Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Clendenning, Scott B.' 'Gehrhus, Barbara' 'Hitchcock, Peter B.' 'Moser, Daniel F.' 'Nixon, J.' 'West, R.' _publ_contact_author_name 'Prof J Nixon' _publ_contact_author_address ; School of Chemistry, Physics and Environmental Sciences Sussex University Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'J.NIXON@SUSSEX.AC.UK' _publ_section_title ; [1+4]-Cycloadditions of silylenes to 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene ; #---------------------------------------------------------------------- # [1+4]-Cycloadditions of Silylenes to 2,4,6-tri-tert-butyl ..... #---------------------------------------------------------------------- data_jan701 _database_code_CSD 171463 _audit_creation_date 2001-01-25T15:47:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '?' _chemical_formula_moiety 'C35 H71 N4 P3 Si2' _chemical_formula_structural 'C35 H71 N4 P3 SI2' _chemical_formula_sum 'C35 H71 N4 P3 Si2' _chemical_formula_weight 697.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3052(3) _cell_length_b 17.7570(3) _cell_length_c 21.9827(7) _cell_angle_alpha 90 _cell_angle_beta 94.8400(10) _cell_angle_gamma 90 _cell_volume 4008.26(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15082 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_T_min 0.9111 _exptl_absorpt_correction_T_max 0.9111 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 23839 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 7042 _reflns_number_gt 5735 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.4097P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7042 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.25 _refine_diff_density_min -0.29 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.47552(5) 0.25590(3) 0.46361(2) 0.02139(13) Uani 1 1 d . . . P2 P 0.36201(5) 0.29963(3) 0.58099(2) 0.02355(13) Uani 1 1 d . . . P3 P 0.30857(5) 0.39786(3) 0.46918(2) 0.02308(13) Uani 1 1 d . . . Si1 Si 0.25452(5) 0.23337(3) 0.45818(2) 0.01820(13) Uani 1 1 d . . . Si2 Si 0.17528(5) 0.22169(3) 0.34958(2) 0.02038(13) Uani 1 1 d . . . N1 N 0.17813(17) 0.29693(9) 0.29924(7) 0.0261(4) Uani 1 1 d . . . N2 N 0.27738(17) 0.16693(9) 0.30807(7) 0.0248(4) Uani 1 1 d . . . N3 N 0.02562(16) 0.18187(9) 0.36066(7) 0.0223(4) Uani 1 1 d . . . N4 N 0.19893(16) 0.14580(8) 0.48306(7) 0.0207(4) Uani 1 1 d . . . C1 C 0.24093(18) 0.32168(10) 0.51563(9) 0.0203(4) Uani 1 1 d . . . C2 C 0.49031(19) 0.26531(11) 0.54824(9) 0.0222(4) Uani 1 1 d . . . C3 C 0.44029(19) 0.35589(10) 0.44393(9) 0.0228(4) Uani 1 1 d . . . C4 C 0.11245(19) 0.34910(11) 0.54477(9) 0.0231(4) Uani 1 1 d . . . C5 C 0.1452(2) 0.41306(12) 0.59126(10) 0.0334(5) Uani 1 1 d . . . H5A H 0.212 0.3957 0.6225 0.05 Uiso 1 1 calc R . . H5B H 0.0666 0.4272 0.6106 0.05 Uiso 1 1 calc R . . H5C H 0.1779 0.4568 0.5701 0.05 Uiso 1 1 calc R . . C6 C 0.0080(2) 0.38173(12) 0.49854(10) 0.0283(5) Uani 1 1 d . . . H6A H 0.0449 0.4237 0.4767 0.042 Uiso 1 1 calc R . . H6B H -0.0655 0.3998 0.52 0.042 Uiso 1 1 calc R . . H6C H -0.0221 0.3426 0.4693 0.042 Uiso 1 1 calc R . . C7 C 0.0531(2) 0.28387(12) 0.57843(10) 0.0283(5) Uani 1 1 d . . . H7A H 0.1191 0.2626 0.6083 0.043 Uiso 1 1 calc R . . H7B H 0.0229 0.2449 0.549 0.043 Uiso 1 1 calc R . . H7C H -0.0206 0.3024 0.5996 0.043 Uiso 1 1 calc R . . C8 C 0.6174(2) 0.24543(12) 0.58780(10) 0.0299(5) Uani 1 1 d . . . C9 C 0.6843(2) 0.31976(14) 0.60880(12) 0.0405(6) Uani 1 1 d . . . H9A H 0.6246 0.3498 0.6314 0.061 Uiso 1 1 calc R . . H9B H 0.7076 0.3481 0.5731 0.061 Uiso 1 1 calc R . . H9C H 0.7632 0.3086 0.6353 0.061 Uiso 1 1 calc R . . C10 C 0.5875(2) 0.20136(15) 0.64541(11) 0.0425(6) Uani 1 1 d . . . H10A H 0.5277 0.2307 0.6685 0.064 Uiso 1 1 calc R . . H10B H 0.6687 0.1924 0.6709 0.064 Uiso 1 1 calc R . . H10C H 0.5473 0.153 0.6334 0.064 Uiso 1 1 calc R . . C11 C 0.7121(2) 0.19905(14) 0.55289(11) 0.0386(6) Uani 1 1 d . . . H11A H 0.6706 0.1515 0.5395 0.058 Uiso 1 1 calc R . . H11B H 0.7909 0.1884 0.5797 0.058 Uiso 1 1 calc R . . H11C H 0.7354 0.2275 0.5172 0.058 Uiso 1 1 calc R . . C12 C 0.5371(2) 0.39767(11) 0.40656(9) 0.0266(5) Uani 1 1 d . . . C13 C 0.5039(2) 0.48157(12) 0.39874(11) 0.0340(5) Uani 1 1 d . . . H13A H 0.5016 0.505 0.439 0.051 Uiso 1 1 calc R . . H13B H 0.4185 0.4869 0.3759 0.051 Uiso 1 1 calc R . . H13C H 0.5702 0.5064 0.3764 0.051 Uiso 1 1 calc R . . C14 C 0.5404(2) 0.36115(13) 0.34347(10) 0.0370(6) Uani 1 1 d . . . H14A H 0.5619 0.3076 0.3483 0.056 Uiso 1 1 calc R . . H14B H 0.6064 0.3861 0.321 0.056 Uiso 1 1 calc R . . H14C H 0.4548 0.3664 0.3208 0.056 Uiso 1 1 calc R . . C15 C 0.6736(2) 0.39191(13) 0.44001(11) 0.0366(6) Uani 1 1 d . . . H15A H 0.6974 0.3388 0.4454 0.055 Uiso 1 1 calc R . . H15B H 0.6737 0.4162 0.48 0.055 Uiso 1 1 calc R . . H15C H 0.7366 0.4171 0.4159 0.055 Uiso 1 1 calc R . . C16 C 0.2513(2) 0.27877(12) 0.24677(9) 0.0332(5) Uani 1 1 d . . . H16A H 0.3006 0.3234 0.2347 0.04 Uiso 1 1 calc R . . H16B H 0.191 0.2632 0.2116 0.04 Uiso 1 1 calc R . . C17 C 0.3436(2) 0.21537(12) 0.26563(10) 0.0320(5) Uani 1 1 d . . . H17A H 0.3647 0.1861 0.2294 0.038 Uiso 1 1 calc R . . H17B H 0.4255 0.2356 0.286 0.038 Uiso 1 1 calc R . . C18 C 0.0989(2) 0.36690(12) 0.29278(10) 0.0305(5) Uani 1 1 d . . . C19 C 0.0081(2) 0.36713(14) 0.23366(11) 0.0422(6) Uani 1 1 d . . . H19A H 0.0599 0.3624 0.1985 0.063 Uiso 1 1 calc R . . H19B H -0.041 0.4144 0.2307 0.063 Uiso 1 1 calc R . . H19C H -0.0526 0.3247 0.2341 0.063 Uiso 1 1 calc R . . C20 C 0.1884(3) 0.43578(13) 0.29251(12) 0.0445(6) Uani 1 1 d . . . H20A H 0.2409 0.4329 0.2574 0.067 Uiso 1 1 calc R . . H20B H 0.2461 0.4368 0.3303 0.067 Uiso 1 1 calc R . . H20C H 0.1356 0.4817 0.2896 0.067 Uiso 1 1 calc R . . C21 C 0.0203(2) 0.37412(12) 0.34764(10) 0.0345(5) Uani 1 1 d . . . H21A H -0.0382 0.3308 0.3492 0.052 Uiso 1 1 calc R . . H21B H -0.0312 0.4206 0.3443 0.052 Uiso 1 1 calc R . . H21C H 0.0793 0.3757 0.385 0.052 Uiso 1 1 calc R . . C22 C 0.3343(2) 0.09009(12) 0.31538(9) 0.0301(5) Uani 1 1 d . . . C23 C 0.4759(2) 0.09374(14) 0.34168(12) 0.0426(6) Uani 1 1 d . . . H23A H 0.5269 0.1227 0.3141 0.064 Uiso 1 1 calc R . . H23B H 0.5112 0.0426 0.3461 0.064 Uiso 1 1 calc R . . H23C H 0.4807 0.1183 0.3817 0.064 Uiso 1 1 calc R . . C24 C 0.2557(2) 0.04432(12) 0.35765(10) 0.0341(5) Uani 1 1 d . . . H24A H 0.165 0.0414 0.3405 0.051 Uiso 1 1 calc R . . H24B H 0.2595 0.0686 0.3978 0.051 Uiso 1 1 calc R . . H24C H 0.2921 -0.0066 0.3619 0.051 Uiso 1 1 calc R . . C25 C 0.3278(3) 0.04862(14) 0.25345(11) 0.0464(7) Uani 1 1 d . . . H25A H 0.237 0.0456 0.2364 0.07 Uiso 1 1 calc R . . H25B H 0.3632 -0.0023 0.2594 0.07 Uiso 1 1 calc R . . H25C H 0.379 0.0763 0.2252 0.07 Uiso 1 1 calc R . . C26 C -0.0122(2) 0.18497(11) 0.42368(9) 0.0235(4) Uani 1 1 d . . . H26A H -0.1068 0.1752 0.4231 0.028 Uiso 1 1 calc R . . H26B H 0.004 0.2365 0.4397 0.028 Uiso 1 1 calc R . . C27 C 0.0598(2) 0.12912(11) 0.46703(9) 0.0243(4) Uani 1 1 d . . . H27A H 0.0152 0.1272 0.5052 0.029 Uiso 1 1 calc R . . H27B H 0.0529 0.0785 0.4482 0.029 Uiso 1 1 calc R . . C28 C -0.0785(2) 0.15334(11) 0.31478(9) 0.0274(5) Uani 1 1 d . . . C29 C -0.0256(2) 0.14605(13) 0.25231(10) 0.0348(5) Uani 1 1 d . . . H29A H 0.0498 0.1122 0.2553 0.052 Uiso 1 1 calc R . . H29B H 0.0009 0.1958 0.2385 0.052 Uiso 1 1 calc R . . H29C H -0.0934 0.1255 0.223 0.052 Uiso 1 1 calc R . . C30 C -0.1968(2) 0.20633(13) 0.30905(11) 0.0371(5) Uani 1 1 d . . . H30A H -0.2321 0.2113 0.3489 0.056 Uiso 1 1 calc R . . H30B H -0.2638 0.1856 0.2794 0.056 Uiso 1 1 calc R . . H30C H -0.1699 0.256 0.2952 0.056 Uiso 1 1 calc R . . C31 C -0.1259(2) 0.07513(12) 0.33323(10) 0.0351(5) Uani 1 1 d . . . H31A H -0.1614 0.0784 0.3731 0.053 Uiso 1 1 calc R . . H31B H -0.0527 0.0397 0.3356 0.053 Uiso 1 1 calc R . . H31C H -0.1939 0.0574 0.3027 0.053 Uiso 1 1 calc R . . C32 C 0.2611(2) 0.08894(11) 0.52756(9) 0.0246(4) Uani 1 1 d . . . C33 C 0.4074(2) 0.08554(12) 0.52256(10) 0.0304(5) Uani 1 1 d . . . H33A H 0.4243 0.0728 0.4806 0.046 Uiso 1 1 calc R . . H33B H 0.4458 0.047 0.5504 0.046 Uiso 1 1 calc R . . H33C H 0.4462 0.1346 0.5335 0.046 Uiso 1 1 calc R . . C34 C 0.2330(2) 0.10815(12) 0.59313(9) 0.0307(5) Uani 1 1 d . . . H34A H 0.1386 0.1101 0.5959 0.046 Uiso 1 1 calc R . . H34B H 0.2712 0.1572 0.6045 0.046 Uiso 1 1 calc R . . H34C H 0.2711 0.0694 0.621 0.046 Uiso 1 1 calc R . . C35 C 0.2086(2) 0.00858(11) 0.51396(10) 0.0332(5) Uani 1 1 d . . . H35A H 0.1143 0.0078 0.5168 0.05 Uiso 1 1 calc R . . H35B H 0.2507 -0.0267 0.5437 0.05 Uiso 1 1 calc R . . H35C H 0.2277 -0.0063 0.4727 0.05 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0198(3) 0.0216(3) 0.0231(3) -0.0013(2) 0.0041(2) -0.0021(2) P2 0.0195(3) 0.0297(3) 0.0213(3) -0.0040(2) 0.0010(2) -0.0011(2) P3 0.0224(3) 0.0192(3) 0.0279(3) -0.0017(2) 0.0035(2) -0.0027(2) Si1 0.0193(3) 0.0184(3) 0.0171(3) 0.0000(2) 0.0027(2) -0.0030(2) Si2 0.0235(3) 0.0213(3) 0.0164(3) 0.0004(2) 0.0019(2) -0.0027(2) N1 0.0330(10) 0.0250(9) 0.0207(9) 0.0035(7) 0.0048(8) -0.0007(7) N2 0.0306(10) 0.0246(9) 0.0201(9) -0.0007(7) 0.0070(7) -0.0005(7) N3 0.0233(10) 0.0266(9) 0.0169(8) -0.0008(7) 0.0001(7) -0.0055(7) N4 0.0224(9) 0.0203(8) 0.0192(8) 0.0017(6) 0.0003(7) -0.0050(7) C1 0.0180(11) 0.0222(10) 0.0209(10) -0.0021(8) 0.0026(8) -0.0018(8) C2 0.0194(11) 0.0232(10) 0.0240(11) -0.0022(8) 0.0006(8) -0.0032(8) C3 0.0220(11) 0.0218(10) 0.0245(11) -0.0025(8) 0.0012(9) -0.0047(8) C4 0.0177(11) 0.0270(11) 0.0246(11) -0.0056(8) 0.0025(8) -0.0002(8) C5 0.0268(12) 0.0358(12) 0.0378(13) -0.0154(10) 0.0051(10) 0.0023(9) C6 0.0214(11) 0.0315(11) 0.0321(12) -0.0036(9) 0.0030(9) 0.0046(9) C7 0.0205(11) 0.0396(12) 0.0256(11) -0.0012(9) 0.0060(9) -0.0015(9) C8 0.0207(11) 0.0383(12) 0.0300(12) -0.0027(9) -0.0014(9) 0.0008(9) C9 0.0245(13) 0.0515(15) 0.0439(14) -0.0117(11) -0.0066(11) -0.0029(10) C10 0.0325(14) 0.0573(16) 0.0369(14) 0.0108(12) -0.0024(11) 0.0057(11) C11 0.0244(13) 0.0480(14) 0.0428(14) -0.0074(11) -0.0011(10) 0.0091(10) C12 0.0247(12) 0.0275(11) 0.0286(11) 0.0023(9) 0.0070(9) -0.0069(8) C13 0.0354(14) 0.0281(12) 0.0388(13) 0.0042(10) 0.0052(11) -0.0092(9) C14 0.0443(15) 0.0357(13) 0.0329(13) 0.0008(10) 0.0135(11) -0.0056(10) C15 0.0236(12) 0.0377(13) 0.0489(15) 0.0056(11) 0.0055(11) -0.0099(9) C16 0.0433(14) 0.0367(13) 0.0202(11) 0.0037(9) 0.0061(10) -0.0067(10) C17 0.0389(14) 0.0325(12) 0.0264(12) -0.0008(9) 0.0140(10) -0.0050(10) C18 0.0346(13) 0.0277(11) 0.0287(12) 0.0064(9) -0.0003(10) -0.0005(9) C19 0.0461(16) 0.0460(14) 0.0336(13) 0.0099(11) -0.0026(11) 0.0047(11) C20 0.0530(17) 0.0305(13) 0.0498(16) 0.0110(11) 0.0024(13) -0.0040(11) C21 0.0404(14) 0.0293(12) 0.0336(13) 0.0019(10) 0.0017(11) 0.0048(10) C22 0.0364(13) 0.0302(11) 0.0244(11) -0.0028(9) 0.0060(10) 0.0045(9) C23 0.0366(15) 0.0467(14) 0.0450(15) 0.0030(12) 0.0060(12) 0.0076(11) C24 0.0459(15) 0.0261(11) 0.0309(12) -0.0007(9) 0.0076(11) 0.0040(10) C25 0.0715(19) 0.0364(13) 0.0326(14) -0.0086(10) 0.0119(13) 0.0074(12) C26 0.0234(11) 0.0267(11) 0.0206(10) -0.0020(8) 0.0026(9) -0.0055(8) C27 0.0266(12) 0.0270(11) 0.0194(10) -0.0001(8) 0.0028(9) -0.0092(8) C28 0.0288(12) 0.0305(11) 0.0223(11) -0.0012(8) -0.0010(9) -0.0075(9) C29 0.0378(14) 0.0426(13) 0.0227(11) -0.0014(10) -0.0048(10) -0.0108(10) C30 0.0294(13) 0.0446(14) 0.0360(13) 0.0003(10) -0.0058(10) -0.0052(10) C31 0.0379(14) 0.0354(12) 0.0314(12) -0.0029(10) -0.0005(10) -0.0133(10) C32 0.0298(12) 0.0233(10) 0.0207(10) 0.0049(8) 0.0012(9) -0.0029(8) C33 0.0347(13) 0.0247(11) 0.0320(12) 0.0063(9) 0.0033(10) 0.0029(9) C34 0.0405(14) 0.0298(12) 0.0219(11) 0.0048(9) 0.0025(10) -0.0032(9) C35 0.0448(14) 0.0231(11) 0.0317(12) 0.0053(9) 0.0041(10) -0.0071(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C3 1.856(2) . ? P1 C2 1.861(2) . ? P1 Si1 2.3055(7) . ? P2 C2 1.673(2) . ? P2 C1 1.863(2) . ? P3 C3 1.683(2) . ? P3 C1 1.8650(19) . ? Si1 N4 1.7601(15) . ? Si1 C1 2.0258(19) . ? Si1 Si2 2.4658(7) . ? Si2 N3 1.7324(17) . ? Si2 N1 1.7365(16) . ? Si2 N2 1.7457(17) . ? N1 C16 1.466(3) . ? N1 C18 1.487(3) . ? N2 C17 1.477(3) . ? N2 C22 1.489(3) . ? N3 C26 1.471(2) . ? N3 C28 1.498(3) . ? N4 C27 1.477(3) . ? N4 C32 1.510(2) . ? C1 C4 1.595(3) . ? C2 C8 1.550(3) . ? C3 C12 1.536(3) . ? C4 C7 1.530(3) . ? C4 C6 1.530(3) . ? C4 C5 1.546(3) . ? C8 C11 1.532(3) . ? C8 C10 1.542(3) . ? C8 C9 1.542(3) . ? C12 C15 1.534(3) . ? C12 C14 1.534(3) . ? C12 C13 1.535(3) . ? C16 C17 1.509(3) . ? C18 C21 1.514(3) . ? C18 C20 1.532(3) . ? C18 C19 1.536(3) . ? C22 C24 1.519(3) . ? C22 C23 1.525(3) . ? C22 C25 1.544(3) . ? C26 C27 1.524(3) . ? C28 C29 1.525(3) . ? C28 C30 1.536(3) . ? C28 C31 1.538(3) . ? C32 C33 1.522(3) . ? C32 C34 1.533(3) . ? C32 C35 1.546(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 P1 C2 98.34(9) . . ? C3 P1 Si1 88.91(7) . . ? C2 P1 Si1 93.70(6) . . ? C2 P2 C1 104.29(9) . . ? C3 P3 C1 102.03(9) . . ? N4 Si1 C1 116.66(8) . . ? N4 Si1 P1 118.90(6) . . ? C1 Si1 P1 87.32(6) . . ? N4 Si1 Si2 97.86(6) . . ? C1 Si1 Si2 129.35(6) . . ? P1 Si1 Si2 108.04(3) . . ? N3 Si2 N1 117.82(8) . . ? N3 Si2 N2 115.41(8) . . ? N1 Si2 N2 92.99(8) . . ? N3 Si2 Si1 97.14(6) . . ? N1 Si2 Si1 122.02(6) . . ? N2 Si2 Si1 112.83(6) . . ? C16 N1 C18 115.04(16) . . ? C16 N1 Si2 111.69(13) . . ? C18 N1 Si2 131.69(14) . . ? C17 N2 C22 113.78(16) . . ? C17 N2 Si2 109.66(13) . . ? C22 N2 Si2 134.71(13) . . ? C26 N3 C28 114.52(15) . . ? C26 N3 Si2 115.25(12) . . ? C28 N3 Si2 129.74(13) . . ? C27 N4 C32 111.74(14) . . ? C27 N4 Si1 115.96(12) . . ? C32 N4 Si1 131.35(13) . . ? C4 C1 P2 106.21(12) . . ? C4 C1 P3 111.08(13) . . ? P2 C1 P3 108.52(10) . . ? C4 C1 Si1 126.17(13) . . ? P2 C1 Si1 103.95(9) . . ? P3 C1 Si1 99.87(9) . . ? C8 C2 P2 120.15(15) . . ? C8 C2 P1 122.30(14) . . ? P2 C2 P1 117.51(11) . . ? C12 C3 P3 122.75(14) . . ? C12 C3 P1 117.61(14) . . ? P3 C3 P1 119.61(11) . . ? C7 C4 C6 108.70(17) . . ? C7 C4 C5 108.08(17) . . ? C6 C4 C5 105.25(16) . . ? C7 C4 C1 110.03(16) . . ? C6 C4 C1 114.20(16) . . ? C5 C4 C1 110.32(16) . . ? C11 C8 C10 108.56(19) . . ? C11 C8 C9 108.81(18) . . ? C10 C8 C9 107.69(19) . . ? C11 C8 C2 112.65(17) . . ? C10 C8 C2 111.02(17) . . ? C9 C8 C2 107.97(17) . . ? C15 C12 C14 108.44(18) . . ? C15 C12 C13 107.78(17) . . ? C14 C12 C13 109.31(18) . . ? C15 C12 C3 108.78(17) . . ? C14 C12 C3 110.12(16) . . ? C13 C12 C3 112.30(17) . . ? N1 C16 C17 107.57(16) . . ? N2 C17 C16 107.11(17) . . ? N1 C18 C21 108.74(16) . . ? N1 C18 C20 109.98(18) . . ? C21 C18 C20 107.36(19) . . ? N1 C18 C19 111.93(18) . . ? C21 C18 C19 110.15(19) . . ? C20 C18 C19 108.58(18) . . ? N2 C22 C24 109.34(17) . . ? N2 C22 C23 110.97(18) . . ? C24 C22 C23 109.47(19) . . ? N2 C22 C25 110.75(17) . . ? C24 C22 C25 107.36(18) . . ? C23 C22 C25 108.88(19) . . ? N3 C26 C27 114.27(16) . . ? N4 C27 C26 115.46(15) . . ? N3 C28 C29 110.15(17) . . ? N3 C28 C30 111.50(17) . . ? C29 C28 C30 108.64(18) . . ? N3 C28 C31 110.69(17) . . ? C29 C28 C31 107.85(17) . . ? C30 C28 C31 107.90(18) . . ? N4 C32 C33 110.38(15) . . ? N4 C32 C34 110.92(16) . . ? C33 C32 C34 110.10(17) . . ? N4 C32 C35 111.69(16) . . ? C33 C32 C35 106.36(17) . . ? C34 C32 C35 107.25(16) . . ? #===END data_sep1600 _database_code_CSD 171464 _audit_creation_date 2000-09-13T15:43:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[P3C3tBu3Si(tBuNCHCHNtBu)]' _chemical_formula_moiety 'C25 H47 N2 P3 Si1' _chemical_formula_structural 'C25 H47 N2 P3 SI' _chemical_formula_sum 'C25 H47 N2 P3 Si' _chemical_formula_weight 496.65 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0847(4) _cell_length_b 17.7623(5) _cell_length_c 14.7350(4) _cell_angle_alpha 90 _cell_angle_beta 101.718(2) _cell_angle_gamma 90 _cell_volume 2840.71(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11183 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_T_min 0.9485 _exptl_absorpt_correction_T_max 0.9485 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18960 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0613 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8244 _reflns_number_gt 6202 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.4217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8244 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.072 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.354 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.90331(4) 0.22727(2) 0.77896(3) 0.02196(10) Uani 1 1 d . . . P2 P 1.04442(4) 0.14417(2) 0.65146(3) 0.02120(10) Uani 1 1 d . . . P3 P 1.06886(4) 0.09804(3) 0.85435(3) 0.02338(11) Uani 1 1 d . . . Si Si 0.87528(4) 0.08024(3) 0.68108(3) 0.01846(10) Uani 1 1 d . . . N1 N 0.72678(14) 0.09374(8) 0.61543(10) 0.0232(3) Uani 1 1 d . . . N2 N 0.86190(14) -0.01795(8) 0.67611(10) 0.0234(3) Uani 1 1 d . . . C1 C 0.90717(15) 0.12521(9) 0.80611(11) 0.0192(3) Uani 1 1 d . . . C2 C 0.98236(16) 0.23181(9) 0.69258(12) 0.0219(3) Uani 1 1 d . . . C3 C 1.13736(16) 0.11087(10) 0.76333(12) 0.0228(3) Uani 1 1 d . . . C4 C 0.82223(16) 0.10626(10) 0.87716(11) 0.0228(3) Uani 1 1 d . . . C5 C 0.86502(19) 0.14954(12) 0.96809(12) 0.0322(4) Uani 1 1 d . . . H5A H 0.8634 0.2037 0.9553 0.048 Uiso 1 1 calc R . . H5B H 0.9492 0.1343 0.9965 0.048 Uiso 1 1 calc R . . H5C H 0.8099 0.1383 1.0106 0.048 Uiso 1 1 calc R . . C6 C 0.68810(17) 0.12789(12) 0.83785(13) 0.0309(4) Uani 1 1 d . . . H6A H 0.6587 0.1008 0.7796 0.046 Uiso 1 1 calc R . . H6B H 0.6827 0.1822 0.8263 0.046 Uiso 1 1 calc R . . H6C H 0.6371 0.1144 0.8825 0.046 Uiso 1 1 calc R . . C7 C 0.82633(19) 0.02178(11) 0.89927(13) 0.0315(4) Uani 1 1 d . . . H7A H 0.7994 -0.0068 0.8419 0.047 Uiso 1 1 calc R . . H7B H 0.7715 0.0109 0.9421 0.047 Uiso 1 1 calc R . . H7C H 0.9108 0.0073 0.928 0.047 Uiso 1 1 calc R . . C8 C 1.01037(19) 0.30879(10) 0.65173(13) 0.0284(4) Uani 1 1 d . . . C9 C 1.0418(2) 0.30192(12) 0.55574(15) 0.0429(5) Uani 1 1 d . . . H9A H 0.9717 0.2801 0.5125 0.064 Uiso 1 1 calc R . . H9B H 1.114 0.2693 0.5594 0.064 Uiso 1 1 calc R . . H9C H 1.06 0.3519 0.5338 0.064 Uiso 1 1 calc R . . C10 C 1.1214(3) 0.34323(13) 0.71703(19) 0.0600(8) Uani 1 1 d . . . H10A H 1.1033 0.3483 0.7791 0.09 Uiso 1 1 calc R . . H10B H 1.1388 0.393 0.694 0.09 Uiso 1 1 calc R . . H10C H 1.1932 0.3105 0.7198 0.09 Uiso 1 1 calc R . . C11 C 0.9016(3) 0.36301(13) 0.6445(2) 0.0572(7) Uani 1 1 d . . . H11A H 0.8801 0.3684 0.7055 0.086 Uiso 1 1 calc R . . H11B H 0.8307 0.3431 0.6003 0.086 Uiso 1 1 calc R . . H11C H 0.9244 0.4123 0.6232 0.086 Uiso 1 1 calc R . . C12 C 1.27763(17) 0.10171(11) 0.77323(14) 0.0297(4) Uani 1 1 d . . . C13 C 1.3347(2) 0.18055(13) 0.77572(18) 0.0457(6) Uani 1 1 d . . . H13A H 1.2999 0.2073 0.7182 0.068 Uiso 1 1 calc R . . H13B H 1.4241 0.1761 0.782 0.068 Uiso 1 1 calc R . . H13C H 1.3166 0.2086 0.8286 0.068 Uiso 1 1 calc R . . C14 C 1.3134(2) 0.05885(14) 0.69199(17) 0.0466(6) Uani 1 1 d . . . H14A H 1.2779 0.0843 0.6337 0.07 Uiso 1 1 calc R . . H14B H 1.2818 0.0073 0.6905 0.07 Uiso 1 1 calc R . . H14C H 1.4034 0.0577 0.7001 0.07 Uiso 1 1 calc R . . C15 C 1.33414(19) 0.06083(13) 0.86361(16) 0.0412(5) Uani 1 1 d . . . H15A H 1.3122 0.0876 0.9161 0.062 Uiso 1 1 calc R . . H15B H 1.424 0.0596 0.871 0.062 Uiso 1 1 calc R . . H15C H 1.3023 0.0092 0.8614 0.062 Uiso 1 1 calc R . . C16 C 0.66343(18) 0.02554(10) 0.62238(13) 0.0285(4) Uani 1 1 d . . . H16 H 0.5762 0.0218 0.6057 0.034 Uiso 1 1 calc R . . C17 C 0.73436(18) -0.03289(10) 0.65390(13) 0.0292(4) Uani 1 1 d . . . H17 H 0.7015 -0.0814 0.661 0.035 Uiso 1 1 calc R . . C18 C 0.66072(17) 0.15347(10) 0.55322(12) 0.0278(4) Uani 1 1 d . . . C19 C 0.5594(2) 0.11941(15) 0.47882(16) 0.0539(7) Uani 1 1 d . . . H19A H 0.4994 0.0935 0.5084 0.081 Uiso 1 1 calc R . . H19B H 0.5957 0.0833 0.4418 0.081 Uiso 1 1 calc R . . H19C H 0.5179 0.1595 0.4385 0.081 Uiso 1 1 calc R . . C20 C 0.6022(2) 0.20990(14) 0.60945(16) 0.0471(6) Uani 1 1 d . . . H20A H 0.544 0.1837 0.6404 0.071 Uiso 1 1 calc R . . H20B H 0.5585 0.2486 0.568 0.071 Uiso 1 1 calc R . . H20C H 0.6667 0.2336 0.6561 0.071 Uiso 1 1 calc R . . C21 C 0.7509(2) 0.19288(13) 0.50480(15) 0.0423(5) Uani 1 1 d . . . H21A H 0.8171 0.2154 0.5511 0.063 Uiso 1 1 calc R . . H21B H 0.708 0.2324 0.4643 0.063 Uiso 1 1 calc R . . H21C H 0.7861 0.1563 0.4676 0.063 Uiso 1 1 calc R . . C22 C 0.94866(19) -0.08290(10) 0.68026(13) 0.0295(4) Uani 1 1 d . . . C23 C 1.0607(3) -0.05852(14) 0.6465(3) 0.0701(9) Uani 1 1 d . . . H23A H 1.1007 -0.017 0.685 0.105 Uiso 1 1 calc R . . H23B H 1.0369 -0.0417 0.582 0.105 Uiso 1 1 calc R . . H23C H 1.1182 -0.1009 0.6502 0.105 Uiso 1 1 calc R . . C24 C 0.9851(3) -0.11081(17) 0.77969(18) 0.0771(11) Uani 1 1 d . . . H24A H 0.9113 -0.1266 0.8016 0.116 Uiso 1 1 calc R . . H24B H 1.0262 -0.0702 0.8193 0.116 Uiso 1 1 calc R . . H24C H 1.0415 -0.1536 0.7823 0.116 Uiso 1 1 calc R . . C25 C 0.8894(3) -0.14755(13) 0.6192(2) 0.0618(8) Uani 1 1 d . . . H25A H 0.8159 -0.1648 0.6406 0.093 Uiso 1 1 calc R . . H25B H 0.9482 -0.1892 0.623 0.093 Uiso 1 1 calc R . . H25C H 0.8659 -0.1303 0.5549 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0228(2) 0.0211(2) 0.0231(2) -0.00246(17) 0.00737(17) -0.00068(17) P2 0.0226(2) 0.0210(2) 0.0218(2) 0.00061(16) 0.00859(17) 0.00023(17) P3 0.0178(2) 0.0299(2) 0.0215(2) 0.00240(17) 0.00197(16) -0.00042(18) Si 0.0193(2) 0.0184(2) 0.0175(2) 0.00022(17) 0.00333(16) -0.00004(17) N1 0.0211(7) 0.0224(7) 0.0240(7) 0.0010(6) -0.0003(6) -0.0008(6) N2 0.0267(8) 0.0177(7) 0.0258(7) 0.0001(5) 0.0051(6) -0.0008(6) C1 0.0178(8) 0.0214(8) 0.0186(7) -0.0006(6) 0.0041(6) -0.0017(6) C2 0.0224(8) 0.0188(8) 0.0249(8) 0.0004(6) 0.0059(7) -0.0003(6) C3 0.0192(8) 0.0223(8) 0.0268(8) -0.0012(7) 0.0046(7) -0.0008(7) C4 0.0209(8) 0.0293(9) 0.0193(8) -0.0007(7) 0.0064(6) -0.0043(7) C5 0.0307(10) 0.0442(11) 0.0231(9) -0.0062(8) 0.0088(7) -0.0083(9) C6 0.0224(9) 0.0439(11) 0.0284(9) -0.0032(8) 0.0098(7) -0.0024(8) C7 0.0350(11) 0.0342(10) 0.0272(9) 0.0044(8) 0.0108(8) -0.0075(8) C8 0.0367(11) 0.0189(8) 0.0322(9) 0.0023(7) 0.0128(8) -0.0002(8) C9 0.0610(15) 0.0322(11) 0.0416(12) 0.0085(9) 0.0245(11) -0.0050(10) C10 0.0753(19) 0.0347(12) 0.0611(16) 0.0095(11) -0.0069(14) -0.0282(13) C11 0.0726(19) 0.0312(11) 0.0808(19) 0.0214(12) 0.0462(16) 0.0174(12) C12 0.0186(9) 0.0319(10) 0.0391(10) 0.0002(8) 0.0070(7) 0.0009(8) C13 0.0231(10) 0.0401(12) 0.0761(17) 0.0003(11) 0.0155(11) -0.0057(9) C14 0.0271(11) 0.0611(15) 0.0555(14) -0.0112(11) 0.0173(10) 0.0077(10) C15 0.0210(10) 0.0489(13) 0.0514(13) 0.0041(10) 0.0017(9) 0.0080(9) C16 0.0239(9) 0.0306(10) 0.0298(9) -0.0039(7) 0.0021(7) -0.0077(8) C17 0.0316(10) 0.0245(9) 0.0315(9) -0.0007(7) 0.0066(8) -0.0074(8) C18 0.0246(9) 0.0306(10) 0.0248(8) 0.0027(7) -0.0027(7) 0.0024(7) C19 0.0498(15) 0.0548(15) 0.0433(13) 0.0101(11) -0.0226(11) -0.0101(12) C20 0.0447(13) 0.0517(14) 0.0436(12) 0.0064(10) 0.0058(10) 0.0258(11) C21 0.0392(12) 0.0504(13) 0.0358(11) 0.0172(10) 0.0043(9) 0.0017(10) C22 0.0376(11) 0.0191(8) 0.0319(9) -0.0013(7) 0.0074(8) 0.0051(8) C23 0.0556(17) 0.0289(12) 0.139(3) -0.0059(14) 0.0495(19) 0.0085(11) C24 0.120(3) 0.0619(18) 0.0462(15) 0.0135(13) 0.0100(16) 0.0584(19) C25 0.0619(18) 0.0340(13) 0.088(2) -0.0268(13) 0.0108(15) 0.0001(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C2 1.6874(17) . ? P1 C1 1.8550(17) . ? P2 C2 1.8528(17) . ? P2 C3 1.8544(18) . ? P2 Si 2.3082(6) . ? P3 C3 1.6855(17) . ? P3 C1 1.8529(17) . ? Si N1 1.7481(15) . ? Si N2 1.7507(14) . ? Si C1 1.9730(16) . ? N1 C16 1.414(2) . ? N1 C18 1.493(2) . ? N2 C17 1.410(2) . ? N2 C22 1.495(2) . ? C1 C4 1.580(2) . ? C2 C8 1.551(2) . ? C3 C12 1.540(2) . ? C4 C6 1.531(3) . ? C4 C5 1.534(2) . ? C4 C7 1.534(3) . ? C8 C10 1.527(3) . ? C8 C9 1.529(3) . ? C8 C11 1.530(3) . ? C12 C13 1.534(3) . ? C12 C15 1.534(3) . ? C12 C14 1.537(3) . ? C16 C17 1.328(3) . ? C18 C21 1.513(3) . ? C18 C20 1.526(3) . ? C18 C19 1.526(3) . ? C22 C23 1.493(3) . ? C22 C24 1.522(3) . ? C22 C25 1.523(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C1 102.51(8) . . ? C2 P2 C3 98.82(8) . . ? C2 P2 Si 88.95(6) . . ? C3 P2 Si 90.05(6) . . ? C3 P3 C1 102.51(8) . . ? N1 Si N2 92.94(7) . . ? N1 Si C1 115.54(7) . . ? N2 Si C1 116.11(7) . . ? N1 Si P2 122.52(5) . . ? N2 Si P2 123.18(5) . . ? C1 Si P2 88.80(5) . . ? C16 N1 C18 117.66(15) . . ? C16 N1 Si 105.55(12) . . ? C18 N1 Si 136.59(12) . . ? C17 N2 C22 118.07(14) . . ? C17 N2 Si 105.64(12) . . ? C22 N2 Si 135.95(13) . . ? C4 C1 P3 110.52(11) . . ? C4 C1 P1 111.12(11) . . ? P3 C1 P1 108.38(8) . . ? C4 C1 Si 120.97(11) . . ? P3 C1 Si 103.22(8) . . ? P1 C1 Si 101.67(7) . . ? C8 C2 P1 120.70(12) . . ? C8 C2 P2 119.81(12) . . ? P1 C2 P2 119.39(9) . . ? C12 C3 P3 121.30(13) . . ? C12 C3 P2 119.06(12) . . ? P3 C3 P2 119.45(10) . . ? C6 C4 C5 108.00(15) . . ? C6 C4 C7 108.08(15) . . ? C5 C4 C7 108.30(15) . . ? C6 C4 C1 111.07(14) . . ? C5 C4 C1 110.60(14) . . ? C7 C4 C1 110.68(14) . . ? C10 C8 C9 107.99(19) . . ? C10 C8 C11 108.3(2) . . ? C9 C8 C11 108.10(18) . . ? C10 C8 C2 107.93(16) . . ? C9 C8 C2 112.96(15) . . ? C11 C8 C2 111.41(16) . . ? C13 C12 C15 108.52(18) . . ? C13 C12 C14 107.48(17) . . ? C15 C12 C14 108.49(17) . . ? C13 C12 C3 108.01(15) . . ? C15 C12 C3 111.01(15) . . ? C14 C12 C3 113.19(16) . . ? C17 C16 N1 115.30(17) . . ? C16 C17 N2 115.38(16) . . ? N1 C18 C21 109.24(16) . . ? N1 C18 C20 110.04(15) . . ? C21 C18 C20 110.27(18) . . ? N1 C18 C19 110.92(16) . . ? C21 C18 C19 107.78(17) . . ? C20 C18 C19 108.56(19) . . ? C23 C22 N2 109.53(16) . . ? C23 C22 C24 109.8(2) . . ? N2 C22 C24 109.50(16) . . ? C23 C22 C25 108.1(2) . . ? N2 C22 C25 111.14(18) . . ? C24 C22 C25 108.7(2) . . ? #===END data_nov1200 _database_code_CSD 171465 _audit_creation_date 2000-11-14T16:08:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[SAT N2Si + P3]' _chemical_formula_moiety 'C25 H49 N2 P3 Si1' _chemical_formula_structural 'C25 H49 N2 P3 SI' _chemical_formula_sum 'C25 H49 N2 P3 Si' _chemical_formula_weight 498.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0980(3) _cell_length_b 17.8562(6) _cell_length_c 14.7586(4) _cell_angle_alpha 90 _cell_angle_beta 100.983(2) _cell_angle_gamma 90 _cell_volume 2871.11(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10940 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_T_min 0.9016 _exptl_absorpt_correction_T_max 0.9016 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18478 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 6821 _reflns_number_gt 5243 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.3871P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6821 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.057 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.556 _refine_diff_density_min -0.59 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.90104(6) 0.22785(4) 0.78237(4) 0.02625(16) Uani 1 1 d . . . P2 P 1.03959(6) 0.14450(4) 0.65372(4) 0.02559(16) Uani 1 1 d . . . P3 P 1.06310(6) 0.09935(4) 0.85573(4) 0.02763(16) Uani 1 1 d . . . Si1 Si 0.86926(6) 0.08035(4) 0.68391(4) 0.02181(15) Uani 1 1 d . . . N1 N 0.72271(19) 0.09444(12) 0.61774(15) 0.0298(5) Uani 1 1 d . . . N2 N 0.8603(2) -0.01679(12) 0.67752(15) 0.0308(5) Uani 1 1 d . . . C1 C 0.9019(2) 0.12652(13) 0.80828(15) 0.0229(5) Uani 1 1 d . . . C2 C 0.9798(2) 0.23227(13) 0.69554(17) 0.0262(5) Uani 1 1 d . A . C3 C 1.1321(2) 0.11165(14) 0.76475(17) 0.0264(5) Uani 1 1 d . . . C4 C 0.6587(3) 0.02340(17) 0.6119(3) 0.0627(11) Uani 1 1 d . . . H4A H 0.5884 0.0278 0.644 0.075 Uiso 1 1 calc R . . H4B H 0.6254 0.0121 0.5462 0.075 Uiso 1 1 calc R . . C5 C 0.7326(3) -0.0358(2) 0.6501(4) 0.0862(17) Uani 1 1 d . . . H5A H 0.7248 -0.0771 0.6046 0.103 Uiso 1 1 calc R . . H5B H 0.7022 -0.0546 0.7048 0.103 Uiso 1 1 calc R . . C6 C 0.8177(2) 0.10850(15) 0.88123(16) 0.0279(5) Uani 1 1 d . . . C7 C 0.6845(2) 0.13085(17) 0.84356(19) 0.0364(6) Uani 1 1 d . . . H7A H 0.6807 0.1843 0.8281 0.055 Uiso 1 1 calc R . . H7B H 0.6346 0.121 0.8904 0.055 Uiso 1 1 calc R . . H7C H 0.6527 0.1015 0.788 0.055 Uiso 1 1 calc R . . C8 C 0.8222(3) 0.02525(17) 0.9053(2) 0.0403(7) Uani 1 1 d . . . H8A H 0.9073 0.0105 0.9297 0.061 Uiso 1 1 calc R . . H8B H 0.7903 -0.004 0.8498 0.061 Uiso 1 1 calc R . . H8C H 0.772 0.0158 0.952 0.061 Uiso 1 1 calc R . . C9 C 0.8614(3) 0.1532(2) 0.97126(18) 0.0449(8) Uani 1 1 d . . . H9A H 0.8592 0.2069 0.9573 0.067 Uiso 1 1 calc R . . H9B H 0.9455 0.1385 0.9986 0.067 Uiso 1 1 calc R . . H9C H 0.8072 0.1426 1.0149 0.067 Uiso 1 1 calc R . . C10 C 1.0083(3) 0.30813(14) 0.65396(19) 0.0341(6) Uani 1 1 d . . . C14 C 1.2719(2) 0.10113(16) 0.7739(2) 0.0355(6) Uani 1 1 d . . . C15 C 1.3325(3) 0.1787(2) 0.7822(3) 0.0626(11) Uani 1 1 d . . . H15A H 1.311 0.2054 0.835 0.094 Uiso 1 1 calc R . . H15B H 1.3034 0.2073 0.7256 0.094 Uiso 1 1 calc R . . H15C H 1.4219 0.173 0.7915 0.094 Uiso 1 1 calc R . . C16 C 1.3262(3) 0.0568(2) 0.8613(3) 0.0583(9) Uani 1 1 d . . . H16A H 1.3053 0.0818 0.9154 0.088 Uiso 1 1 calc R . . H16B H 1.4157 0.0543 0.8678 0.088 Uiso 1 1 calc R . . H16C H 1.2923 0.0059 0.8565 0.088 Uiso 1 1 calc R . . C17 C 1.3070(3) 0.0608(3) 0.6917(3) 0.0725(13) Uani 1 1 d . . . H17A H 1.2734 0.088 0.6349 0.109 Uiso 1 1 calc R . . H17B H 1.2735 0.0098 0.6879 0.109 Uiso 1 1 calc R . . H17C H 1.3966 0.0585 0.6995 0.109 Uiso 1 1 calc R . . C18 C 0.9496(3) -0.07950(15) 0.6823(2) 0.0357(6) Uani 1 1 d . . . C19 C 1.0605(5) -0.0553(2) 0.6501(5) 0.118(3) Uani 1 1 d . . . H19A H 1.0956 -0.0115 0.6857 0.176 Uiso 1 1 calc R . . H19B H 1.0394 -0.0421 0.5845 0.176 Uiso 1 1 calc R . . H19C H 1.1207 -0.0961 0.6585 0.176 Uiso 1 1 calc R . . C20 C 0.9868(7) -0.1048(4) 0.7807(3) 0.158(4) Uani 1 1 d . . . H20A H 0.914 -0.1214 0.8037 0.237 Uiso 1 1 calc R . . H20B H 1.0256 -0.0631 0.8186 0.237 Uiso 1 1 calc R . . H20C H 1.0451 -0.1464 0.784 0.237 Uiso 1 1 calc R . . C21 C 0.8982(5) -0.1459(3) 0.6259(5) 0.123(3) Uani 1 1 d . . . H21A H 0.8241 -0.1634 0.6464 0.185 Uiso 1 1 calc R . . H21B H 0.9593 -0.1862 0.6338 0.185 Uiso 1 1 calc R . . H21C H 0.8776 -0.1317 0.5607 0.185 Uiso 1 1 calc R . . C22 C 0.6628(2) 0.15435(16) 0.55482(18) 0.0343(6) Uani 1 1 d . . . C23 C 0.7481(4) 0.1859(4) 0.5014(4) 0.119(2) Uani 1 1 d . . . H23A H 0.8234 0.2014 0.5432 0.179 Uiso 1 1 calc R . . H23B H 0.7104 0.2294 0.4666 0.179 Uiso 1 1 calc R . . H23C H 0.7679 0.1481 0.4584 0.179 Uiso 1 1 calc R . . C24 C 0.6220(7) 0.2171(3) 0.6113(3) 0.142(3) Uani 1 1 d . . . H24A H 0.5638 0.1974 0.6477 0.213 Uiso 1 1 calc R . . H24B H 0.5822 0.2564 0.5699 0.213 Uiso 1 1 calc R . . H24C H 0.6935 0.2379 0.6529 0.213 Uiso 1 1 calc R . . C25 C 0.5481(5) 0.1308(3) 0.4918(4) 0.131(3) Uani 1 1 d . . . H25A H 0.4908 0.1098 0.5281 0.196 Uiso 1 1 calc R . . H25B H 0.5674 0.0929 0.4488 0.196 Uiso 1 1 calc R . . H25C H 0.5103 0.1743 0.457 0.196 Uiso 1 1 calc R . . C11 C 1.1182(8) 0.3408(4) 0.7188(6) 0.082(3) Uani 0.662(11) 1 d P A 1 H11A H 1.0991 0.3459 0.7806 0.122 Uiso 0.662(11) 1 calc PR A 1 H11B H 1.1375 0.3901 0.6962 0.122 Uiso 0.662(11) 1 calc PR A 1 H11C H 1.1889 0.3075 0.7214 0.122 Uiso 0.662(11) 1 calc PR A 1 C12 C 0.8999(8) 0.3616(3) 0.6462(7) 0.071(3) Uani 0.662(11) 1 d P A 1 H12A H 0.8781 0.368 0.7071 0.107 Uiso 0.662(11) 1 calc PR A 1 H12B H 0.8295 0.3409 0.6032 0.107 Uiso 0.662(11) 1 calc PR A 1 H12C H 0.9222 0.4102 0.6235 0.107 Uiso 0.662(11) 1 calc PR A 1 C13 C 1.0395(8) 0.3005(3) 0.5586(4) 0.0513(18) Uani 0.662(11) 1 d P A 1 H13A H 1.1087 0.2659 0.5614 0.077 Uiso 0.662(11) 1 calc PR A 1 H13B H 1.0619 0.3496 0.5373 0.077 Uiso 0.662(11) 1 calc PR A 1 H13C H 0.9681 0.281 0.5156 0.077 Uiso 0.662(11) 1 calc PR A 1 C11A C 1.1472(9) 0.3235(6) 0.6747(8) 0.041(3) Uiso 0.338(11) 1 d P A 2 H11D H 1.177 0.3233 0.7416 0.061 Uiso 0.338(11) 1 calc PR A 2 H11E H 1.1634 0.3725 0.6496 0.061 Uiso 0.338(11) 1 calc PR A 2 H11F H 1.1896 0.2845 0.6461 0.061 Uiso 0.338(11) 1 calc PR A 2 C12A C 0.9456(10) 0.3754(6) 0.6944(8) 0.041(3) Uiso 0.338(11) 1 d P A 2 H12D H 0.9708 0.376 0.7617 0.062 Uiso 0.338(11) 1 calc PR A 2 H12E H 0.8562 0.3701 0.6778 0.062 Uiso 0.338(11) 1 calc PR A 2 H12F H 0.9705 0.4224 0.6689 0.062 Uiso 0.338(11) 1 calc PR A 2 C13A C 0.9680(13) 0.3096(7) 0.5492(8) 0.050(3) Uiso 0.338(11) 1 d P A 2 H13D H 0.8795 0.3003 0.5328 0.075 Uiso 0.338(11) 1 calc PR A 2 H13E H 1.0121 0.2708 0.5217 0.075 Uiso 0.338(11) 1 calc PR A 2 H13F H 0.9866 0.3588 0.5257 0.075 Uiso 0.338(11) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0262(3) 0.0260(3) 0.0277(3) -0.0020(3) 0.0079(2) 0.0002(2) P2 0.0254(3) 0.0278(3) 0.0252(3) 0.0002(2) 0.0088(2) -0.0010(2) P3 0.0203(3) 0.0365(4) 0.0244(3) 0.0033(3) 0.0003(2) -0.0005(3) Si1 0.0210(3) 0.0235(3) 0.0202(3) 0.0008(2) 0.0020(2) -0.0009(2) N1 0.0260(11) 0.0286(11) 0.0309(11) 0.0034(9) -0.0041(9) -0.0032(9) N2 0.0283(11) 0.0239(10) 0.0377(12) -0.0002(9) 0.0002(9) -0.0018(8) C1 0.0193(11) 0.0277(12) 0.0215(11) 0.0004(9) 0.0034(9) -0.0014(9) C2 0.0252(12) 0.0252(12) 0.0275(12) 0.0009(10) 0.0036(10) -0.0016(9) C3 0.0208(11) 0.0268(12) 0.0311(12) 0.0000(10) 0.0039(10) -0.0009(9) C4 0.0318(16) 0.0320(16) 0.114(3) 0.0020(18) -0.0123(18) -0.0063(13) C5 0.0360(18) 0.0379(19) 0.166(5) 0.038(2) -0.027(2) -0.0155(15) C6 0.0230(12) 0.0392(14) 0.0222(11) -0.0002(10) 0.0059(9) -0.0051(10) C7 0.0260(13) 0.0503(17) 0.0358(14) -0.0011(13) 0.0135(11) -0.0006(12) C8 0.0389(15) 0.0474(17) 0.0371(15) 0.0120(13) 0.0132(12) -0.0056(13) C9 0.0419(16) 0.071(2) 0.0239(13) -0.0115(13) 0.0118(12) -0.0187(15) C10 0.0406(15) 0.0244(13) 0.0379(14) 0.0059(11) 0.0092(12) -0.0037(11) C14 0.0209(12) 0.0391(15) 0.0469(16) -0.0037(12) 0.0072(11) 0.0013(11) C15 0.0251(15) 0.0479(19) 0.115(3) 0.003(2) 0.0135(18) -0.0058(14) C16 0.0285(15) 0.068(2) 0.076(2) 0.0152(19) 0.0041(16) 0.0155(15) C17 0.0304(17) 0.114(4) 0.075(3) -0.032(2) 0.0169(17) 0.0111(19) C18 0.0429(16) 0.0247(13) 0.0394(14) -0.0007(11) 0.0075(12) 0.0047(11) C19 0.087(3) 0.044(2) 0.248(8) 0.015(3) 0.099(4) 0.021(2) C20 0.262(9) 0.148(5) 0.059(3) 0.026(3) 0.017(4) 0.166(6) C21 0.071(3) 0.074(3) 0.217(7) -0.087(4) 0.008(4) 0.003(3) C22 0.0297(13) 0.0393(15) 0.0295(13) 0.0054(11) -0.0054(10) 0.0033(11) C23 0.062(3) 0.169(6) 0.129(4) 0.122(4) 0.025(3) 0.027(3) C24 0.203(7) 0.122(5) 0.072(3) -0.025(3) -0.048(4) 0.124(5) C25 0.106(4) 0.092(4) 0.147(5) 0.067(4) -0.095(4) -0.045(3) C11 0.113(6) 0.048(4) 0.067(5) 0.017(3) -0.025(4) -0.050(4) C12 0.097(6) 0.036(3) 0.095(6) 0.034(4) 0.055(5) 0.029(3) C13 0.081(5) 0.032(2) 0.049(3) 0.013(2) 0.034(3) -0.005(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C2 1.685(2) . ? P1 C1 1.849(2) . ? P2 C2 1.853(3) . ? P2 C3 1.855(3) . ? P2 Si1 2.3249(9) . ? P3 C3 1.682(2) . ? P3 C1 1.857(2) . ? Si1 N2 1.739(2) . ? Si1 N1 1.748(2) . ? Si1 C1 1.982(2) . ? N1 C4 1.449(4) . ? N1 C22 1.488(3) . ? N2 C5 1.438(4) . ? N2 C18 1.488(3) . ? C1 C6 1.587(3) . ? C2 C10 1.544(3) . ? C3 C14 1.544(3) . ? C4 C5 1.391(5) . ? C6 C8 1.527(4) . ? C6 C7 1.531(4) . ? C6 C9 1.547(4) . ? C10 C11 1.516(6) . ? C10 C13 1.518(5) . ? C10 C12 1.523(6) . ? C10 C13A 1.526(11) . ? C10 C11A 1.537(10) . ? C10 C12A 1.563(11) . ? C14 C17 1.524(4) . ? C14 C15 1.534(4) . ? C14 C16 1.536(4) . ? C18 C19 1.467(5) . ? C18 C21 1.498(5) . ? C18 C20 1.501(5) . ? C22 C23 1.456(5) . ? C22 C25 1.487(5) . ? C22 C24 1.516(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C1 102.71(11) . . ? C2 P2 C3 98.40(11) . . ? C2 P2 Si1 89.84(8) . . ? C3 P2 Si1 90.47(8) . . ? C3 P3 C1 102.54(11) . . ? N2 Si1 N1 94.34(10) . . ? N2 Si1 C1 117.63(11) . . ? N1 Si1 C1 116.36(10) . . ? N2 Si1 P2 121.42(8) . . ? N1 Si1 P2 121.72(8) . . ? C1 Si1 P2 87.74(7) . . ? C4 N1 C22 115.9(2) . . ? C4 N1 Si1 107.51(18) . . ? C22 N1 Si1 135.22(18) . . ? C5 N2 C18 116.6(2) . . ? C5 N2 Si1 107.1(2) . . ? C18 N2 Si1 135.82(18) . . ? C6 C1 P1 110.99(16) . . ? C6 C1 P3 109.90(16) . . ? P1 C1 P3 107.47(12) . . ? C6 C1 Si1 121.11(16) . . ? P1 C1 Si1 102.87(11) . . ? P3 C1 Si1 103.51(11) . . ? C10 C2 P1 121.22(18) . . ? C10 C2 P2 119.75(18) . . ? P1 C2 P2 118.96(14) . . ? C14 C3 P3 121.14(19) . . ? C14 C3 P2 119.58(18) . . ? P3 C3 P2 119.15(13) . . ? C5 C4 N1 113.4(3) . . ? C4 C5 N2 114.0(3) . . ? C8 C6 C7 109.0(2) . . ? C8 C6 C9 108.2(2) . . ? C7 C6 C9 107.5(2) . . ? C8 C6 C1 111.0(2) . . ? C7 C6 C1 110.7(2) . . ? C9 C6 C1 110.5(2) . . ? C11 C10 C13 108.8(5) . . ? C11 C10 C12 109.6(5) . . ? C13 C10 C12 107.7(4) . . ? C11 C10 C13A 132.7(6) . . ? C13 C10 C13A 30.3(4) . . ? C12 C10 C13A 80.7(5) . . ? C11 C10 C11A 31.8(4) . . ? C13 C10 C11A 78.7(5) . . ? C12 C10 C11A 130.6(5) . . ? C13A C10 C11A 106.7(6) . . ? C11 C10 C2 106.7(3) . . ? C13 C10 C2 112.9(3) . . ? C12 C10 C2 111.1(3) . . ? C13A C10 C2 112.1(5) . . ? C11A C10 C2 110.5(4) . . ? C11 C10 C12A 80.0(5) . . ? C13 C10 C12A 128.3(5) . . ? C12 C10 C12A 31.1(4) . . ? C13A C10 C12A 107.9(6) . . ? C11A C10 C12A 106.8(6) . . ? C2 C10 C12A 112.5(4) . . ? C17 C14 C15 108.4(3) . . ? C17 C14 C16 107.8(3) . . ? C15 C14 C16 107.6(3) . . ? C17 C14 C3 113.1(2) . . ? C15 C14 C3 108.4(2) . . ? C16 C14 C3 111.3(2) . . ? C19 C18 N2 110.8(3) . . ? C19 C18 C21 107.9(4) . . ? N2 C18 C21 112.9(3) . . ? C19 C18 C20 108.0(5) . . ? N2 C18 C20 109.3(3) . . ? C21 C18 C20 107.7(4) . . ? C23 C22 N1 110.9(3) . . ? C23 C22 C25 109.8(4) . . ? N1 C22 C25 114.5(3) . . ? C23 C22 C24 107.8(5) . . ? N1 C22 C24 109.4(3) . . ? C25 C22 C24 104.0(4) . . ? #===END data_mar501 _database_code_CSD 171466 _audit_creation_date 2001-03-05T15:26:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Mo(CO)4{Si(NCH2tBu)2C6H4}2]' _chemical_formula_moiety 'C36 H52 Mo1 N4 O4 Si2' _chemical_formula_structural 'C36 H52 N4 MO O4 SI2' _chemical_formula_sum 'C36 H52 Mo N4 O4 Si2' _chemical_formula_weight 756.94 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1949(3) _cell_length_b 7.06150(10) _cell_length_c 26.7601(9) _cell_angle_alpha 90 _cell_angle_beta 90.5550(10) _cell_angle_gamma 90 _cell_volume 1926.40(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14408 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.948 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 12511 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_unetI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 3368 _reflns_number_gt 3009 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.0817P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3368 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.071 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.341 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.5 0.5 0 0.02086(10) Uani 1 2 d S . . Si Si 0.55723(5) 0.55282(8) 0.08792(2) 0.02172(14) Uani 1 1 d . . . O1 O 0.23527(15) 0.2979(2) 0.03225(6) 0.0389(4) Uani 1 1 d . . . O2 O 0.65177(18) 0.1054(2) 0.00296(7) 0.0523(5) Uani 1 1 d . . . N1 N 0.48038(16) 0.5023(2) 0.14379(6) 0.0225(4) Uani 1 1 d . . . N2 N 0.68088(15) 0.6733(2) 0.11940(6) 0.0228(4) Uani 1 1 d . . . C1 C 0.3315(2) 0.3697(3) 0.02050(8) 0.0283(5) Uani 1 1 d . . . C2 C 0.5971(2) 0.2460(3) 0.00162(8) 0.0318(5) Uani 1 1 d . . . C3 C 0.54218(19) 0.5900(3) 0.18480(8) 0.0230(4) Uani 1 1 d . . . C4 C 0.65648(19) 0.6887(3) 0.17084(8) 0.0235(4) Uani 1 1 d . . . C5 C 0.7264(2) 0.7928(3) 0.20621(8) 0.0284(5) Uani 1 1 d . . . H5 H 0.8019 0.8624 0.1967 0.034 Uiso 1 1 calc R . . C6 C 0.6851(2) 0.7944(3) 0.25539(8) 0.0321(5) Uani 1 1 d . . . H6 H 0.7336 0.8636 0.2798 0.038 Uiso 1 1 calc R . . C7 C 0.5735(2) 0.6960(3) 0.26935(8) 0.0302(5) Uani 1 1 d . . . H7 H 0.5465 0.6981 0.3032 0.036 Uiso 1 1 calc R . . C8 C 0.5011(2) 0.5945(3) 0.23432(8) 0.0269(4) Uani 1 1 d . . . H8 H 0.4242 0.5286 0.244 0.032 Uiso 1 1 calc R . . C9 C 0.36068(18) 0.3902(3) 0.14986(8) 0.0238(4) Uani 1 1 d . . . H9A H 0.3075 0.402 0.1189 0.029 Uiso 1 1 calc R . . H9B H 0.3093 0.4468 0.1773 0.029 Uiso 1 1 calc R . . C10 C 0.3791(2) 0.1767(3) 0.16124(8) 0.0287(5) Uani 1 1 d . . . C11 C 0.2432(2) 0.0861(4) 0.15587(11) 0.0484(7) Uani 1 1 d . . . H11A H 0.1829 0.1455 0.1795 0.073 Uiso 1 1 calc R . . H11B H 0.2494 -0.0497 0.163 0.073 Uiso 1 1 calc R . . H11C H 0.2102 0.1048 0.1217 0.073 Uiso 1 1 calc R . . C12 C 0.4298(3) 0.1429(3) 0.21448(9) 0.0421(6) Uani 1 1 d . . . H12A H 0.3705 0.2032 0.2383 0.063 Uiso 1 1 calc R . . H12B H 0.5178 0.1974 0.2182 0.063 Uiso 1 1 calc R . . H12C H 0.4336 0.0065 0.2211 0.063 Uiso 1 1 calc R . . C13 C 0.4715(3) 0.0841(3) 0.12412(10) 0.0419(6) Uani 1 1 d . . . H13A H 0.5588 0.1413 0.1273 0.063 Uiso 1 1 calc R . . H13B H 0.4378 0.1032 0.0901 0.063 Uiso 1 1 calc R . . H13C H 0.4775 -0.0519 0.1311 0.063 Uiso 1 1 calc R . . C14 C 0.7937(2) 0.7677(3) 0.09656(8) 0.0279(5) Uani 1 1 d . . . H14A H 0.8091 0.8884 0.1145 0.034 Uiso 1 1 calc R . . H14B H 0.7699 0.7997 0.0616 0.034 Uiso 1 1 calc R . . C15 C 0.9244(2) 0.6561(3) 0.09601(9) 0.0344(5) Uani 1 1 d . . . C16 C 0.9045(2) 0.4566(4) 0.07623(11) 0.0480(7) Uani 1 1 d . . . H16A H 0.9886 0.3893 0.0765 0.072 Uiso 1 1 calc R . . H16B H 0.8701 0.4623 0.0419 0.072 Uiso 1 1 calc R . . H16C H 0.842 0.3893 0.0974 0.072 Uiso 1 1 calc R . . C17 C 1.0164(2) 0.7660(4) 0.06122(10) 0.0528(7) Uani 1 1 d . . . H17A H 1.1011 0.7008 0.0596 0.079 Uiso 1 1 calc R . . H17B H 1.0295 0.8944 0.0743 0.079 Uiso 1 1 calc R . . H17C H 0.9772 0.7729 0.0277 0.079 Uiso 1 1 calc R . . C18 C 0.9885(2) 0.6462(4) 0.14806(9) 0.0442(6) Uani 1 1 d . . . H18A H 1.0704 0.5738 0.1462 0.066 Uiso 1 1 calc R . . H18B H 0.9286 0.5837 0.1713 0.066 Uiso 1 1 calc R . . H18C H 1.0075 0.7746 0.1599 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.01973(15) 0.02320(15) 0.01961(15) -0.00222(9) -0.00212(10) -0.00041(9) Si 0.0198(3) 0.0240(3) 0.0212(3) -0.0024(2) -0.0022(2) -0.0005(2) O1 0.0290(9) 0.0556(10) 0.0323(9) 0.0010(7) -0.0002(7) -0.0124(8) O2 0.0561(11) 0.0368(10) 0.0639(13) -0.0021(8) -0.0021(9) 0.0178(9) N1 0.0217(9) 0.0247(9) 0.0212(9) -0.0017(7) -0.0028(7) -0.0005(6) N2 0.0197(8) 0.0264(9) 0.0223(9) -0.0015(7) -0.0019(7) -0.0015(7) C1 0.0299(12) 0.0327(11) 0.0222(11) -0.0040(9) -0.0061(9) 0.0026(9) C2 0.0308(12) 0.0351(13) 0.0294(12) -0.0014(9) -0.0010(10) -0.0013(10) C3 0.0227(10) 0.0206(10) 0.0256(11) -0.0027(8) -0.0056(8) 0.0036(8) C4 0.0224(10) 0.0232(10) 0.0247(11) -0.0017(8) -0.0035(8) 0.0039(8) C5 0.0252(11) 0.0285(11) 0.0313(13) -0.0054(9) -0.0052(9) -0.0010(8) C6 0.0325(12) 0.0339(11) 0.0297(13) -0.0108(9) -0.0098(10) 0.0025(9) C7 0.0341(12) 0.0344(12) 0.0221(11) -0.0048(9) -0.0018(9) 0.0043(9) C8 0.0257(11) 0.0299(11) 0.0250(12) -0.0015(9) -0.0009(9) 0.0017(9) C9 0.0171(10) 0.0298(11) 0.0245(11) 0.0001(8) -0.0005(8) -0.0005(8) C10 0.0269(11) 0.0288(11) 0.0302(12) 0.0016(9) -0.0025(9) -0.0057(9) C11 0.0423(15) 0.0501(16) 0.0527(17) 0.0086(13) -0.0054(12) -0.0207(12) C12 0.0538(15) 0.0339(12) 0.0384(14) 0.0069(10) -0.0133(12) -0.0026(11) C13 0.0524(15) 0.0270(12) 0.0465(15) -0.0001(10) 0.0063(12) 0.0068(11) C14 0.0254(11) 0.0299(11) 0.0284(12) -0.0004(9) -0.0027(9) -0.0073(8) C15 0.0220(11) 0.0491(14) 0.0321(13) -0.0019(10) 0.0005(9) -0.0047(10) C16 0.0317(13) 0.0526(15) 0.0595(18) -0.0119(13) -0.0026(12) 0.0121(11) C17 0.0318(13) 0.087(2) 0.0397(16) 0.0019(14) 0.0053(11) -0.0151(13) C18 0.0258(12) 0.0675(17) 0.0391(15) 0.0004(12) -0.0055(11) 0.0052(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C1 2.029(2) . ? Mo C1 2.029(2) 3_665 ? Mo C2 2.049(2) . ? Mo C2 2.049(2) 3_665 ? Mo Si 2.4472(5) 3_665 ? Mo Si 2.4472(6) . ? Si N2 1.7325(16) . ? Si N1 1.7317(18) . ? O1 C1 1.150(3) . ? O2 C2 1.139(3) . ? N1 C3 1.405(3) . ? N1 C9 1.465(2) . ? N2 C4 1.405(3) . ? N2 C14 1.468(3) . ? C3 C8 1.394(3) . ? C3 C4 1.411(3) . ? C4 C5 1.390(3) . ? C5 C6 1.385(3) . ? C6 C7 1.388(3) . ? C7 C8 1.387(3) . ? C9 C10 1.549(3) . ? C10 C13 1.523(3) . ? C10 C11 1.532(3) . ? C10 C12 1.529(3) . ? C14 C15 1.548(3) . ? C15 C16 1.518(3) . ? C15 C18 1.535(3) . ? C15 C17 1.538(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo C1 180.00(11) . 3_665 ? C1 Mo C2 90.42(8) . . ? C1 Mo C2 89.58(8) 3_665 . ? C1 Mo C2 89.58(8) . 3_665 ? C1 Mo C2 90.42(8) 3_665 3_665 ? C2 Mo C2 180 . 3_665 ? C1 Mo Si 89.78(6) . 3_665 ? C1 Mo Si 90.22(6) 3_665 3_665 ? C2 Mo Si 89.86(6) . 3_665 ? C2 Mo Si 90.14(6) 3_665 3_665 ? C1 Mo Si 90.22(6) . . ? C1 Mo Si 89.78(6) 3_665 . ? C2 Mo Si 90.14(6) . . ? C2 Mo Si 89.86(6) 3_665 . ? Si Mo Si 180.000(7) 3_665 . ? N2 Si N1 90.84(8) . . ? N2 Si Mo 135.06(6) . . ? N1 Si Mo 133.86(6) . . ? C3 N1 C9 121.31(17) . . ? C3 N1 Si 112.35(13) . . ? C9 N1 Si 126.27(14) . . ? C4 N2 C14 121.30(16) . . ? C4 N2 Si 112.30(13) . . ? C14 N2 Si 126.16(14) . . ? O1 C1 Mo 179.18(19) . . ? O2 C2 Mo 179.3(2) . . ? C8 C3 N1 128.03(18) . . ? C8 C3 C4 119.82(18) . . ? N1 C3 C4 112.10(18) . . ? C5 C4 N2 127.86(19) . . ? C5 C4 C3 120.00(19) . . ? N2 C4 C3 112.07(17) . . ? C6 C5 C4 119.5(2) . . ? C5 C6 C7 120.6(2) . . ? C8 C7 C6 120.6(2) . . ? C7 C8 C3 119.4(2) . . ? N1 C9 C10 116.61(16) . . ? C13 C10 C11 108.9(2) . . ? C13 C10 C12 109.60(19) . . ? C11 C10 C12 108.63(19) . . ? C13 C10 C9 111.36(18) . . ? C11 C10 C9 106.23(18) . . ? C12 C10 C9 111.96(18) . . ? N2 C14 C15 116.80(17) . . ? C16 C15 C18 109.2(2) . . ? C16 C15 C17 109.7(2) . . ? C18 C15 C17 108.39(19) . . ? C16 C15 C14 111.33(18) . . ? C18 C15 C14 111.94(19) . . ? C17 C15 C14 106.2(2) . . ? #===END