1_555 yes P(2) C(36) C(41) C(40) 179.1(4) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(1) C(17) -55(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(1) C(22) 68(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(1) C(28) -166(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(2) C(29) 177.3(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(2) C(30) 62.0(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(2) C(36) -68.8(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(4) C(55) -15.9(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(4) C(57) -128.5(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) P(4) C(62) 104.7(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) Si(1) C(10) -30.4(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) Si(1) C(16) -156.4(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) Si(1) C(56) 94.6(1) 1_555 1_555 1_555 1_555 yes P(3) Mo(1) C(1) N(1) -45(6) 1_555 1_555 1_555 1_555 yes P(3) C(42) C(43) C(44) -176.0(4) 1_555 1_555 1_555 1_555 yes P(3) C(42) C(47) C(46) 176.7(3) 1_555 1_555 1_555 1_555 yes P(3) C(48) C(49) C(50) 171.4(4) 1_555 1_555 1_555 1_555 yes P(3) C(48) C(53) C(52) -171.1(3) 1_555 1_555 1_555 1_555 yes P(3) C(54) C(55) P(4) -47.4(3) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(1) C(17) -96.4(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(1) C(22) 27.5(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(1) C(28) 152.2(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(2) C(29) -59.4(4) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(2) C(30) -174.6(4) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(2) C(36) 54.6(4) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(3) C(42) 111.4(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(3) C(48) -122.8(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) P(3) C(54) -6.3(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) Si(1) C(10) -107.2(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) Si(1) C(16) 126.9(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) Si(1) C(56) 17.9(1) 1_555 1_555 1_555 1_555 yes P(4) Mo(1) C(1) N(1) 34(5) 1_555 1_555 1_555 1_555 yes P(4) C(57) C(56) Si(1) -5.4(3) 1_555 1_555 1_555 1_555 yes P(4) C(57) C(56) C(61) 178.0(3) 1_555 1_555 1_555 1_555 yes P(4) C(57) C(58) C(59) -178.8(3) 1_555 1_555 1_555 1_555 yes P(4) C(62) C(63) C(64) 177.2(4) 1_555 1_555 1_555 1_555 yes P(4) C(62) C(67) C(66) -176.7(3) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(1) C(17) -23.3(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(1) C(22) 100.6(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(1) C(28) -134.7(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(2) C(29) 69.3(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(2) C(30) -45.9(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(2) C(36) -176.7(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(3) C(42) 38.4(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(3) C(48) 164.1(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(3) C(54) -79.3(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(4) C(55) 90.2(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(4) C(57) -22.4(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) P(4) C(62) -149.2(1) 1_555 1_555 1_555 1_555 yes Si(1) Mo(1) C(1) N(1) 71(6) 1_555 1_555 1_555 1_555 yes Si(1) C(10) C(11) C(12) 177.4(3) 1_555 1_555 1_555 1_555 yes Si(1) C(10) C(15) C(14) -177.2(3) 1_555 1_555 1_555 1_555 yes Si(1) C(16) C(17) C(18) -172.6(3) 1_555 1_555 1_555 1_555 yes Si(1) C(16) C(21) C(20) 173.7(3) 1_555 1_555 1_555 1_555 yes Si(1) C(56) C(57) C(58) 175.9(3) 1_555 1_555 1_555 1_555 yes Si(1) C(56) C(61) C(60) -174.8(3) 1_555 1_555 1_555 1_555 yes N(1) C(2) C(3) C(4) 177.3(4) 1_555 1_555 1_555 1_555 yes N(1) C(2) C(3) C(8) -2.7(6) 1_555 1_555 1_555 1_555 yes N(1) C(2) C(7) C(6) -175.7(4) 1_555 1_555 1_555 1_555 yes N(1) C(2) C(7) C(9) 5.0(6) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(1) C(17) 179.3(1) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(1) C(22) -56.8(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(1) C(28) 67.9(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(2) C(29) -94.0(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(2) C(30) 150.7(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(2) C(36) 19.9(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(3) C(42) -164.4(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(3) C(48) -38.7(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(3) C(54) 77.9(1) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(4) C(55) -105.2(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(4) C(57) 142.2(1) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) P(4) C(62) 15.4(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) Si(1) C(10) -145.3(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) Si(1) C(16) 88.7(2) 1_555 1_555 1_555 1_555 yes C(1) Mo(1) Si(1) C(56) -20.3(2) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(2) C(3) -27(9) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(2) C(7) 153(9) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 0.0(7) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(6) C(5) -3.3(7) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(7) C(6) 5.7(6) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(7) C(9) -173.5(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 2.3(8) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(7) -4.2(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -0.6(8) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(3) C(8) -180.0(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(9) 176.0(5) 1_555 1_555 1_555 1_555 yes C(7) C(2) C(3) C(8) 175.8(4) 1_555 1_555 1_555 1_555 yes C(10) Si(1) C(16) C(17) -164.2(2) 1_555 1_555 1_555 1_555 yes C(10) Si(1) C(16) C(21) 22.5(3) 1_555 1_555 1_555 1_555 yes C(10) Si(1) C(56) C(57) 126.8(3) 1_555 1_555 1_555 1_555 yes C(10) Si(1) C(56) C(61) -56.7(3) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) -0.4(7) 1_555 1_555 1_555 1_555 yes C(10) C(15) C(14) C(13) 0.0(7) 1_555 1_555 1_555 1_555 yes C(11) C(10) Si(1) C(16) -115.6(3) 1_555 1_555 1_555 1_555 yes C(11) C(10) Si(1) C(56) -10.5(3) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(15) C(14) 1.2(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 1.6(7) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(10) C(15) -1.0(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -1.4(7) 1_555 1_555 1_555 1_555 yes C(15) C(10) Si(1) C(16) 62.8(3) 1_555 1_555 1_555 1_555 yes C(15) C(10) Si(1) C(56) 167.8(3) 1_555 1_555 1_555 1_555 yes C(16) Si(1) C(56) C(57) -126.2(3) 1_555 1_555 1_555 1_555 yes C(16) Si(1) C(56) C(61) 50.3(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) P(1) C(22) -121.5(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) P(1) C(28) 134.1(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) -2.1(6) 1_555 1_555 1_555 1_555 yes C(16) C(21) C(20) C(19) -1.3(6) 1_555 1_555 1_555 1_555 yes C(17) P(1) C(22) C(23) 51.8(3) 1_555 1_555 1_555 1_555 yes C(17) P(1) C(22) C(27) -129.6(3) 1_555 1_555 1_555 1_555 yes C(17) P(1) C(28) C(29) -70.3(3) 1_555 1_555 1_555 1_555 yes C(17) C(16) Si(1) C(56) 89.4(3) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(21) C(20) 0.4(5) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 1.2(6) 1_555 1_555 1_555 1_555 yes C(18) C(17) P(1) C(22) 57.3(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) P(1) C(28) -47.1(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(16) C(21) 1.3(5) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) 0.5(6) 1_555 1_555 1_555 1_555 yes C(21) C(16) Si(1) C(56) -83.9(3) 1_555 1_555 1_555 1_555 yes C(22) P(1) C(28) C(29) -170.9(2) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) -0.1(7) 1_555 1_555 1_555 1_555 yes C(22) C(27) C(26) C(25) 0.0(8) 1_555 1_555 1_555 1_555 yes C(23) C(22) P(1) C(28) 153.7(3) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(27) C(26) 0.4(6) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 0.5(9) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(27) -0.3(6) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -0.4(9) 1_555 1_555 1_555 1_555 yes C(27) C(22) P(1) C(28) -27.6(4) 1_555 1_555 1_555 1_555 yes C(28) C(29) P(2) C(30) 161.2(2) 1_555 1_555 1_555 1_555 yes C(28) C(29) P(2) C(36) -95.7(3) 1_555 1_555 1_555 1_555 yes C(29) P(2) C(30) C(31) -147.7(3) 1_555 1_555 1_555 1_555 yes C(29) P(2) C(30) C(35) 33.3(4) 1_555 1_555 1_555 1_555 yes C(29) P(2) C(36) C(37) -110.7(4) 1_555 1_555 1_555 1_555 yes C(29) P(2) C(36) C(41) 69.8(3) 1_555 1_555 1_555 1_555 yes C(30) P(2) C(36) C(37) -8.4(4) 1_555 1_555 1_555 1_555 yes C(30) P(2) C(36) C(41) 172.2(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -1.0(8) 1_555 1_555 1_555 1_555 yes C(30) C(35) C(34) C(33) 1.4(9) 1_555 1_555 1_555 1_555 yes C(31) C(30) P(2) C(36) 111.2(3) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(34) 0.2(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 2.6(8) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(30) C(35) -0.4(7) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(35) -2.8(9) 1_555 1_555 1_555 1_555 yes C(35) C(30) P(2) C(36) -67.7(4) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) -0.5(9) 1_555 1_555 1_555 1_555 yes C(36) C(41) C(40) C(39) 0.4(8) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(41) C(40) -0.4(7) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) 0.5(9) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(41) 0.4(7) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) -0.4(9) 1_555 1_555 1_555 1_555 yes C(42) P(3) C(48) C(49) -65.0(4) 1_555 1_555 1_555 1_555 yes C(42) P(3) C(48) C(53) 107.6(3) 1_555 1_555 1_555 1_555 yes C(42) P(3) C(54) C(55) -96.6(3) 1_555 1_555 1_555 1_555 yes C(42) C(43) C(44) C(45) -0.7(8) 1_555 1_555 1_555 1_555 yes C(42) C(47) C(46) C(45) -0.6(6) 1_555 1_555 1_555 1_555 yes C(43) C(42) P(3) C(48) -28.9(4) 1_555 1_555 1_555 1_555 yes C(43) C(42) P(3) C(54) -130.1(3) 1_555 1_555 1_555 1_555 yes C(43) C(42) C(47) C(46) -0.4(6) 1_555 1_555 1_555 1_555 yes C(43) C(44) C(45) C(46) -0.4(8) 1_555 1_555 1_555 1_555 yes C(44) C(43) C(42) C(47) 1.1(7) 1_555 1_555 1_555 1_555 yes C(44) C(45) C(46) C(47) 1.0(7) 1_555 1_555 1_555 1_555 yes C(47) C(42) P(3) C(48) 154.2(3) 1_555 1_555 1_555 1_555 yes C(47) C(42) P(3) C(54) 52.9(3) 1_555 1_555 1_555 1_555 yes C(48) P(3) C(54) C(55) 164.6(2) 1_555 1_555 1_555 1_555 yes C(48) C(49) C(50) C(51) -0.1(8) 1_555 1_555 1_555 1_555 yes C(48) C(53) C(52) C(51) -0.7(7) 1_555 1_555 1_555 1_555 yes C(49) C(48) P(3) C(54) 37.8(4) 1_555 1_555 1_555 1_555 yes C(49) C(48) C(53) C(52) 1.7(6) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) 1.2(8) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(48) C(53) -1.3(7) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) -0.8(8) 1_555 1_555 1_555 1_555 yes C(53) C(48) P(3) C(54) -149.6(3) 1_555 1_555 1_555 1_555 yes C(54) C(55) P(4) C(57) 164.3(2) 1_555 1_555 1_555 1_555 yes C(54) C(55) P(4) C(62) -89.1(3) 1_555 1_555 1_555 1_555 yes C(55) P(4) C(57) C(56) -95.5(3) 1_555 1_555 1_555 1_555 yes C(55) P(4) C(57) C(58) 83.1(3) 1_555 1_555 1_555 1_555 yes C(55) P(4) C(62) C(63) -12.6(4) 1_555 1_555 1_555 1_555 yes C(55) P(4) C(62) C(67) 166.6(3) 1_555 1_555 1_555 1_555 yes C(56) C(57) P(4) C(62) 157.8(2) 1_555 1_555 1_555 1_555 yes C(56) C(57) C(58) C(59) -0.3(6) 1_555 1_555 1_555 1_555 yes C(56) C(61) C(60) C(59) -1.8(6) 1_555 1_555 1_555 1_555 yes C(57) P(4) C(62) C(63) 91.0(4) 1_555 1_555 1_555 1_555 yes C(57) P(4) C(62) C(67) -89.7(3) 1_555 1_555 1_555 1_555 yes C(57) C(56) C(61) C(60) 1.7(5) 1_555 1_555 1_555 1_555 yes C(57) C(58) C(59) C(60) 0.3(7) 1_555 1_555 1_555 1_555 yes C(58) C(57) P(4) C(62) -23.6(4) 1_555 1_555 1_555 1_555 yes C(58) C(57) C(56) C(61) -0.7(5) 1_555 1_555 1_555 1_555 yes C(58) C(59) C(60) C(61) 0.7(7) 1_555 1_555 1_555 1_555 yes C(62) C(63) C(64) C(65) 0.0(7) 1_555 1_555 1_555 1_555 yes C(62) C(67) C(66) C(65) -1.1(6) 1_555 1_555 1_555 1_555 yes C(63) C(62) C(67) C(66) 2.6(6) 1_555 1_555 1_555 1_555 yes C(63) C(64) C(65) C(66) 1.6(7) 1_555 1_555 1_555 1_555 yes C(64) C(63) C(62) C(67) -2.0(6) 1_555 1_555 1_555 1_555 yes C(64) C(65) C(66) C(67) -1.1(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Mo(1) Si(1) 2.5593(9) . . ? C(4) C(20) 3.479(6) . 1_554 ? C(4) C(19) 3.575(7) . 1_554 ? C(5) C(19) 3.479(7) . 1_554 ? C(5) C(44) 3.598(7) . 1_655 ? C(45) C(63) 3.591(6) . 2_555 ? C(60) C(65) 3.542(6) . 2_656 ? #------------------------------------------------------------------------------